WO2025181222A1

WO2025181222A1 - Method for preparing aqueous high solids emulsions

Info

Publication number: WO2025181222A1
Application number: PCT/EP2025/055320
Authority: WO
Inventors: Rob VAN HOOGHTEN; Jean VANHOEBOST
Original assignee: Emulco Laboratories BV
Current assignee: Emulco Laboratories BV
Priority date: 2024-02-27
Filing date: 2025-02-27
Publication date: 2025-09-04
Anticipated expiration: 2026-08-27
Also published as: BE1032396A1

Abstract

The present invention provides a method for preparing a substantially solvent-free, aqueous emulsion of an EPDM polymer, comprising the steps of: (i) heating EPDM polymer to a temperature T_i of at least 50°C, thereby obtaining a heated EPDM polymer; (ii) adding a surfactant to said heated EPDM polymer, thereby obtaining a homogenous premix; (iii) adding incremental parts of water to said homogenous premix at a temperature T_iii of at least 50°C, obtaining a heated EPDM in water dispersion; and (iv) mixing of the heated EPDM in water dispersion at a temperature T_iv, until an EPDM emulsion is obtained.

Description

METHOD FOR PREPARING AQUEOUS HIGH SOLIDS EMULSIONS

TECHNICAL FIELD

The present invention relates to the field of methods for preparing aqueous high solids emulsions. The present invention relates to a solvent-free, aqueous emulsion of an elastomeric polymer, comprising an EPDM polymer dispersed in an aqueous phase and a surfactant.

INTRODUCTION

Highly viscous materials, especially highly viscous polymers, are interesting candidates for applications such as sealants, adhesives and roofing. Due to their high viscosity, these materials are difficult to handle. To improve their handling, emulsion of said materials have been proposed. Especially aqueous emulsions are of high interest since the absence of organic solvents broadens the scope of applicability in an eco-friendly manner.

The preparation of aqueous emulsions of highly viscous materials is a challenging task since such highly viscous materials are difficult in handling, both in their respective solid state as in contact with water. Various approaches have been reported in the state of the art, such as US9321915.

US9321915 discloses a solvent free method for making an ethylene propylene diene terpolymer emulsion by blending water with 1 weight per cent to 50 weight percent surfactant. Solvent-free ethylene propylene diene terpolymer is blended with water and surfactant at a low pressure to form a terpolymer mixture. Via high shear mixing, meaning mixing is performed at greater than 1000 rpm, the terpolymer mixture is mixed at 0.5 atm to 1.5 atm for 5 minutes to 24 hours at a temperature from 20 degrees Celsius to 100 degrees Celsius to form a solvent free ethylene propylene diene terpolymer emulsion. The solvent-free ethylene propylene diene terpolymer emulsion has a viscosity from 10 Pa.s to 2000 Pa.s, a density from 0.8 to 1.1 and a shelf life of from 7 days to 365 days without separating or stratifying of the terpolymer emulsion.

Feasible preparation methods require processing conditions that yield stable aqueous emulsions with good handling properties and stability, while allowing for optimal use of materials and energy. In this regard, a reduced use of surfactants or emulsifiers is especially advantageous. Also, high solids content emulsions are especially desirable since they limit the total weight of the composition, which is i.e. beneficial during transportation. The present invention aims to provide improved method and composition for preparing such aqueous emulsions.

SUMMARY OF THE INVENTION

The current invention provides in a solution for at least one of the above mentioned problems by providing a method for preparing aqueous high solids emulsion.

In a first aspect, the present invention provides a method for preparing a substantially solvent-free, aqueous emulsion of an elastomeric polymer, in accordance with claim 1.

The inventors found that heating of the elastomeric polymer in step (i) to (iv) allows for the use of lower amounts of surfactants and resulted in aqueous emulsions having a reduced tackiness. Also, it was found that aqueous emulsion with high solids contents could be obtained and having smaller distributions of average particle sizes due to prolonged mixing after a heated elastomeric polymer in water dispersion is obtained.

In a second aspect, the present invention provides a aqueous emulsion of an elastomeric polymer obtained by a method according to the first aspect of the invention, in accordance with claim 7. The inventors found that a aqueous emulsion produced by the first aspect, in a particular preferred embodiment such aqueous emulsions according to the second aspect have an average particle size of at most 5 pm and a narrow standard deviation with a high solid content. Said aqueous emulsions having long shelf lives with limited stratification and sedimentation, having reduced tackiness and faster coating formation.

In a third aspect, the invention provides a waterproofing kit according to claim 10. The EPDM emulsion remains uncured and easily processable, allowing for smooth application onto the textile material, which serves as a support. As the water evaporates, the curing agent facilitates cross-linking of the EPDM, forming a durable, water-resistant coating. This system provides a convenient, non-tacky, and highly effective waterproofing solution, offering flexibility in curing methods while ensuring strong adhesion and long-term performance.

DETAILED DESCRIPTION OF THE INVENTION

Unless otherwise defined, all terms used in disclosing the invention, including technical and scientific terms, have the meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. By means of further guidance, term definitions are included to better appreciate the teaching of the present invention.

As used herein, the following terms have the following meanings:

"A", "an", and "the" as used herein refers to both singular and plural referents unless the context clearly dictates otherwise. By way of example, "a compartment" refers to one or more than one compartment.

"About" as used herein referring to a measurable value such as a parameter, an amount, a temporal duration, and the like, is meant to encompass variations of +/- 20% or less, preferably +/-10% or less, more preferably +/-5% or less, even more preferably +/-1% or less, and still more preferably +/-0.1% or less of and from the specified value, in so far such variations are appropriate to perform in the disclosed invention. However, it is to be understood that the value to which the modifier "about" refers is itself also specifically disclosed.

"Comprise," "comprising," and "comprises" and "comprised of" as used herein are synonymous with "include", "including", "includes" or "contain", "containing", "contains" and are inclusive or open-ended terms that specifies the presence of what follows e.g. component and do not exclude or preclude the presence of additional, non-recited components, features, element, members, steps, known in the art or disclosed therein.

The recitation of numerical ranges by endpoints includes all numbers and fractions subsumed within that range, as well as the recited endpoints. All percentages are to be understood as percentage by weight and are abbreviated as "wt%", unless otherwise defined or unless a different meaning is obvious to the person skilled in the art from its use and in the context wherein it is used. Where a compositions or a method for making a composition is described in terms of "parts," it is understood that these "parts" define "parts-by-weight," and are defined relative to the total amount of said composition, unless otherwise specified. Where molecular weights of polymers are mentioned, these are to be understood as weight average molecular weights, M_w, and are expressed in g/mol, unless otherwise noted.

Preferably, the molecular weight M_w can be measured by gel permeation chromatography (GPC) coupled with multi-angle light scattering (MALS). The GPC can be carried out on a PLgel Mixed-B column (i.e. Agilent). The preferred solvent is 1,2,4-trichlorobenzene (HPLC grade).

The following protocol can be used:

1. Sample preparation:

If the sample is a dispersion or emulsion, it should be dried under vacuum at 80°C for a period of at least 12 hours before testing. If the sample weight has not stabilized by 12 hours, the drying process should be repeated. 5 mg of dried EPDM should be weighed and dissolved in 2 mL of TCB with 250 ppm BHT as antioxidant, at a temperature of 135°C under continuous stirring, for a period of 4 hours to ensure complete dissolution. If aggregates or particles are noticed, the sample should be ultrasonicated. The dissolved EPDM should be filtered on a pre-heated PFTE syringe filter (0.45 pm) directly into an autosampler vial. At no point should the sample temperature drop below 100°C.

2. GPC-MALS conditions:

The autosampler vial is inserted into the GPC. The PLgel Mixed-B column is used. The flow rate is set to 1.0 mL/min, with a column temperature of 135°C and an injection volume of 200 pL. The mobile phase is TCB with 250 ppm BHT. The MALS is set to a laser wavelength of 658 nm, with at least 15 detection angles used at a data collection rate of at least 1 Hz. The column and MALS can both be calibrated with a polystyrene standard.

The terms "watery phase" or "aqueous phase" are to be understood as a part of the emulsion system that primarily consists of water, optionally including dissolved products or additives therein. Preferably, the term "aqueous" excludes the presence of organic solvents or at least limits the presence of organic solvents to an amount of less than 5 wt%, relative to the total amount of the composition, and more preferably to an amount of less than 2 wt% and even less than 1 wt%, and most preferably to an amount of less than 0.5 wt%. The term "homogenous" is to be understood as a state or condition in which the components or substances of a mixture are uniformly distributed throughout the mixture, meaning that they are evenly and thoroughly mixed at a molecular or microscopic level.

The term "emulsion" and "dispersion" are both used to describe polymer emulsions or polymer dispersions. It should be noted that the polymers described herein, in particular the more preferred embodiments such as (uncured) EPDM and PiB are best described as a viscoelastic liquids. It is generally difficult to classify these materials as a liquid or solid, as they exhibit properties of both. These polymers especially at high molecular weights are highly viscous, but do not have a fixed shape and deform when subjected to stress. After deformation, they do not return perfectly to their original shape, showing both viscous and elastic properties. They generally exhibit shear-thinning behaviour typical for non-Newtonian liquids.

The terms "solids content" refers to the non-volatile fraction of the dispersion or emulsion, regardless of whether this non-volatile fraction is a solid, gel-like or highly viscous liquid. This is generally accepted in the art of polymer dispersions.

First aspect: METHOD

In a first aspect, the present invention provides a method for preparing a substantially solvent-free, aqueous emulsion of an elastomeric polymer, comprising the steps of: i) heating said EPDM polymer thereby obtaining heated EPDM polymer, ii) adding one or more surfactants to said heated EPDM polymer under low shear mixing until a homogeneous premix is obtained, iii) dosing water in parts under low shear mixing to said homogeneous premix until a heated EPDM in water dispersion is obtained, iv) mixing of said heated EPDM in water dispersion until an EPDM emulsion is obtained.

The inventors found that heating of the elastic polymer, preferably an EPDM polymer, in step (i) to (iv) allows for the use of lower amounts of surfactants. Lower amounts of surfactants are of interest not only because they are generally expensive, but also because they were found to increase the tackiness of the resulting emulsion. A reduced tackiness is especially advantageous during handling of the emulsion. Furthermore, the inventors found that the obtained emulsions proved to be highly stable and showed a uniform and small particle size distribution. A uniform particle size distribution allows for a better control on the emulsion properties. Also, it was found that aqueous emulsion with high solids contents could be obtained.

Mixing equipment

In a preferred embodiment, the present invention provides a method according to the first aspect of the invention, whereby said EPDM polymer is mechanically agitated during step (i), step (ii), step (iii), step (iv) and any further processing steps. The term "mechanically agitation" is to be understood as a process step whereby a mechanical force is applied to a material or composition, such as, but not limiting to, stirring, mixing, kneading and/or extruding. Preferably, said EPDM polymer is mechanically agitated at least during step (i), step (ii), step (iii) and step (iv).

In a preferred embodiment, said EPDM polymer is mixed via low shear equipment. Preferred mixing equipment for low shear mixing in a batch process is selected from the list of: change-can helical mixers, kneaders, batch mixers equipped with high viscosity mixing capability or blades. Preferred mixing equipment for low shear mixing in a continuous process is selected from the list of: twin-screw extruders, corotating or counter-rotating, single, two- or multi-stage extruders where the mixing times are relatively short. An advantage of a batch process is a lower amount of surfactant is required for stabilisation of an emulsion.

In a more preferred embodiment, the EPDM polymer is mixed at shear rates lower than 1000 s ~¹, more preferably lower than 500 s ¹, more preferably lower than 300 s ~¹, more preferably lower than 200 s ~¹, more preferably lower than 100 s ~¹, more preferably lower than 80 s ~¹, more preferably lower than 75 s ~¹, more preferably lower than 60 s ~¹, more preferably lower than 50 s ~¹, more preferably lower than 40 s ~¹, more preferably lower than 30 s ~¹, more preferably lower than 25 s ~¹, more preferably lower than 20 s ~¹, more preferably lower than 15 s ~¹, more preferably lower than 10 s ~¹, more preferably lower than 8 s ~¹, more preferably lower than 5 s’ ^more preferably lower than 3 s ¹, more preferably lower than 1 s ¹. Low shear mixing is advantageous as low shear rates result in less temperature build up, lower energy use and higher energy efficiency during mixing. In an embodiment the present invention provides a method according to the first aspect of the invention, whereby said EPDM polymer is mechanically agitated. Said EPDM polymer is mixed, kneaded and/or extruded during step (ii) and step (iii), and is stirred during step (iv) and step (iv). Further process steps preferably comprise of stirring.

Mixing temperature

Preferably, said EPDM polymer is heated in step (i) to a temperature Ti above 50°C, more preferably above 60°C and even more preferably above 70°C. A higher heating temperature Ti proves to be especially advantageous for processing EPDM polymers having a high viscosity.

In a preferred embodiment, the present invention provides a method according to the first aspect of the invention, whereby said temperature Ti is at least 75°C. Preferably, said EPDM polymer is heated in step (i) to a temperature Ti above 80°C. Furthermore, the present invention provides a process according to the first aspect of the invention, whereby said temperature Ti is at most 100°C and more preferably Ti is below 95°C. A sufficiently low temperature is recommendable in order to avoid unnecessary usage of thermal energy as well as to avoid steam generation or evaporation of water.

Most preferably, said EPDM polymer is heated in step (i) to a temperature Ti of about 80.0°C, 82.5°C, °C, 85.0°C, 87.5°C or 90.0°C, or any value there in between. It is advisable to apply a higher temperature where the viscosity of the EPDM polymer is higher. Some of the advantages of the above described method is that the average particle size of the EPDM emulsion obtained by said method is significantly reduced and that the particle size distribution of said EPDM emulsion is relatively low. Thereby, an EPDM emulsion with small average particle size and a highly uniform particle size distribution is obtained, which gives rise to good flowing properties, low tackiness, relatively low viscosities and high stability of said emulsion.

Surfactant

In a preferred embodiment, the present invention provides a method according to the first aspect of the invention, whereby said surfactant is added to said heated EPDM polymer in step (ii) in an amount of at most 30 parts relative to the total weight of said EPDM polymer, and preferably in an amount of at most 15 parts, and even more preferably in an amount of at most 10 parts to obtain a homogenous premix. A sufficiently high content of surfactants or stabilizers is beneficial for the ease of forming a micro-emulsion, but goes at the expense of a higher materials use and cost, and leads to a higher tackiness, and thus a more difficult handling of the obtained emulsion.

The inventors found that an amount of surfactants lower than 6 parts relative to the total weight of said EPDM may be used, and even lower than 5 parts, or even 4 parts, or any amount there in between, may be used. Preferably, the amount of surfactants is at least 1 part, and more preferably at least 2 parts, and even more preferably at least 3 parts of surfactants, relative to the total weight of said EPDM polymer, in order to allow for a sufficient stabilisation of the aqueous emulsion and at the same time to allow for a better distribution of the surfactant materials in elastomeric and/or aqueous phase.

Any type of surfactants known to the person skilled in the art may be used. Preferably, the used surfactant or emulsifier will be selected from the group of anionic, cationic or non-ionic surface-active compounds. Preferably, said surfactant is added to said heated EPDM polymer at a temperature TH equal to temperature T.

Homogeneous premix

In a preferred embodiment, the homogeneous premix comprises at least 50 wt.% of EPDM relative to the homogeneous premix. More preferably, the homogeneous premix comprises at least 60 wt.% of EPDM, more preferably at least 70 wt.% of EPDM, more preferably at least 75 wt.% of EPDM, more preferably at least 80 wt.% of EPDM, more preferably at least 85 wt.% of EPDM, more preferably at least 90 wt.% of EPDM, more preferably at least 95 wt.% of EPDM, more preferably at least 96 wt.% of EPDM, more preferably at least 97 wt.% of EPDM. Often plasticizers, fillers, emulsifiers or other additives are combined with viscous polymers to improve their processability, in the context of emulsions and in general. However, these additives are generally difficult to remove and negatively impact the final uses. Present application aims to provide a method to produce high solids content emulsions with a low particle size, wherein the solids content is predominantly EPDM.

Dosing water In a preferred embodiment, the present invention provides a method according to the first aspect of the invention, whereby dosing parts of water added to the homogeneous premix in slow, incremental portions until a heated EPDM in water dispersion is obtained. The heated EPDM in water dispersion is obtained after catastrophic phase inversion takes place. By adding water slowly, in sufficiently small increments, improved mixing conditions are obtained. This results in both an improvement in energy efficiency as well as an improvement in the resulting emulsion, such as a reduction in the average particle size and particle size distribution.

In a preferred embodiment, water is dosed to the homogeneous premix in incremental portions. Preferably, each incremental portion comprises less than 10 wt.% relative to the weight of the homogeneous premix and each incremental portion of water is added successively to the previous portion after the dispersion of the previous incremental portion is homogeneously mixed. Adding less than 10 wt.% of water per incremental portion is advantageous because an incremental portion is faster dispersed to obtain a homogeneous EPDM in water dispersion. Preferably, said incremental portions of water are added to said heated homogeneous premix at a temperature Tm equal to temperature TH.

In one of the embodiments, said incremental portions are less than 8 wt% relative to the weight of the homogeneous premix, more preferably below 6 wt% and even more preferably at most 4 wt%. This is advantageous as low amounts of water per portion gives faster homogeneous dispersion of the water in the heated EPDM in water dispersion. Even so, preferred incremental portions decrease in percentage when the molecular weight of the EPDM increases. The lower limit for said incremental portions is 0.5 wt% relative to the weight of the homogeneous premix as lower amounts cause long mixing times. One of the values above or any amount there in between, may be used. Having large incremental portions is disadvantageous as the water remains at a surface and in between the homogeneous premix and walls and/or kneading element, creating slip between the homogeneous premix and surfaces of a kneading equipment. This leads to inefficient mixing of water into the EPDM.

Rate of water addition

The inventors have found advantageous benefits to adding water sufficiently slowly to ensure sufficient mixing between the aqueous phase and the homogeneous premixture. This is true both when water is added batch-wise in increments, in which each increment needs to be sufficiently small, as well as when water is slowly added in a continuous manner. We will further describe preferred addition rates of water to the EPDM mixture. These should be adhered to both when addition of water is done in incremental batches as well as when water is continuously dosed into the homogeneous premixture.

In another preferred embodiment, dosing water in parts under low shear mixing to the homogeneous premix comprises the slow addition of water to the homogeneous premix. Preferably, water is dosed at a rate of at most 1 wt.% per minute, relative to the weight of the homogeneous premix or the EPDM. More preferably, water is dosed at a rate of at most 0.9 wt.% per minute, more preferably at most 0.8 wt.% per minute, more preferably at most 0.7 wt.% per minute, more preferably at most 0.6 wt.% per minute, more preferably at most 0.5 wt.% per minute, more preferably at most 0.4 wt.% per minute, more preferably at most 0.3 wt.% per minute, more preferably at most 0.2 wt.% per minute, more preferably at most 0.1 wt.% per minute. All weights are relative to the weight of the homogeneous premix or relative to the weight of the EPDM. Most preferably relative to the weight of the EPDM. Preferably, the homogeneous premix predominantly comprises EPDM.

In a further preferred embodiment, water is added at a rate between 0.05 and 0.50 wt.% per minute, more preferably at a rate between 0.10 and 0.50 wt.% per minute, more preferably at a rate between 0.05 and 0.50 wt.% per minute, more preferably at a rate between 0.10 and 0.45 wt.% per minute, more preferably at a rate between 0.15 and 0.40 wt.% per minute, more preferably at a rate between 0.20 and 0.40 wt.% per minute, more preferably at a rate between 0.20 and 0.35 wt.% per minute, most preferably at a rate between 0.20 and 0.30 wt.% per minute. All weights are relative to the weight of the homogeneous premix or relative to the weight of the EPDM. Most preferably relative to the weight of the EPDM. Preferably, the homogeneous premix predominantly comprises EPDM.

Too slow addition rates of water needlessly extend the processing time. However, too fast addition rates of water are problematic for both the energy efficiency and the resulting emulsion; as water is not appropriately mixed into the highly viscous EPDM phase. The slow addition of water is particularly important as long as the water to homogeneous premix ratio is low. Preferably, the mentioned low rates of addition are maintained while the water to homogeneous premix ratio is lower than 10/90 by weight, more preferably lower than 15/85 by weight, more preferably lower than 20/80 by weight, more preferably lower than 25/75 by weight.

In a further preferred embodiment, water is added at a rate between 0.05 and 0.50 wt.% per minute, more preferably at a rate between 0.10 and 0.50 wt.% per minute, more preferably at a rate between 0.10 and 0.45 wt.% per minute, more preferably at a rate between 0.10 and 0.40 wt.% per minute, more preferably at a rate between 0.15 and 0.40 wt.% per minute, more preferably at a rate between 0.20 and 0.40 wt.% per minute, more preferably at a rate between 0.20 and 0.35 wt.% per minute, most preferably at a rate between 0.20 and 0.30 wt.% per minute as long as the water to homogeneous premix ratio is lower than 15/85 by weight. Preferably, once the water to homogeneous premix ratio is higher than 15/85 by weight, the water addition rate is significantly increased. Preferably the water addition rate is at least factor 1.5 higher, more preferably at least factor 2 higher, most preferably about factor 3 higher. In a further preferred embodiment, water is added at a rate between 0.15 and 1.50 wt.% per minute, more preferably at a rate between 0.30 and 1.50 wt.% per minute, more preferably at a rate between 0.30 and 1.2 wt.% per minute, more preferably at a rate between 0.5 and 1.20 wt.% per minute, more preferably at a rate between 0.60 and 1.2 wt.% per minute, more preferably at a rate between 0.60 and 1.0 wt.% per minute, most preferably at a rate between 0.6 and 0.90 wt.% per minute. All weights are relative to the weight of the homogeneous premix or relative to the weight of the EPDM. Most preferably relative to the weight of the EPDM. Preferably, the homogeneous premix predominantly comprises EPDM. Once sufficient water is mixed into the homogeneous premix comprising predominantly EPDM, further addition to water becomes easier and may be sped up to reduce processing times.

In a preferred embodiment, said incremental portions are between 0.5 wt% and 3 wt% relative to the weight of the homogeneous premix when an EPDM for an emulsion has a molecular weight between 20 kg/mol and 50 kg/mol. Said incremental portions are between 1 wt% and 4 wt% relative to the weight of the homogeneous premix when an EPDM for an emulsion has a molecular weight below 20 kg/mol. The lower percentage of incremental portions is advantageous as phase separation and slip at the walls of a mixing equipment, mixing element of a mixing equipment or a combination thereof can be avoided.

In an embodiment, the heated EPDM in water dispersion is obtained after catastrophic phase inversion takes place. Phase inversion is a physical process which is difficult to control. It depends on the mixture of EPDM, water and surfactant. It is strongly influenced by particle size, surfactant and temperature. Generally, catastrophic phase inversion takes place after a total amount of no more than 20 wt% water relative to the weight of the homogeneous premix, preferably no more than 15 wt%, even more preferably no more than 10 wt%, 9 wt%, 8 wt%, 7 wt%, 6 wt%, 5 wt% of water is added to the EPDM premix.

In a preferred embodiment, whereby said temperature Tj_V is at least 75°C. Preferably, said water is added to said homogeneous premix in step (iii) to a temperature T above 80°C. Furthermore, the present invention provides a process according to the first aspect of the invention, whereby said temperature Tj_V is at most 100°C. A sufficiently low temperature is recommendable in order to avoid unnecessary usage of thermal energy. Preferably, said water is added to said homogenous premix in step (iii) at a temperature Tj_V below 100°C and more preferably below 90°C. Most preferably, said water is added to said homogenous premix in step (iii) at a temperature Tm of about 80.0°C, 82.5°C, °C, 85.0°C, 87.5°C or 90.0°C, or any value there in between. Wherein the dosing and mixing occurs in a closed reactor. This is advantageous to prevent the escape of steam from the processed mixture.

In a preferred embodiment, the present invention provides a process according to the first aspect of the invention, further comprising step (iii) wherein water is dosed to said homogeneous premix at a temperature Tj_V of at least 50°C at controlled incremental steps of water of at most 10 wt% relative to the weight of the homogenous premix. Preferably, water is added to said homogenous premix at a temperature Tm of at least 75°C and more preferably at least 80°C; and said controlled incremental steps of at most 10 wt% relative to the weight of the homogenous premix and preferably at most 8 wt%, more preferably at most 6 wt% and even more preferably at most 4 wt%. Most preferably, said controlled incremental steps is above 1 wt% or any value in between the above. The weight percentage of the incremental steps of dosing water to the homogenous premix may increase during step (iii) but cannot exceed the limit of 10 wt%. In a preferred embodiment, the present invention provides a process according to the first aspect of the invention, further comprising step (iii) wherein water is dosed to said homogeneous premix at a temperature Tj_V of at least 50°C at controlled incremental steps of water of at most 10 wt% relative to the weight of the homogenous premix, whereby at a solid content of at most 95 wt% Preferably, water is added to said homogenous premix at a temperature Tm of at least 75°C and more preferably at least 80°C; and said controlled incremental steps of at most 10 wt% relative to the weight of the homogenous premix and preferably at most 8 wt%, more preferably at most 6 wt% and even more preferably at most 4 wt%. Most preferably, said controlled incremental steps is above 1 wt% or any value in between the above. The weight percentage of the incremental steps of dosing water to the homogenous premix may increase during step (iii) but cannot exceed the limit of 10 wt%.

In a preferred embodiment, the total amount of incremental portions added to the homogeneous premix is until the heated EPDM in water dispersion goes from viscoelastic liquid to a viscoelastic solid. The inventors found that an increase in torque of at least 10% of a motor rotating the mixing elements may be used to indicate the transition from viscoelastic liquid to a viscoelastic solid. Preferably an increase in torque as indication of the transition of at least 10%, more preferably an increase in torque of at least 20%, more preferably an increase in torque of at least 30%, more preferably an increase in torque of at least 40%%, more preferably an increase of at least torque is 50% %, more preferably an increase in torque of at least 60%%, more preferably an increase of at least torque 70%. Preferably, the increase of motor torque does not exceed 300%, preferably does not exceed 200%, preferably does not exceed 100% in order to avoid blockage of the mixer. The indication of motor toque increase is defined and measured over a short period of time, preferably at most 5 minutes, more preferably at most 3 minutes, more preferably at most 180 seconds, more preferably at most 60 seconds, more preferably at most 30 seconds, more preferably at most 10 seconds, most preferably at most 5 seconds.

In an embodiment, the present invention provides a process according to the first aspect of the invention, further comprising an intermediate step in step (iii) wherein additional EPDM polymer is dosed to said heated EPDM in water dispersion at a temperature T of at least 50°C of at most 250 wt% relative to the weight of the EPDM polymer present in the heated EPDM in water dispersion. Preferably dosing the additional EPDM polymer to said heated EPDM in water dispersion is at controlled incremental steps of the additional EPDM polymer of at most 10 wt% relative to the weight of the total additional EPDM polymer to be added in the heated EPDM in water dispersion. Preferably, additional EPDM polymer is added to said heated EPDM in water dispersion at a temperature T of at least 75°C and more preferably at least 80°C; and said controlled incremental steps of at most 7 wt% relative to the weight of the heated EPDM in water dispersion and preferably at most 4 wt%. Most preferably, said controlled incremental steps is above 1 wt% or any value in between the above. The weight percentage of the incremental steps of dosing water to the homogenous premix may increase during the intermediate step (iii) but cannot exceed the limit of 10 wt%. Dosing additional EPDM polymer as intermediate to step (iii) is beneficial to counter incomplete mixing of dosing water in a higher range of the incremental steps as described above. By dosing the additional EPDM polymer, an increase in friction is created in the mixing equipment, hence regaining smaller particle sizes of the heated EPDM in water dispersion after step (iii) is finished.

In a preferred embodiment mixing the heated EPDM in water dispersion until an aqueous EPDM emulsion is obtained, wherein said aqueous EPDM emulsion is defined as when no further increase and thus a stable motor torque of mixing elements is obtained. A stable motor torque is defined as a data point of motor torque that remains within an acceptable percentage of deviation from a reference value, ensuring no further phase inversion changes in morphology of the aqueous EPDM emulsion occurs. In a preferred embodiment an acceptable change in deviation in motor torque is no higher than 5% measured within 60 seconds. In a preferred embodiment stabilisation of said motor torque should last for at least 120 seconds, more preferably 300 seconds. Prolonged mixing of the EPDM in water dispersion to obtain a aqueous EPDM emulsion has the advantage of obtaining a finer standard deviation to the average particle size as a result of phase inversion having taken place in the entire heated EPDM in water dispersion. Preferably, said mixing of heated EPDM in water dispersion is at a temperature Tj_V equal to temperature T .

In an embodiment, the period of stabilisation of the torque last for 5 minutes or more preferably even 30 minutes may be used, any period in between may be used. The period of stabilisation of the torque should not exceed 60 minutes as it consumes more energy and does no longer contribute to finer standard deviation of the average particle size and avoids unnecessary usage of thermal energy as well. When operating too short mixing times, phase separation occurs and results in a non-homogeneous emulsion.

In an embodiment, the present invention provides a process according to the first aspect of the invention, comprising the step of cooling and/or allowing to cool said emulsion to a temperature below 50°C, and more preferably to a temperature below 40°C, or even below 35°C, and adding additives, i.e. thermally unstable additives.

In an embodiment an EPDM emulsion resulting from step (iv) is cooled to room temperature. In a preferred embodiment the cooling is performed while being mechanically agitated.

In an preferred embodiment, an EPDM emulsion resulting from step (iv) is cooled to room temperature and heat-sensitive additives are intermixed. Examples of these heat-sensitive additives are: peroxides, sulfur derivates, biocides, dyes and so on.

Second aspect: EMULSION

In a preferred embodiment according to the second aspect, an EPDM emulsion comprising: an EPDM polymer dispersed in an aqueous phase wherein the EPDM polymer comprises ethylene, propylene and optionally diene monomer units and a surfactant, wherein the surfactant is selected from the list of: anionic surfactants, cationic surfactants, non-ionic surfactants and mixtures thereof. The EPDM emulsion having an average particle size lower than 5 pm and a high solid content. The average particle size and particle size distribution are determined by laser diffraction, preferably measured on a Beckman Coulter LS 13 3320 laser diffractometer. The solid content is determined by thermogravimetric moisture analysis, preferably with a halogen heating system. More preferably, the sample size is at least 1g, more preferably the sample size is 5g. Preferably, the halogen heating system is set to a drying temperature of 110°C. Most preferably, the solid content is determined with a Mettler Toledo HR 73 halogen moisture analyser, with end-point determination set to automatic mode. The moisture analyser will stop the measurement when the weight loss stabilizes, indicating no further evaporation of free water.

In a preferred embodiment, the EPDM emulsion is stable. More preferably, the EPDM emulsion maintains an average particle size lower than 5 pm for at least 5 days, more preferably at least 50 days, more preferably at least 100 days, more preferably at least 200 days, more preferably at least 300 days, more preferably at least 1 year, more preferably at least 2 years, more preferably at least 3 years, more preferably at least 5 years.

EPDM polymer

In an embodiment, the present invention provides a process according to the first aspect of the invention, whereby said EPDM polymer is selected from the group comprising natural rubber, styrene-butadiene rubber, butadiene rubber, ethylene- propylene-diene (EPDM) rubber, butene rubber, polyisobutene, nitrile rubber, chloroprene rubber, fluorocarbon elastomer, polysulfide rubber.

EPDM polymer's properties vary with its ethylene, propylene and diene content. Higher ethylene content in EPDM results in improved low-temperature flexibility and processability. High ethylene contents also contributes to cost-effectiveness, making EPDM with high ethylene content suitable for applications where these properties are essential, such as automotive weatherstripping and construction seals. Higher propylene content enhances the heat resistance, chemical resistance, and resistance to aging and weathering of EPDM. It also provides excellent electrical insulation properties, making it suitable for electrical cable insulation, roofing materials, and outdoor applications. The ratio of ethylene/propylene is preferably between 40/60 to 85/15, more preferably between 40/60 to 75/25.

In a preferred embodiment, the present invention provides a process according to the first aspect of the invention, whereby said EPDM polymer is ethylene propylene diene rubber (EPDM). EPDM is a polymer obtained by polymerisation, generally by anionic polymerisation, of ethylene, propylene and optionally diene as fundamental monomeric units.

EPDM exists in different molecular weights. Low molecular weight is understood as a molecular weight up to 100 kg/mol, and preferably 5 kg/mol to 75 kg/mol; medium molecular weight is understood from 100 kg/mol to 200 kg/mol; and high molecular weight is understood as above 200 kg/mol. Dienes are advantageous as an EPDM comprising diene monomeric units are more easy to cure. During dosing of water to the homogenous premix in a batch mixer, a thin layer is formed protecting the unsaturated EPDM polymer of the homogeneous premix underneath. In a further preferred embodiment, the EPDM polymer has a molecular weight higher than 1.000 g/mol, more preferably higher than 1.500 g/mol, more preferably higher than 2.000 g/mol, more preferably higher than 3.000 g/mol, more preferably higher than 4.000 g/mol, more preferably higher than 5.000 g/mol, more preferably higher than 6.000 g/mol, more preferably higher than 7.000 g/mol, more preferably higher than 8.000 g/mol, more preferably higher than 10.000 g/mol, more preferably higher than 20.000 g/mol, more preferably higher than 30.000 g/mol, more preferably higher than 40.000 g/mol, more preferably higher than 50.000 g/mol, more preferably higher than 60.000 g/mol, more preferably higher than 70.000 g/mol, more preferably higher than 80.000 g/mol, more preferably higher than 90.000 g/mol, preferably higher than 100.000 g/mol. Preferably the molecular weight is lower than 1.000.000 g/mol, more preferably lower than 500.000 g/mol, more preferably lower than 400.000 g/mol, more preferably lower than 300.000 g/mol, more preferably lower than 200.000 g/mol, more preferably lower than 180.000 g/mol, more preferably lower than 160.000 g/mol, more preferably lower than 140.000 g/mol, more preferably lower than 120.000 g/mol, more preferably lower than 100.000 g/mol, more preferably lower than 95.000 g/mol more preferably lower than 90.000 g/mol more preferably lower than 85.000 g/mol more preferably lower than 80.000 g/mol more preferably lower than 75.000 g/mol more preferably lower than 70.000 g/mol, more preferably lower than 65.000 g/mol, more preferably lower than 55.000 g/mol. Higher molecular weights are currently not economical to emulsify, due to excessive energy requirements and difficulties with handling. Lower molecular weights are not as advantageous to emulsify, as the uncured polymer is sufficiently liquid and processable to process directly without requiring emulsification.

In a preferred embodiment, the present invention provides a process according to the first aspect of the invention, whereby said EPDM polymer has a glass transition temperature T_g of at most 50°C, preferably at most 25°C, or even at most 0°C. More preferably, said glass transition temperature T_g is lower than -10°C, and more preferably lower than -30°C. This is advantageous since a sufficiently low glass transition temperature allows for a good processing, especially at higher temperatures, i.e. during mechanical agitation.

In a preferred embodiment, the present invention provides a process according to the first aspect of the invention, whereby said EPDM polymer has a viscosity of at least 30.000 mPa.s, as determined by Brookfield viscometer at 150°C. Preferably, said EPDM polymer has a viscosity of higher than 40.000 mPa.s, or even higher than 50.000 mPa.s, higher than 60.000 mPa.s, higher than 70.000 mPa.s, higher than 80.000 mPa.s, or higher than 90.000 mPa.s. More preferably, said EPDM polymer has a viscosity of 100.000 mPa.s to 1.500.000 mPa.s, and even more preferably of 120.000 mPa.s to 1.000.000 mPa.s or of 140.000 mPa.s to 800.000 mPa.s.

Preferably, said EPDM polymer has a viscosity of at least 150.000 mPa.s, more preferably at least 200.000 mPa.s, more preferably at least 250.000 mPa.s, more preferably at least 300.000 mPa.s, more preferably at least 350.000 mPa.s, more preferably at least 400.000 mPa.s, more preferably at least 450.000 mPa.s, more preferably at least 500.000 mPa.s, more preferably at least 550.000 mPa.s, more preferably at least 600.000 mPa.s, more preferably at least 650.000 mPa.s, more preferably at least 700.000 mPa.s, most preferably at least 750.000 mPa.s. This is especially advantageous since the devised method is especially suitable for such highly viscous materials.

EPDM polymer with various molecular weights are commercially available. Examples of EPDM produced by The Dow Chemical Company are: Nordel 3720P, Nordel 3722P, Nordel 4520, Nordel 4570, Nordel 4725P, Nordel. Examples produced by Lion Copolymer Geismar LLC: Trilene® 65, Trilene® 67, Trilene® 77, Trilene® CP80, Trilene® CP600, Trilene® CP1100, Trilene® CP2000. Examples produced by ExxonMobil Chemical Company are Vistaion 1703P, Vistaion 2504, Vistaion 703, Vistaion 706, Vistaion 722, Vistaion 785, Vistaion 805, Vistaion 8731, Vistaion 878P. Examples produced by Arlenxeo are Keltan® 2450, Keltan® 2470E, Keltan® 2470S, Keltan® 2650, Keltan® 2750, Keltan® 3470, Keltan® 3973, Keltan® 4450, Keltan® 4465, Keltan® 4460D, Keltan® 4577, Keltan® 4869C, Keltan® 5465.

Water

Water is selected from the list of: distilled water, deionized water, tap water, process water or a combination thereof. In a preferred embodiment, water is selected from the list of: distilled water, deionized water or mixture thereof. Distilled and deionized water have the advantage that no ions are present in the water to interact with surfactants. In another embodiment, the water is process water. The use of process water has the advantage of reusing water and is an ecologic benefit for the application wherein the resulting composition is used.

Particle size Solvent-free EPDM emulsion having an average particle size of at most 10 pm, preferably lower than 5 pm and more preferably below 2 pm and is determined using a Beckman Coulter LS 13 320 laser diffractometer MW. More preferably, said emulsion of an EPDM polymer has an average particle size of at most 1 pm, more preferably at most 800 nm, more preferably at most 750 nm, more preferably at most 600 nm, more preferably at most 500 nm, more preferably at most 400 nm, more preferably at most 250 nm, more preferably at most 150 nm, more preferably at most 100 nm, most preferably at most 50 nm. This is advantageous because said average particle size provides a high stability of said emulsion, especially of said EPDM emulsion and has faster curing rates.

In a preferred embodiment, said EPDM emulsion have a narrow particle size distributions with a variation of at most 1.0 pm, more preferably at most 0.9 pm, more preferably at most 0.8 pm, more preferably at most 0.7 pm, more preferably at most 0.6 pm, more preferably at most 0.5pm, more preferably at most 0.4 pm, more preferably at most 0.3 pm, more preferably at most 0.2 pm, more preferably at most 0.1 pm. Particle size distribution is determined using a Beckman Coulter LS 13 320 laser diffractometer MW. Preferably, the EPDM emulsion has both a low average particle size and a narrow particle size distribution. The smaller the variation in particle size, the more stable the EPDM emulsion and longer stability of the emulsion is obtained, meaning no sedimentation or stratification occurs.

EPDM emulsion having a solids content below 95 wt%, more preferable between 40 wt% to 90 wt%. In a preferred embodiment, the EPDM emulsions have a solids content of at least 50 wt%, more preferably at least 55 wt%, more preferably at least 60 wt%, more preferably at least 65 wt%, more preferably at least 70 wt%, more preferably at least 75 wt%, most preferably at least 80 wt.% In a preferred embodiment, the EPDM emulsions have a solids content of at most 90 wt%, more preferably at most 85 wt%, most preferably at most 80%. Solid content of the EPDM emulsion is determined using a Mettler Toledo HR 73 halogen moisture analyzer. Higher solid content is more desirable for applications and transport. Furthermore, higher solids content provides better stability of the emulsion and faster curing.

Diene monomer

In an preferred embodiment, an EPDM emulsion comprising of an EPDM polymer having diene monomer units selected from: norbornene derivates, linear and short branched alkyl dienes, cycloalkyl dienes, chloroalkyl dienes or a combination thereof. Non-limiting examples are selected from the list of: methylidene norbornene, dicyclopentadiene, ethylidene norbornene, a 1,4-hexadiene, norbornadiene, isoprene, vinyl norbornene or a combination thereof. Choosing one or more of the diene monomer units is in order to tailor the flexibility and elasticity of the final EPDM product. By selecting branched, long chain or a combination thereof, monomer units the final EPDM product will be more flexible. Cyclic diene monomers improved rigidity, especially at higher temperatures and to an extend the elasticity of an EPDM final product.

In an embodiment, an EPDM emulsion comprising of an EPDM polymer having diene monomer units, said diene monomer units are present in a percentage relative to the EPDM polymer. Diene monomer unit content is preferably between 1 wt% to 15 wt%, more preferable between 2 wt% to 13 wt%, even more preferable between 7 wt%, 8 wt%, 10 wt%, 11 wt% or any diene monomer unit content there in between. A higher diene content provides enhanced flexibility, elasticity, and impact resistance. Hence, higher diene content in EPDM polymer is used in applications where material needs to bend and flex without cracking.

In an embodiment, an EPDM emulsion comprising of an EPDM polymer having diene monomer units, said diene monomer units are present in a percentage relative to the EPDM polymer. Diene monomer unit content is preferably between 1 wt% to 15 wt%, more preferable between 2 wt% to 13 wt%, even more preferable between 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt% or any diene monomer unit content there in between. A lower diene content has excellent weather resistance, UV resistance, and ozone resistance. Lower diene content is used in outdoor applications, such as roofing membranes and automotive weather sealing.

In a preferred embodiment, said EPDM polymer comprises diene. More preferably, the diene is chosen from the list of: ethylidene norbornene (ENB), dicyclopentadiene (DCPD), 1,4-hexadiene (HD), or mixtures thereof. Most preferably, the diene is ethylidene norbornene (ENB) or dicyclopentadiene (DCPD). In a preferred embodiment, the EPDM polymer has a diene content of at least 0.5 wt.%, more preferably at least 1.0 wt.%, even more preferably at least 1.5 wt.%, still more preferably at least 2.0 wt.%, yet more preferably at least 2.5 wt.%, even yet more preferably at least 3.0 wt.%, most preferably at least 3.5 wt.%, particularly preferably at least 4.0 wt.%, more particularly preferably at least 4.5 wt.%, especially preferably at least 5.0 wt.%, more especially preferably at least 5.5 wt.%, even more especially preferably at least 6.0 wt.%, still even more especially preferably at least 6.5 wt.%, and most especially preferably at least 7.0 wt.%. In a preferred embodiment, the EPDM polymer has a diene content of at most 15.0 wt.%, more preferably at most 14.5 wt.%, even more preferably at most 14.0 wt.%, still more preferably at most 13.5 wt.%, yet more preferably at most 13.0 wt.%, even yet more preferably at most 12.5 wt.%, most preferably at most 12.0 wt.%, particularly preferably at most 11.5 wt.%, more particularly preferably at most 11.0 wt.%, especially preferably at most 10.5 wt.%, more especially preferably at most 10.0 wt.%, even more especially preferably at most 9.5 wt.%, still even more especially preferably at most 9.0 wt.%, and most especially preferably at most 8.5 wt.%, with an upper limit of 8.0 wt.% in the most refined embodiment. EPDM with ENB or DCPD offers significant advantages over HD for waterproofing applications, particularly when applied as an aqueous emulsion to create a durable, high- performance coating. ENB enhances cross-linking efficiency, leading to improved mechanical strength and long-term elasticity, ensuring that the waterproof membrane retains its flexibility even after prolonged exposure to environmental conditions. Its high reactivity allows for fast curing, improving processability and reducing application time. Additionally, ENB contributes to excellent heat and oxidation resistance, making it well-suited for outdoor waterproofing solutions. DCPD, on the other hand, provides superior thermal and oxidative stability, which extends the lifespan of the waterproofing membrane under extreme weather conditions. Its lower reactivity compared to ENB minimizes unwanted side reactions, resulting in improved formulation control, particularly in emulsion-based coatings. DCPD-containing EPDM further enhances hydrolysis resistance, preventing degradation when exposed to prolonged moisture or standing water. The increased rigidity of DCPD-based EPDM offers additional benefits in structural waterproofing applications where dimensional stability is required. These properties make ENB- or DCPD-based EPDM the preferred choice for waterproofing membranes that demand a balance of durability, flexibility, and resistance to environmental stress while maintaining efficient processability and strong adhesion to a variety of substrates.

The EPDM polymer and EPDM emulsion is preferably uncured. It is the aim of present invention to apply uncured EPDM in a processable and easy manner, avoiding tackiness and once applied it can be cured in place. It should be noted that in certain conditions, cured EPDM can also be dispersed. However, this is not envisaged by present application. Furthermore, the method described in the first aspect of the invention does not lend itself to dispersion of EPDM with a high degree of curing. Uncured EPDM is preferably characterized by a gel fraction of at most 40%, more preferably at most 30%, more preferably at most 20%, more preferably at most 10%, most preferably at most 5%. Gel fraction is measured in toluene, over a period of 48 hours at 20°C, followed by centrifugation and drying at 60°C until a constant weight is obtained. The gel fraction is determined as the ratio by weight of the dried insoluble gel to the weight of the sample.

Surfactants

In one of the embodiments anionic surfactants can be selected from: saponified fatty acids, derivatives of fatty acids with carboxylic groups, carboxylates, sulphonates, fatty acid alcohol sulphates or a combination thereof. Non-limiting examples are: sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, stearates, oleates, laurates, cocoates of alkaline metals or ammonium, alkanolamines, ether carboxylates, ethoxylated fatty acid glycerides, alkyl benzene sulphonates, alkyl naphthalene sulphonates condensed with formaldehyde, lignin sulphonates, alkyl sulphonates, sulphonated oil, olefin sulphonates, aromatic sulphonates, fatty acid alcohol sulfate, coco fatty acid alcohol ether sulphates or ether sulphates.

In one of the embodiments cationic surfactants can be selected from a non-limiting list of: dialkyl benzene alkyl ammonium chloride, alkyl benzyl methyl ammonium chloride, N-alkyl tallow propylene diamine, alkyl benzyl dimethyl ammonium bromide, benzalkonium chloride, cetyl trimethyl ammonium chloride, cetyl pyridinium bromide, dodecyl trimethyl ammonium bromides, halide salts of quaternary polyoxy-ethylalkylamines, dodecyl benzyl triethyl ammonium chloride, dodecylbenzene sulfonic acid quaternary ammonium or combination thereof.

In one of the embodiments non-ionic surfactants can be selected from a non-limiting list of: ethoxylated castor oil, ethoxylated sorbitan monolaurate, polyoxyethylene sorbitan monooleate, ethoxylated glyceryl monostearate, ethoxylates glyceryl oleate, ethoxylated isotearyl alcohol, polyvinyl alcohol, polyacrylic acid, methalose, methyl cellulose, ethyl cellulose, propyl cellulose, hydroxy ethyl cellulose, carboxymethyl cellulose, polyoxyethylene cetyl ether, polyoxyethylene lauryl ether, polyoxyethylene octyl ether, polyoxyethylene octylphenyl ether, polyoxyethylene oleyl ether, polyoxyethylene sorbitan monolaurate, polyoxyethylene stearyl ether or combination thereof. In one of the embodiment surfactants are anionic surfactants and present in the EPDM emulsion in a range of 0.1 wt% to 30 wt% relative to the EPDM emulsion, more preferably between 0.5 wt% to 20.0 wt% and even more preferable between 1.0 wt%, 2.0 wt%, 3.0 wt%, 4.0 wt%, 5.0 wt% or any anionic surfactant content in between. The anionic surfactants are prevalent in emulsions for their ability to provide a negatively charged interface, contributing to effective dispersion and stabilization. Anionic surfactants find applications in formulations whereas the pH of such applications are above a pH of 8. The pH is determined with a WTW Inolab® pH 7110 with SenTix® 81 electrode.

In one of the embodiment surfactants are cationic surfactants and present in the EPDM emulsion in a range of 0.1 wt% to 30 wt% relative to the EPDM emulsion, more preferably between 0.5 wt% to 20 wt% and even more preferable between 0.5 wt%, 1.0 wt%, 1.5 wt%, 2.0 wt%, 2.5 wt%, 3.0 wt%, 3.5 wt% or any cationic surfactant content in between. Cationic surfactants are positively charged, hence the emulsion has application in correspondence with a pH below 6. The pH is determined with a WTW Inolab® pH 7110 with SenTix® 81 electrode.

In one of the embodiment surfactants are non-ionic surfactants, percentage added to an EPDM emulsion can range from 0.1 wt% to 30.0 wt% relative to the EPDM emulsion, more preferably between 0.5 wt% to 20.0 wt% and even more preferable between 1.0 wt%, 2.0 wt%, 3.0 wt%, 4.0 wt%, 5.0 wt%, 6.0 wt%, 7.0 wt%, 8.0 wt%, 9.0 wt%, 10.0 wt% or any non-ionic surfactant content in between. Non-ionic surfactants are known for their compatibility with a wide range of substances. Non- ionic surfactants are used in emulsions requiring a pH between 6 to 8. The pH is determined with a WTW Inolab® pH 7110 with SenTix® 81 electrode.

Curing agent

In a preferred embodiment, an EPDM emulsion comprises a curing agent and is selected from the non-limitative list of: sulfur, sulfur derivatives, peroxides, hydroperoxides, peroxy-carbonate, thiuram, thiazole, dithiocarbamate, xanthate, siccatives such as metal carboxylates (including cobalt, manganese, zirconium, or calcium salts), or a combination thereof. In a further preferred embodiment, the curing agent in the EPDM emulsion comprises a siccative, preferably chosen from the non-limitative list of: cobalt octoate, manganese octoate, zirconium octoate, calcium octoate, or a combination thereof. More preferably, the siccative is cobalt octoate or manganese octoate, as these provide efficient oxidative curing and promote cross-linking while maintaining stability in the emulsion. Most preferably, the siccative is cobalt octoate, which ensures rapid curing and optimal mechanical properties of the resulting EPDM coating.

In one embodiment, the curing agent added to an EPDM emulsion is present in an amount ranging from 0.1 wt% to 15.0 wt% relative to the EPDM emulsion, more preferably from 0.5 wt% to 10.0 wt%, and even more preferably from 1.0 wt% to 7.5 wt%. For sulfur or sulfur derivative curing agents, the preferred amount ranges from 0.5 wt% to 5.0 wt%, more preferably from 1.0 wt% to 4.0 wt%, and even more preferably from 1.5 wt% to 3.0 wt%. These concentrations ensure sufficient crosslinking while maintaining the desired flexibility and processability of the EPDM composition. Peroxide-based curing agents, including peroxides, hydroperoxides, and peroxy-carbonates, are more preferably present in amounts ranging from 0.5 wt% to 10.0 wt%, more preferably from 1.0 wt% to 5.0 wt%, and even more preferably from 1.0 wt% to 3.0 wt%. This range balances efficient peroxide-initiated crosslinking with optimal mechanical properties. Thiuram, thiazole, dithiocarbamate, or xanthate curing agents are even more preferably used in amounts from 0.5 wt% to 2.0 wt%, more preferably from 0.75 wt% to 1.5 wt%, and even more preferably from 1.0 wt% to 1.25 wt%. These accelerators facilitate rapid curing while minimizing over-curing risks. Epoxide curing agents are most preferred in amounts ranging from 0.2 wt% to 5.0 wt%, more preferably from 0.5 wt% to 3.0 wt%, and even more preferably from 1.0 wt% to 2.0 wt%. These levels contribute to effective epoxy crosslinking while maintaining stability in the emulsion. Siccatives, such as metal carboxylates, are preferably present in amounts ranging from 0.1 wt% to 1.5 wt%, more preferably from 0.1 wt% to 1.0 wt%, and even more preferably from 0.1 wt% to 0.3 wt%. These compounds help accelerate oxidative curing and improve film formation in coatings or adhesives applications. These ranges provide balanced crosslinking efficiency, mechanical properties, and processing stability for EPDM emulsions, taking into account typical industry standards for elastomeric materials.

In an embodiment, an EPDM emulsion comprises of a sulfur activator and is selected from the non-limitative list of: zinc oxide, diethyldithiocarbamate, zinc benzothiozole or a combination thereof. The sulfur activator acts as an accelerator during the vulcanisation process if sulfur or sulfur derivates are present in the EPDM emulsion as curing agents. Hence lower curing temperatures are required which is beneficial for ecological reasons.

In an embodiment, an EPDM emulsion comprises a curing agent selected from the list of: peroxides, hydroperoxides, peroxy-carbonates, and a peroxide coagent, wherein said peroxide coagent is selected from the list of: triallyl isocyanurate (TAIC), trimethylolpropane trimethacrylate (TMPTMA), high vinyl polybutadiene, or a combination thereof. The peroxide coagent is beneficial during the curing of an EPDM emulsion as it provides optimized curing control. More preferably, the EPDM emulsion comprises a combination of a primary coagent, such as TAIC or TMPTMA, with high vinyl polybutadiene as a secondary coagent. High vinyl polybutadiene, as a type II coagent, improves crosslinking efficiency by reacting with radicals formed during peroxide decomposition, thereby enhancing the mechanical properties of the cured EPDM.

Peroxide coagents can be classified into type I and type II coagents based on their reaction mechanism. Type I coagents, such as TAIC and TMPTMA, contain multifunctional unsaturated groups that directly participate in crosslinking by forming covalent bonds between polymer chains. In contrast, type II coagents, including high vinyl polybutadiene, function by generating additional reactive sites through hydrogen abstraction, thereby promoting controlled crosslink density and improving elastomeric properties. The inclusion of high vinyl polybutadiene as a secondary coagent is particularly advantageous for achieving an optimal balance of elasticity, heat resistance, and mechanical strength in the cured EPDM composition.

In a preferred embodiment, an EPDM emulsion comprising a curing agent wherein said curing agent is added to water and administered to a homogenous premix while dosing the water to the homogenous premix. More preferable, the curing agent is added to the homogenous premix via the water, only at final dosages of water. The final dosages of water are defined as at least 50 wt%, relative to total amount of water to produce an EPDM emulsion, is already administered to the homogenous premix. More preferably at least 60 wt% is already administered to the homogenous premix. Even more preferably at least 65 wt%, 70 wt%, 75 wt%, 80 wt%, 85 wt%, 90 wt%, 95 wt% or amount of water in between is already administered to the homogenous premix. The advantage of adding the curing agent to the water is that fast curing does not occur before applying the EPDM emulsion to a surface. Additionally, finely dispersed curing agent enhances faster curing of the EPDM emulsion. Optionally the sulfur activator or peroxide coagent is added to the homogenous premix in the same way as the curing agent.

In an embodiment, a curing agent is mixed with an EPDM emulsion prior to applying the EDPM emulsion to a surface. More preferably the curing agent is already added to the EPDM emulsion during production of an EPDM emulsion according to the first aspect, and are the sulfur activator or peroxide coagent mixed prior to applying the EPDM emulsion to a surface. The benefits of administering the sulfur activator or peroxide coagent is that the EPDM emulsion can be stored at higher temperatures.

Additives

In an embodiment, an EPDM emulsion comprises a rheology modifier selected from the list of: non-ionic surfactants, associative thickeners, fumed or colloidal silica, clay minerals, or a combination thereof. In another or further preferred embodiment, the zero-shear viscosity of the EPDM emulsion is between 0.1 Pa.s and 10000.0 Pa.s. Preferably, the zero-shear viscosity of the EPDM emulsion is lower than 5000.0 Pa.s, more preferably lower than 2000.0 Pa.s, more preferably lower than 1000.0 Pa.s, more preferably lower than 500.0 Pa.s, more preferably lower than 200.0 Pa.s, more preferably lower than 100.0 Pa.s, more preferably lower than 50.0 Pa.s, more preferably lower than 20.0 Pa.s, more preferably lower than 10.0 Pa.s, more preferably lower than 5.0 Pa.s, more preferably lower than 2.0 Pa.s, and most preferably between 0.1 Pa.s and 1.0 Pa.s. Zero-shear viscosity is determined by a rotational rheometer with a cone-plate configuration using a creep test as measured at 20.0°C. The use of rheology modifiers in an EPDM emulsion is beneficial as they tailor the rheology by improving stabilization while ensuring that the emulsion maintains a controlled viscosity profile depending on application needs. A low-viscosity, non-tacky EPDM emulsion is particularly advantageous for waterproofing applications, as it enables easy application by spraying, brushing or rolling while maintaining excellent substrate wetting and adhesion. The low viscosity enhances processability and facilitates uniform coverage over large surfaces, making it especially suitable for construction and sealing applications where ease of handling and consistent film formation are critical.

Additives can have a positive influence on the production process of an emulsion, and may provide certain desired characteristics to emulsions. An example of possibly used additives are: defoaming agent, anti-foaming agents fillers, pigments, antioxidants, biocides, anti-settling agent, bases to optimize the saponification process, as well as bactericides, dyes. It should be clear to one skilled in the art that these are just examples of possibly used additives, and that other options are also possible.

In an embodiment, the present invention provides a process according to the first aspect of the invention, whereby no aromatic and/or chlorinated organic solvents are added during any step of said process.

In a preferred embodiment, the present invention provides a process according to the first aspect of the invention, whereby the prepared EPDM emulsion is essentially free of organic solvents, i.e. no organic solvents are added during any step of said process.

As used herein, the phrase "essentially free of organic solvents" means that solvents are not added to the EPDM polymer and surfactant premix in order to create a mixture of suitable viscosity that can be processed on typical emulsification devices. More specifically, "organic solvents" as used herein is meant to include any water immiscible low molecular weight organic material added to the non-aqueous phase of an emulsion for the purpose of enhancing the formation of the emulsion, and is subsequently removed after the formation of the emulsion, such as evaporation during a drying or film formation step. Thus, the phrase "essentially free of organic solvent" is not meant to exclude the presence of solvent in minor quantities in process or emulsions of the present invention. For example, there may be instances where the EPDM polymer or surfactant used in the premix composition contains minor amounts of solvent as supplied commercially. Small amounts of solvent may also be present from residual cleaning operations in an industrial process. Furthermore, small amounts of solvent may also be added to the process of the present invention for purposes other than to enhance the formation of the EPDM emulsion. Preferably, the amount of solvent present in the premix should be less than 5 % by weight of the premix, more preferably the amount of solvent should be less than 2% by weight of the premix, and most preferably the amount of solvent should be less than 1% by weight of the premix. Illustrative examples of "organic solvents" that are included in the above definition are relatively low molecular weight hydrocarbons having normal boiling points below 200°C, such as alcohols, ketones, ethers, esters, aliphatics, alicyclics, or aromatic hydrocarbon, or halogenated derivatives thereof. As merely illustrative of solvents to be included in the definition of "organic solvents", there may be mentioned butanol, pentanol, cyclopentanol, methyl isobutyl ketone, secondary butyl methyl ketone, diethyl ketone, ethyl isopropyl ketone, diisopropyl ketone, diethyl ether, sec-butyl ether, petroleum ether, ligroin, propyl acetate, butyl and isobutyl acetate, amyl and isoamyl acetate, propyl and isopropyl propionate, ethyl butyrate, pentane, hexane, heptane, cyclopentane, cyclohexane, cycloheptane, methylene chloride, carbon tetrachloride, hexyl chloride, chloroform, ethylene dichloride, benzene, toluene, xylene, chlorobenzene, and mixtures thereof with each other and/or more water soluble solvents.

In a particular preferred embodiment, the EPDM emulsion comprises an (uncured) EPDM polymer with following properties:

- the ethylene to propylene ratio is preferably between 45/55 and 55/45;

- the diene content is 6 wt.% to 12 wt.%, more preferably 9 wt.% to 11 wt.%, all relative to the weight of the EPDM polymer; preferably the diene is chosen from ENB and DCPD;

- the molecular weight M_w of the EPDM is between 30000 Da and 100000 Da, more preferably between 35000 Da and 50000 Da;

- the surfactant is preferably selected from the list of anionic, cationic or nonionic surfactants;

- the solids content is preferably at least 50.0 wt.%, more preferably at least 51.0 wt.%, more preferably at least 52.0 wt.%, more preferably at least 53.0 wt.%, more preferably at least 54.0 wt.%, more preferably at least 55.0 wt.%, relative to the weight of the EPDM emulsion;

- The EPDM emulsion preferably comprises EPDM in an amount of at least 50.0 wt.%, more preferably at least 51.0 wt.% EPDM, more preferably at least 52.0 wt.% EPDM, more preferably at least 53.0 wt.% EPDM, more preferably at least 54.0 wt.% EPDM, more preferably at least 55.0 wt.% EPDM, all relative to the weight of the EPDM emulsion;

- The EPDM emulsion has a zero-shear viscosity lower than 10.0 Pa.s, more preferably lower than 1.0 Pa.s.

The preferred EPDM emulsion is preferably cured using a curing package comprising sulfur or sulfur derivatives, peroxides, UV initiators, siccatives, or mixtures thereof. More preferably, the curing package comprises peroxides, UV initiators, siccatives, or mixtures thereof. Even more preferably, the curing package consists essentially of peroxides, UV initiators, or a combination of peroxides and siccatives. The preferred EPDM emulsion forms a stable, pumpable, and easily mixable composition, ideal for efficient processing, drying, and curing. With an ethylene-to-propylene ratio of 45/55 to 55/45, a diene content of 6-12 wt.% (preferably 9-11 wt.%), and a molecular weight of 30,000-100,000 Da (preferably 35,000-50,000 Da), it balances flexibility and durability. The high solids content (>50 wt.%, preferably >55 wt.%) ensures rapid drying, while the zero-shear viscosity (<10 Pa.s, preferably <1 Pa.s) allows smooth handling. The curing package includes sulfur derivatives, peroxides, UV initiators, and siccatives, ensuring controlled crosslinking. Optimized for waterproofing, this emulsion is particularly suited for a kit comprising the EPDM emulsion, a curing package, and a textile material, enabling durable, flexible, and easy-to-apply coatings.

In a third aspect, the present invention relates to a kit suitable for waterproofing, comprising an EPDM emulsion preferably according to the second aspect; a textile material, and a curing agent, wherein the curing agent may be present in the EPDM emulsion, the textile material, or as a separate component within the kit. The invention provides a non-tacky, easily handled, and efficiently curable waterproofing solution, particularly suited for applications where a flexible yet durable waterproof layer is required.

The EPDM emulsion included in the kit preferably comprises uncured EPDM dispersed in an aqueous phase, thereby allowing for easy application and uniform distribution over the textile material. The EPDM polymer is selected to maintain stability in the emulsion state while remaining non-tacky upon drying. The uncured EPDM preferably has a gel fraction below 20%, more preferably below 10%, when measured after 48 hours of extraction in toluene at 20°C. It is the aim of the kit to cure EPDM once it is applied and appropriately mixed with the textile material. The curing process may be triggered thermally, chemically, through drying out of the emulsion or through exposure to UV or sunlight.

The kit further comprises a textile material, which serves as a reinforcing support onto which the EPDM emulsion is applied. The textile material may be either woven or non-woven, with non-woven materials being particularly preferred due to their uniform porosity, enhanced impregnation properties, and mechanical flexibility. Suitable materials include, but are not limited to, polyester, polypropylene, glass fiber, cellulose-based fibers, or blends thereof. The selection of the textile material can be optimized based on the desired mechanical properties, adhesion requirements, and end-use application. The curing agent is included in the kit in various possible configurations, allowing for controlled curing of the EPDM once applied to the textile material. In certain embodiments, the curing agent is pre-impregnated into the textile material, ensuring that the EPDM emulsion undergoes cross-linking upon contact with the support. Furthermore, this ensures separation of the curing agent and the EPDM until both textile material and EPDM are brought into contact. Furthermore, the aqueous bulk phase of the emulsion prevents immediate curing upon contact. This allows workability and spreadability of the EPDM emulsion for a period of time prior to initiation of curing. In other embodiments, the curing agent is incorporated into the aqueous phase of the EPDM emulsion, preferably as a water-dispersible or water-soluble curing agent, which remains separate from the EPDM phase until the emulsion dries. This is particularly beneficial from a safety point of view, as it prevents direct contact between often reactive and harmful curing agent and those applying the kit. Advantageously, both of these embodiments improve ease of use, promoting uniform distribution of the curing agent brought into contact with EPDM. These embodiments are both particularly suitable for in-situ curing of EPDM by consumers, rather than professionals, while promoting safety and highly performant waterproofing. Alternatively, the curing agent may be provided as a separate solvent-based or aqueous dispersion, allowing for independent dosing and activation. This flexibility enables tailored curing conditions based on the application requirements. A curing agent is considered water-dispersible if, when incorporated into the EPDM emulsion, the majority of the curing agent resides in the aqueous phase rather than the EPDM phase. This means that the curing agent remains substantially distributed within the continuous water phase and does not significantly partition into the dispersed EPDM phase. As a result, the curing agent comes into bulk contact with the EPDM phase predominantly upon drying of the emulsion, ensuring that curing occurs primarily during or after water evaporation rather than within the emulsion itself.

Upon application of the EPDM emulsion onto the textile material, the water present in the emulsion evaporates, leaving behind a uniform, uncured EPDM coating on the textile substrate. The curing process can then be initiated through heat, moisture, or chemical activation, depending on the curing agent formulation. The resulting waterproofed textile exhibits excellent resistance to water penetration, high mechanical durability, and long-term flexibility, making it suitable for applications such as roofing membranes, protective coatings, and barrier layers in construction and industrial applications. By providing the curing agent within the textile material, the emulsion, or separately, the kit ensures an easy-to-use and efficient curing process while maintaining storage stability and ease of handling. The ability to cure the EPDM coating only after application prevents premature cross-linking, enabling smooth application and extended workability. The kit offers several advantages over traditional waterproofing solutions, particularly those relying on pre-vulcanized or solvent-based EPDM coatings. The aqueous nature of the EPDM emulsion eliminates the need for harmful organic solvents, making the system environmentally friendly and safer to handle. Furthermore, by using an uncured EPDM composition, the material retains high flexibility during processing, ensuring strong adhesion to the textile substrate while allowing for post-application curing. The option to select the curing mode and agent delivery method provides additional versatility for different end-use applications.

The present invention provides a use of a aqueous emulsion of an EPDM polymer according to the second aspect of the invention. These emulsions are suitable for applications, such as gluing systems, cosmetic, plant protection, preparation and treatment of paper, production and processing of textiles and leather, coatings, pharmaceutical applications, construction, wood treatment, water and gas barrier for e.g. methane, carbon dioxide, radon, protected coating for radioactive radiation.

EXAMPLES

In the following examples are intended to further clarify the present invention, and are nowhere intended to limit the scope of the present invention.

EXAMPLE 1

1800 g of EPDM polymer with a molecular weight of 47 kg/mol with ethylene/propylene ratio of 50/50 and dipentacyclopentadiene of 10 wt%, relative to the weight of the EPDM polymer, EPDM polymer is charged into a batch Z-plate kneader, set at a constant temperature of about 85°C and at a pressure of 1 bar. The EPDM polymer is stirred at 50 rpm and a surfactant solution of 80 g stearic acid and 22 g 2-amino-2-methyl-l- propanol is added, at controlled equal increments parts 670 g of soft water is added to the homogenous premix. Subsequently, water is added in equal increments parts to the homogenous premix until the solids content is 74 wt%. The mixture forms a EPDM emulsion and heating is switched off.

The final composition of the obtained EPDM emulsion is a creamy paste and its physical properties are reported in Table 1 and Table 2, respectively.

Table 1. Composition of EPDM emulsion according to Example 1.

Composition (g) Composition (wt.%)

EPDM 47 1800 70.0 stearic acid 80 3.1

2-amino-2-methyl- 22 0.9

Ipropanolis water 670 26.0 acticide ® MBS 1.74 0.0

Table 2. Physical properties of EPDM emulsion according to Example 1. testing parameter testing method appearance visual creamy paste solids content (%) MT 74 mean particle size (pm) BC 1.1 pH (at 22.8°C) WTW 8.4

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 2

1800 g of EPDM polymer with a molecular weight of 47 kg/mol with ethylene/propylene ratio of 50/50 and dipentacyclopentadiene of 10 wt%, relative to the weight of the EPDM polymer, the EPDM polymer is loaded into a batch Z-plate kneader, set at a constant temperature of about 85°C and he mixer is stirred at 50 rpm. 80 g N-alkyl-tallow propylene diamine and 25 g acetic acid are added to heated EPDM polymer.

Subsequently, 1885 g of deionized water is added at equal incremental parts obtaining an EPDM emulsion characterised as low viscous liquid. The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 3 and Table 4, respectively.

Table 3. Composition of EPDM emulsion according to Example 2.

Composition (g) Composition (wt.%)

EPDM 47 1800 47.5

N-alkyl-tallow propylene 80 2.1 diamine acetic acid 25 0.7 water 1885 49.7

Table 4. Physical properties of PIB emulsion according to Example 2. testing parameter testing method appearance visual low viscous liquid solids content (%) MT 50 mean particle size (pm) BC 0.9 pH (at 22.8°C) WTW 5.5

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 3

1800 g of EPDM polymer with a molecular weight of 47 kg/mol with ethylene/propylene ratio of 50/50 and dipentacyclopentadiene of 10 wt%, relative to the weight of the EPDM polymer, is loaded into a batch Z-plate kneader, set at a constant temperature of about 85°C and the EPDM polymer is stirred at 50 rpm. 40 g ethoxylated caster oil (200 EO) and 40 g ethoxylated isostearyl alcohol (8 EO) is added.

Subsequently, 415 g of soft water is added at equal incremental parts obtaining an EPDM emulsion characterised as a creamy paste. The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 5 and Table 6, respectively.

Table 5. Composition of EPDM emulsion according to Example 3. Composition (g) Composition (wt.%)

EPDM 47 1800 78.4 ethoxylated caster oil 40 1.7 ethoxylated isostea ryl 40 1.7 alcohol water 415 18.1

Table 6. Physical properties of PIB emulsion according to Example 3. testing parameter testing method appearance visual creamy paste solids content (%) MT 82 mean particle size (pm) BC 1.5 pH (at 22.8°C) WTW 6.5

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 4

1800 g of EPDM polymer with a molecular weight of 39 kg/mol with ethylene/propylene ratio of 46/54 and ethylidene norbornene of 9.5 wt%, relative to the weight of the EPDM polymer, is loaded into a batch Z-plate kneader, set at a constant temperature of about 85°C and the EPDM polymer is stirred at 50 rpm. 80 g stearic acid and 22 g 2-amino-2methyl-l-propanol is added.

Subsequently, 530 g of soft water is added at equal incremental parts obtaining an EPDM emulsion characterised as a creamy paste. The final composition of the obtained EPDM emulsion its physical properties are reported in Table 7 and Table 8, respectively.

Table 7. Composition of EPDM emulsion according to Example 4.

Composition (g) Composition (wt.%)

EPDM 47 1800 74.0 stearic acid 80 3.3

2-amino-2methyl-l- 22 1.0 propanol Water 530 21.8

Table 8. Physical properties of EPDM emulsion according to Example 4. testing parameter testing method appearance visual creamy paste solids content (%) MT 78 mean particle size (pm) BC 1.2 pH (at 22.8°C) WTW 8.3

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 5

1800 g of EPDM polymer with a molecular weight of 23 kg/mol with ethylene/propylene ratio of 41/59 is loaded into a batch Z-plate kneader, set at a constant temperature of about 85°C and the EPDM polymer is stirred at 50 rpm. 80 g stearic acid and 22 g 2-amino-2methyl-l-propanol is added.

Subsequently, 634 g of soft water is added at equal incremental parts obtaining an EPDM emulsion characterised as a creamy paste. The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 9 and Table 10, respectively.

Table 9. Composition of EPDM emulsion according to Example 5.

Composition (g) Composition (wt.%)

EPDM 47 1800 7k0 stearic acid 80 3.2

2-amino-2methyl-l- 22 1.0 propanol

Water 634 25.0

Table 10. Physical properties of EPDM emulsion according to Example 5. testing parameter testing method appearance visual creamy paste solids content (%) MT 75 mean particle size (pm) BC 0.6 pH (at 22.8°C) WTW 8.5

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 6

1800 g of EPDM polymer with a molecular weight of 23 kg/mol with ethylene/propylene ratio of 41/59 is loaded into a batch Z-plate kneader, set at a constant temperature of about 80°C and the EPDM polymer is stirred at 50 rpm. 20 g stearic acid, 12 g 2-amino-2methyl-l-propanol, 60 g alkyl benzene sulfonic acid and 7 g ammonia is added to heated EPDM polymer.

Subsequently, 1260 g of deionized water is added at equal incremental parts obtaining an EPDM emulsion characterised as a high viscous liquid.

The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 11 and Table 12, respectively.

Table 11. Composition of EPDM emulsion according to Example 6.

Composition (g) Composition (wt.%)

EPDM 47 1800 57?0 stearic acid 20 0.6

2-amino-2methyl-l- 12 0.4 propanol alkyl benzene sulfonic 60 1.9 acid ammonia 7 0.2

Water 1260 39.9

Table 12. Physical properties of EPDM emulsion according to Example 6. testing parameter testing method appearance visual high viscous liquid solids content (%) MT 60 mean particle size (pm) BC 0.8 pH (at 22.8°C) WTW 8 5

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 7

1800 g of EPDM polymer with a molecular weight of 23 kg/mol with ethylene/propylene ratio of 41/59 is loaded into a batch Z-plate kneader, set at a constant temperature of about 85°C and the EPDM polymer is stirred at 50 rpm. 11 g stearic acid, 7 g 2-amino-2methyl-l-propanol, 33 g alkyl benzene sulfonic acid and 4 g ammonia is added to heated EPDM polymer.

Subsequently, 200 g of deionized water is added at equal incremental parts obtaining an EPDM emulsion characterised as a creamy paste. The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 13 and Table 14, respectively.

Table 13. Composition of EPDM emulsion according to Example 7.

Composition (g) Composition (wt.%)

EPDM 47 1800 87.6 stearic acid 11 0.5

2-amino-2methyl-l- 7 0.3 propanol alkyl benzene sulfonic 33 1.6 acid ammonia 4 0.2

Water 200 9.7

Table 14. Physical properties of EPDM emulsion according to Example 7. testing parameter testing method appearance visual creamy paste solids content (%) MT 84 mean particle size (pm) BC 1.5 pH (at 22.8°C) WTW 8.5

K (pS/cm)

MT = Mettler Toledo HR 73 halogen moisture analyser BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 8

750 g of EPDM polymer with a molecular weight of 23 kg/mol with ethylene/propylene ratio of 41/59 is loaded into a batch kitchen aid, set at a constant temperature of about 85°C and the EPDM polymer is stirred at 50 rpm. 33 g alkyl benzene sulfonic acid, 4.5 g potassium hydroxide is added to heated EPDM polymer.

The batch kitchen aid is capable of measuring torque of the mixing element in-line. After loading and heating the EPDM polymer the torque decreases while the surfactants alkyl benzene sulfonic acid and potassium hydroxide are mixed under low shear mixing. Water is dosed to the homogenous premix and the torque inverts (point of inversion) after 30 minutes and starts to increase with addition of further incremental steps of water to the homogenous premix. At a given moment the torque is double of the torque at the point of inversion and the heated EPDM polymer in water dispersion goes from a viscoelastic liquid to a viscoelastic solid and the torque decreases again to a stabilisation level after 90 minutes and is continuously stirred for 20 minutes. The time is measured from the first step of water dosages.

Subsequently, 650 g of soft water is added at equal incremental parts obtaining an EPDM emulsion characterised as a low viscous liquid. The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 15 and Table 16, respectively.

Table 15. Composition of EPDM emulsion according to Example 8.

Composition (g) Composition (wt.%)

EPDM 47 750 52.2 alkyl benzene sulfonic 33 2.3 acid potassium hydroxide 4.5 0.3

Water 650 45.2

Table 16. Physical properties of EPDM emulsion according to Example 8. testing parameter testing method appearance visual low viscous liquid solids content (%) MT 55 mean particle size (pm) BC 1.7 pH (at 22.8°C) WTW 10.2

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 9

4.75 g of EPDM polymer with a molecular weight of 8 kg/mol with ethylene/propylene ratio of 43/57 is loaded into a stationary mixing equipment, set at a constant temperature of about 85°C. 0.25 g alkyl benzene sulfonic acid, 0.05 g 2-amino-2-methyl-l-propanol is added to heated EPDM polymer.

The stationary mixing equipment is capable of measuring torque of the mixing element in-line. After loading and heating the EPDM polymer the torque remains stable while the surfactants alkyl benzene sulfonic acid and potassium hydroxide are mixed under low shear mixing. Water is dosed to the homogenous premix and the torque and starts to increase after 20 minutes with addition of further incremental steps of water to the homogenous premix. At a given moment the torque is one and a half of the torque of initial torque and the heated EPDM polymer in water dispersion goes from a viscoelastic liquid to a viscoelastic solid resulting in a decrease in the torque to a stabilisation level after 75 minutes. The time is measured from the first step of water dosages.

Subsequently, 0.7 g of soft water is added at equal incremental parts obtaining an EPDM emulsion characterised as a creamy paste. The final composition of the obtained EPDM emulsion and its physical properties are reported in Table 17 and Table 18, respectively.

Table 17. Composition of EPDM emulsion according to Example 9.

Composition (g) Composition (wt.%)

EPDM 47 4.75 82.6 alkyl benzene sulfonic 0.25 4.3 acid potassium hydroxide 0.05 0.9

Water 0.7 12.2

Table 18. Physical properties of EPDM emulsion according to Example 9. testing parameter testing method appearance visual creamy paste solids content (%) MT 88 mean particle size (pm) BC 2.3 pH (at 22.8°C) WTW 8.6

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 10

1800 g of EPDM polymer with a molecular weight of 47 kg/mol with ethylene/propylene ratio of 50/50 and dipentacyclopentadiene of 10 wt%, relative to the weight of the EPDM polymer, EPDM polymer is charged into a batch Z-plate kneader, set at a constant temperature of about 85°C and at a pressure of 1 bar. The EPDM polymer is stirred at 50 rpm and a surfactant solution of 70 g isostearic acid and 24 g morpholine is added.

Subsequently, water is added in equal increments to the homogenous premix until the solids content is 75 wt% at a rate of 15 ml water I minute. The mixture forms a EPDM emulsion and heating is switched off.

The final composition of the obtained EPDM emulsion is a creamy paste and its physical properties are reported in Table 19 and Table 20, respectively. As shown in table 20, the resulting EPDM emulsion has a high mean particle size.

Table 19. Composition of EPDM emulsion according to Example 10.

Composition (g) Composition (wt.%)

EPDM 47 1800 72.1

Isostearic acid 70 2.8

Morpholine 24 1.0 Water 600 24.0

Acticide ® MBS 1.0 0.0

Table 20. Physical properties of EPDM emulsion according to Example 10. testing parameter testing method appearance visual creamy paste solids content (%) MT 75.2 mean particle size (pm) BC 2.5 pH (at 22.8°C) WTW 8.5

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer

WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

EXAMPLE 11

900 g of the above EPDM emulsion in example 10 is charged into a batch Z-plate kneader, set at a constant temperature of about 85°C and at a pressure of 1 bar. The EPDM emulsion is stirred at 50 rpm. To this emulsion 2000 g of the EPDM polymer of the above EPDM emulsion in example 10 is added in increments of 200g. The resulting mixture has a solids content of 93%.

After the finale addition, the mixture is continuously stirred during 30 minutes. Subsequently, water is added in equal increments parts to the homogenous premix at an addition rate of 5 ml/minute until the solids content is 85% is reached. After a solids content of 85% is obtained, the addition rate of water is increased to 15 ml/min.

The final composition of the obtained EPDM emulsion is a creamy paste and its physical properties are reported in Table 21 and Table 22, respectively. These results show a clear decrease in the mean particle size of the obtained emulsion.

Table 21. Composition of EPDM emulsion according to Example 11.

Composition (g) Composition (wt.%)

EPDM emulsion of 900 25.2

EXAMPLE 10

EPDM 47 2000 56.0

Water 670 18.8 Acticide ® MBS 2.5

Table 22. Physical properties of EPDM emulsion according to Example 11. testing parameter testing method appearance visual Low viscous liquid solids content (%) MT 75 mean particle size (pm) BC 0.5 pH (at 22.8°C) WTW 8.1

MT = Mettler Toledo HR 73 halogen moisture analyser

BC = Beckman Coulter LS 13 3320 laser diffractometer WTW = WTW Inolab® pH 7110 with SenTix® 81 electrode

Claims

1. A solvent free method for making ethylene propylene diene (EPDM) terpolymer emulsion formulation, wherein the emulsion has a solid content equal to or greater than 50.0 wt.% as measured by thermogravimetric moisture analysis, and an average particle size less than 5 pm as measured by laser diffraction, the method comprising the steps of: heating the EPDM polymer, thereby obtaining heated EPDM polymer; adding one or more surfactants to the heated EPDM polymer under low shear mixing until a homogeneous premix is obtained; dosing water in parts under low shear mixing to the homogeneous premix, until a heated EPDM in water dispersion is obtained; and mixing of the heated EPDM in water dispersion, until an EPDM emulsion is obtained.

2. A solvent free method for making EPDM emulsion formulation according claim 1, comprising of the steps of: mixing an EPDM at low shear, wherein said low shear mixing occurs in mixing equipment operates at low shear whereby low shear is defined by operating at shear rates below 100 s-1.

3. A solvent free method for making EPDM emulsion formulation according to any of the preceding claims 1 or 2, comprising of the step of: heating an EPDM, wherein the temperature of heating ranges from 50°C to 100°C, more preferably between 80°C to 90°C.

4. A solvent free method for making EPDM emulsion formulation according to any of the preceding claims 1- 3, comprising of the step of: dosing parts of water, wherein said water is added to the homogeneous premix in incremental portions, whereby each incremental portion comprises less than 10 wt% relative to the weight of the homogeneous premix and each incremental portion of water is added successively to the previous after the dispersion of the previous incremental portion is homogeneously mixed, wherein the total amount of incremental portions added to the homogeneous premix is until the heated EPDM in water dispersion goes from viscoelastic liquid to a viscoelastic solid defined by an increase of at least 10% torque of a motor rotating mixing elements.

5. A solvent free method for making EPDM emulsion formulation according to any of the preceding claims 1 - 4, comprising of the step of: mixing of the heated EPDM in water dispersion until an EPDM emulsion is obtained, wherein said EPDM emulsion is defined as no further increase and stabilisation of torque of a motor rotating mixing elements.

6. A solvent free method for making EPDM emulsion formulation according to any of the preceding claims 1 - 5, the method comprising the step of : dosing water at a rate between 0.05 and 0.50 wt.% water per minute, relative to the weight of the homogeneous premix while the ratio of water to homogeneous premix by weight is lower than 15/85.

7. An EPDM emulsion comprising: an EPDM polymer dispersed in an aqueous phase, wherein the EPDM polymer comprises ethylene, propylene and optionally diene monomer units, wherein a ratio of ethylene/propylene units is between 40/60-85/15; and a surfactant, wherein the surfactant is selected from the list of: anionic surfactants, cationic surfactants, non-ionic surfactants and mixtures thereof; wherein the EPDM emulsion has an average particle size lower than 5 pm as measured by laser diffraction and a solids content greater than 50.0 wt% as measured by thermogravimetric moisture analysis.

8. An EPDM emulsion according to the preceding claim 7, wherein said EPDM polymer has a molecular weight between 5 - 75 kg/mol.

9. An EPDM emulsion according to any of the preceding claims 7 or 8, wherein said EPDM polymer has diene monomer units selected from the list of: methylidene norbornene, dicyclopentadiene, ethylidene norbornene, a 1.4-hexadiene, norbornadiene, vinyl norbornene or a combination thereof.

10. Kit suitable for waterproofing, the kit comprising: (a) an EPDM emulsion according to any one of claims 7 to 9; and

(b) a textile material; wherein the kit, the EPDM emulsion or the textile material comprises a curing agent.

11. Kit according to claim 10, wherein said textile material is impregnated with said curing agent.

12. Kit according to claim 10, wherein said EPDM emulsion comprises said curing agent, preferably said curing agent is water-dispersible.

13. Kit according to claim 10, wherein said kit comprises:

(c) a solvent-based or aqueous curing agent.

14. Kit according to any of claims 10-13, wherein said textile material is a nonwoven.

15. Kit according to any of claims 10-14, wherein said EPDM emulsion comprises uncured EPDM; preferably said uncured EPDM has a gel fraction below 20% after 48 hours in toluene at 20°C.