WO2008059309A1 - Nanocomposite flame retardant based on pvc and nanoclays - Google Patents
Nanocomposite flame retardant based on pvc and nanoclays Download PDFInfo
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- WO2008059309A1 WO2008059309A1 PCT/IB2006/003256 IB2006003256W WO2008059309A1 WO 2008059309 A1 WO2008059309 A1 WO 2008059309A1 IB 2006003256 W IB2006003256 W IB 2006003256W WO 2008059309 A1 WO2008059309 A1 WO 2008059309A1
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- WIPO (PCT)
- Prior art keywords
- flame retardant
- nanocomposite
- making
- nanoclay
- pvc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/44—Products obtained from layered base-exchange silicates by ion-exchange with organic compounds such as ammonium, phosphonium or sulfonium compounds or by intercalation of organic compounds, e.g. organoclay material
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
- C09K21/10—Organic materials containing nitrogen
Definitions
- the present invention relates to a process for making a nanocomposite flame retardant, in particular, of the type comprising particles of smectitic clays dispersed in a polymeric PVC matrix.
- a product largely used in the industry of cables for achieving good mechanical and chemical features, which is suitable for obtaining a high resistance against abrasion at low costs, is polyvinylchloride or PVC.
- PVC has some drawbacks that hamper its use as flame retardant.
- PVC degrades before melting.
- Such problem is traditionally faced using stabilizers based on lead, for removing the hydrochloric acid (HCl) formed during the reaction of "unzipping". More in detail, the stabilizers isolate the HCl produced by the dehydrohalogenation of PVC and block therefore the acceleration of the PVC thermal degradation.
- HCl hydrochloric acid
- Such stabilizers normally are capable of removing, in addition to HCl, also other basic or acid species that otherwise would accelerate the PVC degradation process.
- lead based compounds has a strong environmental impact.
- Other compounds provide the use of barium or cadmium salts.
- these compounds have certain drawbacks and, in particular, a high toxicity, in addition to high costs and not fully satisfactory performances.
- a technical field in a continuous evolution also concerning flame retardants is that of nanocomposites.
- nocomposites materials comprising in general a polymeric matrix in which particles of smectitic clays of nanometric size are dispersed, so-called nanoclays.
- the high dispersion rate allows to obtain a consistent improvement of the material features, and, in particular, of thermal stability and of resistance against flames.
- the latter feature is due to a reduced speed of thermal release during combustion and to a decrease of the temperature of fire ignition, i.e. a reduced speed of fire propagation.
- the resistance to flames is responsive to the production of on the surface of the material of a carbonaceous layer, so-called "char".
- This layer is very compact and therefore reduces the gaseous exchanges among comburent, i.e. oxygen, and combustible material.
- the carbonaceous layer is expected to act as a protective barrier, capable of reducing the heat and mass transfer between flames and polymer.
- reaction of a smectitic clay with an organic modifier obtaining an organophilic nanoclay
- the organophilic nanoclay removal of the excess of organic modifier not chemically bound to the organophilic nanoclay; — dispersion of the organophilic nanoclay in a matrix of polyvinylchloride (PVC) making a mixture of nanoclay flakes dispersed among the PVC molecules; whose main feature is that the organic modifier used is a salt of quaternary ammonium etoxylate in ethylenglycol comprising a [CH 2 -CH 2 ⁇ O] n iH group, where i is a number set between 1 and 4 and the summation of the ni gives an integer set between 1 and 100.
- PVC polyvinylchloride
- the nitrogen atom of the ammonium salt is less basic and then less adapted to bind the hydrogen atom of the polymer than the known organic modifiers. More in detail, the presence of the C-O bond shifts the nitrogen electrons on the oxygen and decreases, therefore, the basicity of the nitrogen same. This feature avoids the production of HCl and then the decomposition of polyvinylchloride.
- the salt of quaternary ammonium etoxylate may have the following structure formula (I) : [CH 2 CH 2 O] n1 H
- the summmation of the ni of the [CH 2 - CH 2 -O] ⁇ iH groups of the salt of quaternary ammonium etoxylate gives an integer set between 4 and 20.
- the sum of the ni of the [CH 2 -CH 2 -O] ni H groups of the salt of quaternary ammonium etoxylate gives an integer set between 7 and 10.
- a step is provided of addition of an inorganic additive flame retardant to the nanocomposite.
- the inorganic additive flame retardant is selected from the group comprised of:
- the combination of a nanoclay with an inorganic additive has a synergistic effect and provides a product with surprising flame retardant properties.
- the nanoclay is obtained starting from a smectitic clay selected from the group comprised of:
- the nanoclay is previously purified by the impurities embedded therein obtaining a purified nanoclay, in particular, the process for purification lowers the content of impurities less than 2% by weight, preferably less than 1% by weight.
- the nanocomposite is obtained by mixing:
- the nanocomposite comprises between 0 to 30 parts by weight of inorganic additive on 100 parts by weight of polymeric matrix.
- a measured amount of montmorillonite previously subject to an intense purification is caused to react in aqueous suspension with a salt of quaternary ammonium etoxylate having the following structure formula:
- a measured amount is added of PVC in a Hnesche mixer.
- the mixture is then heated up to a temperature of 65 0 C.
- dioctil phtalate is then added as plasticising agent and the whole is then heated up to about 105-110 0 C.
- the plasticising agent is used to coat the nanoclay and to inhibit further the reaction of unzipping the PVC. It acts as mechanical barrier between the nanoclay and the PVC.
- the nanocomposite thus obtained is put into the mixing chamber of a Brabender mixer and kept at 160 0 C for about 10 minutes.
- ammonium etoxylate salt has the following structure formula:
- ammonium etoxylate salt has the following structure formula:
- ammonium etoxylate salt used has [CH 2 -CH 2 -O] n H group and has the following features: activity 50.5%, density 1,059 g/cm 3 and mean molecular weight 410 g/mol .
- ammonium etoxylate salt has a [CH2-CH2-O] n H group, where n is 8.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Λ Process for making a nanocomposite flame retardant based on polyvinylchloride (PVC) and nanoclays obtained from a reaction of a smectitic clay with an organic modifier obtaining an organophilic nanoclay and by dispersing the organophilic nanoclay in a PVC matrix is disclosed. In particular, the organic modifier is a salt of quaternary ammonium ethoxylate in ethyleneglycol . The nanocomposite flame retardant, according to the invention, allows to exploit the good mechanical and chemical features of polyvinylchloride avoiding the drawbacks of the nanocomposite, in particular due to the reaction of 'unzipping' the PVC. The nanocomposite that is obtained has improved flame retardant properties and is cheap with respect to traditional flame retardants of prior art besides having comparable resistance to temperature and to flames.
Description
TITLE NANOCOMPOSITE FLAME RETARDANT BASED ON PVC AND NANOCLAYS
DESCRIPTION Field of the invention The present invention relates to a process for making a nanocomposite flame retardant, in particular, of the type comprising particles of smectitic clays dispersed in a polymeric PVC matrix.
Background of the invention As well known, many materials exist with flame retardant properties, for example for making lining protections for electric cables.
A product largely used in the industry of cables for achieving good mechanical and chemical features, which is suitable for obtaining a high resistance against abrasion at low costs, is polyvinylchloride or PVC.
However, PVC has some drawbacks that hamper its use as flame retardant. In particular, owing to a mechanism known as "autocatalytic dehydrohalogenation" or "unzipping" reaction, PVC degrades before melting.
Such problem is traditionally faced using stabilizers based on lead, for removing the hydrochloric acid (HCl) formed during the reaction of "unzipping". More in detail, the stabilizers isolate the HCl produced by the dehydrohalogenation of PVC and block therefore the acceleration of the PVC thermal degradation.
Furthermore, such stabilizers normally are capable of removing, in addition to HCl, also other basic or acid species that otherwise would accelerate the PVC degradation process.
The steadiness of the lead chlorides formed during the degradation process allows removing the HCl even at high
temperatures and in extreme conditions, and it offers then higher performances than other similar substances.
However, the use of lead based compounds has a strong environmental impact. Other compounds provide the use of barium or cadmium salts. Also these compounds have certain drawbacks and, in particular, a high toxicity, in addition to high costs and not fully satisfactory performances.
A technical field in a continuous evolution also concerning flame retardants is that of nanocomposites.
Among nocomposites materials are known comprising in general a polymeric matrix in which particles of smectitic clays of nanometric size are dispersed, so-called nanoclays. The high dispersion rate allows to obtain a consistent improvement of the material features, and, in particular, of thermal stability and of resistance against flames. The latter feature is due to a reduced speed of thermal release during combustion and to a decrease of the temperature of fire ignition, i.e. a reduced speed of fire propagation. The resistance to flames is responsive to the production of on the surface of the material of a carbonaceous layer, so-called "char". This layer is very compact and therefore reduces the gaseous exchanges among comburent, i.e. oxygen, and combustible material. The carbonaceous layer is expected to act as a protective barrier, capable of reducing the heat and mass transfer between flames and polymer.
Presently, the attempts to obtain nanocomposites comprising a polymeric matrix, i.e. a PVC matrix, that would give desirable advantages, have given unsatisfactory results. This is because PVC degrades after esfoliation owing to the "unzipping" reaction, above described.
Summary of the invention
It is therefore a feature of the present invention to provide a process for the production of a nanocomposite with flame retardant properties, in particular that can be used as coating for electric cables, that is cheap with respect to traditional flame retardants of prior art and with comparable resistance to temperature and to flames.
This and other features are accomplished with one exemplary process for the production of a nanocomposite flame retardant comprising the steps of:
— reaction of a smectitic clay with an organic modifier obtaining an organophilic nanoclay;
— removal of the excess of organic modifier not chemically bound to the organophilic nanoclay; — dispersion of the organophilic nanoclay in a matrix of polyvinylchloride (PVC) making a mixture of nanoclay flakes dispersed among the PVC molecules; whose main feature is that the organic modifier used is a salt of quaternary ammonium etoxylate in ethylenglycol comprising a [CH2-CH2~O]niH group, where i is a number set between 1 and 4 and the summation of the ni gives an integer set between 1 and 100.
In particular, in the above described organic modifier the nitrogen atom of the ammonium salt is less basic and then less adapted to bind the hydrogen atom of the polymer than the known organic modifiers. More in detail, the presence of the C-O bond shifts the nitrogen electrons on the oxygen and decreases, therefore, the basicity of the nitrogen same. This feature avoids the production of HCl and then the decomposition of polyvinylchloride.
In particular, the salt of quaternary ammonium etoxylate may have the following structure formula (I) :
[CH2CH2 O] n1 H
B NH -A
where A is selected from the group comprised of: H, CH3, [CH2-CH2-O]112H; B is selected from the group comprised of: H, CH3, [CH2-CH2-O] n3H; C is selected from the group comprised of: H, CH3, [CH2-CH2-O] n4H with n4.
Advantageously, the summmation of the ni of the [CH2- CH2-O] πiH groups of the salt of quaternary ammonium etoxylate gives an integer set between 4 and 20.
Preferably, the sum of the ni of the [CH2-CH2-O] niH groups of the salt of quaternary ammonium etoxylate gives an integer set between 7 and 10.
Advantageously, a step is provided of addition of an inorganic additive flame retardant to the nanocomposite.
In particular, the inorganic additive flame retardant is selected from the group comprised of:
— aluminum hydroxide;
— magnesium oxide; — magnesium hydroxide.
The combination of a nanoclay with an inorganic additive has a synergistic effect and provides a product with surprising flame retardant properties.
In particular, the nanoclay is obtained starting from a smectitic clay selected from the group comprised of:
— montmorillonite,
— hectorite,
— saponite.
Advantageously, the nanoclay is previously purified by the impurities embedded therein obtaining a purified nanoclay, in particular, the process for purification lowers the content of impurities less than 2% by weight, preferably less than 1% by weight.
Preferably, the nanocomposite is obtained by mixing:
— from 1 to 10 parts by weight of a nanoclay;
— 100 parts by weight of the polymeric PVC matrix. Preferably, the nanocomposite comprises between 0 to 30 parts by weight of inorganic additive on 100 parts by weight of polymeric matrix.
The following are examples of some possible methods of synthesis of a nanocomposite flame retardant, according to the present invention. EXAMPLE 1
A measured amount of montmorillonite previously subject to an intense purification is caused to react in aqueous suspension with a salt of quaternary ammonium etoxylate having the following structure formula:
[CH2CH2 O] 8H
CH3
To the organophilic nanoclay thus obtained a measured amount is added of PVC in a Hnesche mixer. The mixture is then heated up to a temperature of 650C. To the heated mixture dioctil phtalate is then added as plasticising agent and the whole is then heated up to about 105-1100C. The plasticising agent is used to coat the
nanoclay and to inhibit further the reaction of unzipping the PVC. It acts as mechanical barrier between the nanoclay and the PVC.
The nanocomposite thus obtained is put into the mixing chamber of a Brabender mixer and kept at 1600C for about 10 minutes.
EXAMPLE 2
Following the steps of example 1 with the difference that the used ammonium etoxylate salt has the following structure formula:
[CH2CH2 O] 4H
[CH2CH2 O] 4 H
EXAMPLE 3
Following the steps of example 1 with the difference that the used ammonium etoxylate salt has the following structure formula:
[CH2CH2 O] 3 H
H N+ [CH2CH2 O] 3 H
[CH2CH2 O] 3 H
EXAMPLE 4
Following the steps of example 1 with the difference that the ammonium etoxylate salt used has [CH2-CH2-O]nH group and has the following features: activity 50.5%, density 1,059 g/cm3 and mean molecular weight 410 g/mol .
EXAMPLE 5
Following the steps of example 1 with the difference that the used ammonium etoxylate salt has a [CH2-CH2-O] nH group, where n is 8.
EXAMPLE 6
Following the steps of example 1 with the difference that the used ammonium etoxylate salt has a [CH2-CH2-O]nH group where n is 9. The foregoing description of a specific embodiment will so fully reveal the invention according to the conceptual point of view, so that others, by applying current knowledge, will be able to modify and/or adapt for various applications such an embodiment without further research and without parting from the invention, and it is therefore to be understood that such adaptations and modifications will have to be considered as equivalent to the specific embodiment. The means and the materials to realise the different functions described herein could have a different nature without, for this reason, departing from the field of the invention. It is to be understood that the phraseology or terminology employed
herein is for the purpose of description and not of limitation.
Claims
1. Process for making a nanocomposite flame retardant comprising the steps of:
— reaction of a smectitic clay with an organic modifier obtaining an organophilic nanoclay;
— removal of the excess of said organic modifier not chemically bound to said organophilic nanoclay;
— dispersion of said organophilic nanoclay in a matrix of polyvinylchloride (PVC) making a mixture of nanoclay flakes dispersed among the PVC molecules; characterised in that said organic modifier is a salt of quaternary ammonium etoxylate in ethylenglycol comprising a [CH2-CH2-O] nχH group, where i is a number set between 1 and 4 and the summation of the ni gives an integer set between 1 and 100.
2. Process for making a nanocomposite flame retardant, according to claim 1, wherein said salt of quaternary ammonium etoxylate has the following structure formula
(I):
[CH2CH2 O] n1H
B -N4 -A
Where A is selected from the group comprised of: H, CH3, [CH2-CH2-O]n2H; B is selected from the group comprised of: H, CH3, [CH2-CH2-O]113H; C is selected from the group comprised of: H, CH3, [CH2-CH2-OIn4H.
3. Process for making a nanocomposite flame retardant, according to claim 1, wherein said summation of the ni of said [CH2-CH2-O] niH group gives an integer set between 4 and 20.
4. Process for making a nanocomposite flame retardant, according to claim 1, wherein said summation of the ni of said [CH2-CH2-O] niH group gives an integer set between 7 and 10.
5. Process for making a nanocomposite flame retardant, according to claim 1, where it is provided furthermore, a step of addition of an inorganic additive flame retardant to said nanocomposite.
6. Process for making a nanocomposite flame retardant, according to claim 5, wherein said inorganic additive flame retardant is selected from the group comprised of:
— aluminum hydroxide;
— magnesium oxide; — magnesium hydroxide.
7. Process for making a nanocomposite flame retardant, according to claim 1, wherein said smectitic clay is selected from the group comprised of:
— montmorillonite, — hectorite,
— saponite.
8. Process for making a nanocomposite flame retardant, according to claim 1, wherein said nanoclay is previously subject to a step of purification from the impurities embedded therein obtaining a purified nanoclay.
9. Process for making a nanocomposite flame retardant, according to claim 8, wherein said step of purification reduces the content of impurities to a value less than 2% by weight, preferably less than 1% by weight .
10. Process for making a nanocomposite flame retardant, according to claim 1, wherein said nanocomposite is obtained by mixing: — from 1 to 10 parts by weight of a nanoclay; —- 100 parts by weight of polymeric PVC matrix.
11. Process for making a nanocomposite flame retardant, according to claim 1, wherein said nanocomposite comprises between 0 to 30 parts by weight of an inorganic additive on 100 parts by weight of polymeric PVC matrix.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/IB2006/003256 WO2008059309A1 (en) | 2006-11-17 | 2006-11-17 | Nanocomposite flame retardant based on pvc and nanoclays |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/IB2006/003256 WO2008059309A1 (en) | 2006-11-17 | 2006-11-17 | Nanocomposite flame retardant based on pvc and nanoclays |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2008059309A1 true WO2008059309A1 (en) | 2008-05-22 |
Family
ID=38006986
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IB2006/003256 Ceased WO2008059309A1 (en) | 2006-11-17 | 2006-11-17 | Nanocomposite flame retardant based on pvc and nanoclays |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2008059309A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2456693C1 (en) * | 2011-05-10 | 2012-07-20 | Закрытое акционерное общество "Кабельный завод "Кавказкабель" | Electrically insulating composition |
| RU2469055C1 (en) * | 2011-05-17 | 2012-12-10 | Закрытое акционерное общество "Кабельный завод "Кавказкабель" | Electrically insulating composition |
| WO2014184429A1 (en) | 2013-05-13 | 2014-11-20 | Teknologian Tutkimuskeskus Vtt | Flame resistant thermoplastic composite |
| CN106633520A (en) * | 2016-12-20 | 2017-05-10 | 新疆嘉锋新型建材开发有限公司 | High-strength impact-resistant weather-resistant PVC building board and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4105717A (en) * | 1976-05-18 | 1978-08-08 | Armstrong Cork Company | Nailable vinyl chloride-based injection-molding compound |
| WO2000034180A1 (en) * | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | A polymer/clay nanocomposite having improved gas barrier comprising a clay material with a mixture of two or more organic cations and a process for preparing same |
| WO2000066657A1 (en) * | 1999-04-30 | 2000-11-09 | Alcan International Limited | Fire retardant compositions |
| WO2003002651A1 (en) * | 2001-06-29 | 2003-01-09 | Ciba Specialty Chemicals Holding Inc. | Synergistic combinations of nano-scaled fillers and hindered amine light stabilizers |
| US20040106720A1 (en) * | 2001-04-06 | 2004-06-03 | Robert Jerome | Nanocomposite polyster preparation method |
| WO2004063268A1 (en) * | 2003-01-15 | 2004-07-29 | Ciba Specialty Chemicals Holding Inc. | Stabilization of thermoplastic nanocomposites |
| US6919392B1 (en) * | 1978-08-29 | 2005-07-19 | Arkema Inc. | Stabilization of vinyl halide polymers |
| EP1645590A1 (en) * | 2004-10-06 | 2006-04-12 | Laviosa Chimica Mineraria S.p.A. | Process for making a flameproof composition |
-
2006
- 2006-11-17 WO PCT/IB2006/003256 patent/WO2008059309A1/en not_active Ceased
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4105717A (en) * | 1976-05-18 | 1978-08-08 | Armstrong Cork Company | Nailable vinyl chloride-based injection-molding compound |
| US6919392B1 (en) * | 1978-08-29 | 2005-07-19 | Arkema Inc. | Stabilization of vinyl halide polymers |
| WO2000034180A1 (en) * | 1998-12-07 | 2000-06-15 | Eastman Chemical Company | A polymer/clay nanocomposite having improved gas barrier comprising a clay material with a mixture of two or more organic cations and a process for preparing same |
| WO2000066657A1 (en) * | 1999-04-30 | 2000-11-09 | Alcan International Limited | Fire retardant compositions |
| US20040106720A1 (en) * | 2001-04-06 | 2004-06-03 | Robert Jerome | Nanocomposite polyster preparation method |
| WO2003002651A1 (en) * | 2001-06-29 | 2003-01-09 | Ciba Specialty Chemicals Holding Inc. | Synergistic combinations of nano-scaled fillers and hindered amine light stabilizers |
| WO2004063268A1 (en) * | 2003-01-15 | 2004-07-29 | Ciba Specialty Chemicals Holding Inc. | Stabilization of thermoplastic nanocomposites |
| EP1645590A1 (en) * | 2004-10-06 | 2006-04-12 | Laviosa Chimica Mineraria S.p.A. | Process for making a flameproof composition |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2456693C1 (en) * | 2011-05-10 | 2012-07-20 | Закрытое акционерное общество "Кабельный завод "Кавказкабель" | Electrically insulating composition |
| RU2469055C1 (en) * | 2011-05-17 | 2012-12-10 | Закрытое акционерное общество "Кабельный завод "Кавказкабель" | Electrically insulating composition |
| WO2014184429A1 (en) | 2013-05-13 | 2014-11-20 | Teknologian Tutkimuskeskus Vtt | Flame resistant thermoplastic composite |
| CN106633520A (en) * | 2016-12-20 | 2017-05-10 | 新疆嘉锋新型建材开发有限公司 | High-strength impact-resistant weather-resistant PVC building board and preparation method thereof |
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