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WO2025201605A1 - Procédé de séchage - Google Patents

Procédé de séchage

Info

Publication number
WO2025201605A1
WO2025201605A1 PCT/DE2025/100308 DE2025100308W WO2025201605A1 WO 2025201605 A1 WO2025201605 A1 WO 2025201605A1 DE 2025100308 W DE2025100308 W DE 2025100308W WO 2025201605 A1 WO2025201605 A1 WO 2025201605A1
Authority
WO
WIPO (PCT)
Prior art keywords
salts
alkyl polyglycosides
iminodisuccinic acid
drying process
bed reactor
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.)
Pending
Application number
PCT/DE2025/100308
Other languages
German (de)
English (en)
Inventor
Olga IWANOW
Christian FUCHS-RICHERT
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Inprotec GmbH
Original Assignee
Inprotec GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Inprotec GmbH filed Critical Inprotec GmbH
Publication of WO2025201605A1 publication Critical patent/WO2025201605A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/662—Carbohydrates or derivatives
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2082—Polycarboxylic acids-salts thereof

Definitions

  • the invention relates to a drying process, in particular a spray-drying process for producing a pourable mixture comprising alkyl polyglycosides and salts of iminodisuccinic acid, and to the pourable mixture obtained therefrom.
  • a pourable mixture comprising alkyl polyglycosides and salts of iminodisuccinic acid is of interest because the two substances are biodegradable, well tolerated by humans and can be used in a variety of everyday products, such as detergents and dishwashing detergents, hand soaps and cosmetic products.
  • anhydrous cosmetics especially foaming products certified according to the international COSMOS standard and with a high naturalness index
  • foaming products reduce water consumption and require less packaging, thus addressing environmental concerns and the trend toward "zero waste.”
  • higher concentration offers greater efficacy and better value for money.
  • Anhydrous cosmetics also make it possible to eliminate preservatives from the formulations. These can can cause skin sensitization or even trigger allergies. Preservatives are also responsible for imbalances in the skin's microbiome and disruption of the dermis's protective barrier.
  • a process for producing a powder or granulate which comprises at least one chelating agent selected from the alkali metal salts of methylglycinediacetic acid (MGDA), glutamic acid diacetate (GLDA), and iminodisuccinic acid (IDS), and at least one enzyme in a weight ratio of 5:1 to 1,000:1.
  • the powder or granulate contains at least 75% by weight of chelating agent (A), the process comprising the following steps:
  • WO 2020/104231 A1 discloses neither a pourable mixture comprising alkyl polyglycosides and salts of iminodisuccinic acid nor a process for its preparation.
  • the applicant has surprisingly found that low drying temperatures are required for optimal drying to obtain a pourable mixture comprising alkyl polyglycosides and salts of iminodisuccinic acid This is surprising because, as the temperature increases and the associated faster drying process when the substances to be dried, which are preferably in liquid form, are introduced or sprayed into the fluidized bed reactor, smaller particles are usually obtained. However, the applicant was unable to observe this when alkyl polyglycosides and salts of iminodisuccinic acid were introduced. Rather, the applicant found that larger particles are formed as the temperature increases. The applicant suspects that this is due to increased agglomeration during drying, with the agglomeration probably occurring due to the chemical properties of the alkyl polyglycosides.
  • the proportion of alkyl polyglycosides is greater than the proportion of iminodisuccinic acid salts.
  • the higher proportion of alkyl polyglycosides results in improved particle formation. It is assumed that this is due to micelle formation of the alkyl polyglycosides. Ratios of 7:3 to 9:1 have proven particularly advantageous.
  • the proportion of Alkyl polyglycosides and salts of iminodisuccinic acid are present in a ratio of 8:2 and 4:1, respectively. This mixing ratio of the pourable mixture exhibits lower hygroscopic properties than other ratios.
  • a further alternative is to introduce the alkyl polyglycosides and the salts of iminodisuccinic acid in a common liquid phase and, in addition, alkyl polyglycosides in a separate liquid phase and/or salts of iminodisuccinic acid in a separate liquid phase.
  • the fluidized bed reactor is operated with spatially offset zones, wherein these zones have different temperature levels. This is also referred to as a multi-zone process.
  • the combined liquid phase of the alkyl polyglycosides and the iminodisuccinic acid salts is introduced into a first zone of this type, which has a first temperature level.
  • the separate liquid phase of the iminodisuccinic acid salts is introduced into a second zone of this type of the fluidized bed reactor, wherein this second zone has a second temperature level.
  • the first temperature level may differ from the second temperature level.
  • a nucleating agent is introduced into the fluidized-bed reaction.
  • a nucleating agent is a compound that promotes or initiates crystallization. These compounds serve, in particular, to provide nucleation sites right at the beginning of the process, promote crystal formation, adjust and refine the size of the growing crystals, and prevent the forming particles from agglomerating. and clumping, as well as influencing the rate of crystallization and the formation of specific crystal phases.
  • Examples of nucleating agents are SiO2, Na2SO4, CaCO3, TiC, Al2O3, Fe2O3, Ba2SO4, and MgO.
  • the invention provides for the process in a further advantageous embodiment that the pourable mixture is cooled to room temperature.
  • the alkyl polyglycosides of the pourable mixture have an alkyl chain with 4 to 12 carbon atoms.
  • the pourable mixture is detergent, solubilizing, non-foaming, and sequestering.
  • Detergent refers to the property of separating and cleaning impurities.
  • Solubilizing refers to the property of dissolving impurities and dirt or making them more soluble.
  • non-foaming refers to the property of preventing the formation of foam.
  • the term “sequestering” refers to the property of a compound forming complexes with metal ions and thus reducing their availability in the solution. This prevents metal ions from reacting or forming complexes with other compounds present, thereby improving the cleaning effect and stability of the pourable mixture and preventing a deterioration in the physicochemical properties of the pourable mixture.
  • the particles have a surface roughness between 7 and 9 pm.
  • Surface roughness refers to the morphological property of the pourable mixture. It quantifies the distance between the peaks and valleys present on the surface of the particles. It refers to a characteristic depth of the grooves or irregularities that run through the surface of the particles.
  • the surface roughness of the pourable mixture can be measured, for example, using a VK-X160K confocal 3D laser scanning microscope from Keyence.
  • the pourable mixture can have a wet dissolution time of between 245 and 255 seconds for a mass of 20 g of pourable mixture in 200 ml of water.
  • 'Dissolution' refers to the transition from the solid phase of the pourable mixture to the aqueous phase.
  • the wet dissolution time can be measured by adding 20 g of granules to 200 ml of water while stirring with a bar magnet at 21 °C.
  • the water activity of a pourable mixture can be determined using a water activity counter AQUALab 3 TE from Decagon Devices.
  • it has a flow function in the range of 63 to 73, particularly 68.
  • the term "flow function,” also referred to as ffc, refers to the flow function of a bulk material and is the ratio between the maximum principal stress, o1 , that the bulk material can experience without changing its consolidation, and the maximum stress, f c , that the bulk material can bear on a free surface developed for this consolidation state. It is calculated using the formula:
  • a flow function of 10 or more is considered free.
  • the pourable mixture exhibits free flow. "Free flow” means that the particles can flow relatively easily and without significant resistance. The pourable mixture thus possesses easy mobility.
  • the flow function can be determined, for example, using a Ring Shear Tester RST-XS.s from Dietmar Schulze®.
  • the pourable mixture has a specific surface area between 3 and 9 m2 /kg.
  • “Specific surface area” is a measure of the total surface area of the particles per unit mass.
  • the specific surface area of a pourable mixture can be measured using a Mastersizer 3000 granulometer from Malvern Panalytical, which is equipped with an air pressure dispersion module.
  • tamped density 700 to 715 kg/m3, in particular 712 kg/m3, the tamped density being measured using a Ring Shear Tester RST-XS.s from Dr. Dietmar Schulze GmbH ®.
  • the pourable mixture has an elemental composition comprising:
  • the term "elemental composition” refers to the quantitative determination of the chemical elements composing the pourable mixture. Silicon may be present in the elemental composition of the pourable mixture if a nucleating agent (SiO2) has been introduced into the pourable mixture in an amount of less than 5 wt.% to initiate crystallization.
  • a nucleating agent SiO2
  • the elemental composition of a granule population can be determined using energy dispersive X-ray spectroscopy using a Zeiss Supra 55 VP microscope.
  • the invention provides for the use of the pourable mixture obtained from the process according to the invention for the production of detergents, soaps and/or cosmetic products.
  • AC 2000 Coco Source (batch: 230515ACO4B; quantity: 1100 kg; solid content: 50.9 wt.%) and Baypure CX 100 (batch: CHASME2128; quantity: 250 kg; solid content: 34 wt.%) were used as starting materials.
  • Examples 1 to 3 were carried out in an AGT 400 fluidized-bed spray granulator.
  • Example 4 was carried out in a GF25 fluidized-bed spray granulator.
  • the systems are equipped with a fluidized-bed reactor, a filter house with PES filter cloth, a wet scrubber, a tumbler screen (200 pm/1000 pm), a Retsch mill (750 pm), and a Verderflex Smart B40 peristaltic feed pump (10 mm).
  • Baypure CX 100 was introduced into the system as a carrier at 20 wt.% based on the dry mass through a 500 ⁇ m sieve, resulting in a fluidized bed mass of approximately 6 mbar.
  • the addition of 80 wt.% alkyl polyglycosides based on the dry mass was carried out at 47°C at a very slow feed rate of approximately 200 g/min. After two hours, unloading began (approximately 5 mbar), and a final product yield of 15.5 kg was achieved. The residual moisture content in the final product was 5.13%.
  • the granules were stable and had good flowability. Microscopic analysis revealed almost transparent, round particles with a recognizable white core, see Figure 1 .
  • the discharged granules were sieved to 500–1000 ⁇ m. The coarse and fine fractions of the fluidized bed were continuously separated and recycled via a cyclone, in this case a Retsch mill, during spray drying.
  • Example 2 Preparation of a pourable mixture comprising alkyl polyglycosides and salts of iminodisuccinic acid from a liquid mixture comprising alkyl polyglycosides and salts of iminodisuccinic acid in a ratio of 4:1
  • the spray drying described below was carried out under the process conditions listed below:
  • a liquid batch of 20.0 kg (10.1 kg solid) AC 2000 with 7.3 kg (2.5 kg solid) Baypure CX 100 was formed, heated to 60°C, and sprayed into the fluidized bed reactor with moderate stirring.
  • the spray granulation proceeded stably at low drying temperatures and with continuous recirculation of the coarse and fine fractions using a Retsch mill to stabilize the bed mass and increase the drying surface for granulation.
  • a liquid batch of 20.0 kg (10.1 kg solid) AC 2000 with 3.24 kg (1.1 kg solid) Baypure CX 100 was formed, heated to 60°C, and sprayed into the fluidized bed reactor with moderate stirring.
  • the spray granulation proceeded stably at low drying temperatures and with continuous recirculation of the coarse and fine fractions using a Retsch mill to stabilize the bed mass and increase the drying surface for granulation.
  • the areas or zones 1/2 and 3 of the fluidized bed reactor have different temperatures.
  • a liquid mixture of 20.0 kg (10.1 kg solid) AC 2000 and 3.24 kg (1.1 kg solid) Baypure CX 100 was formed, heated to 60°C, and sprayed into the front section of a horizontal fluidized bed reactor (chamber 1/2) with moderate stirring.
  • the separately prepared solution of Baypure CX 100 (42% dry matter, 1.4 kg solid) was fed separately into the middle section of the fluidized bed reactor at a feed temperature of 60°C, thus combining co-granulation and coating in a multi-stage process to achieve a final granulate ratio of 4:1 APG:IDS.
  • the spray granulation was stable at low drying temperatures and with continuous recirculation of the coarse and fine fractions to the front area of the fluidized bed reactor (zone 1) by means of a Retsch mill to stabilize the bed mass and enlarge the drying surface for granulation.
  • the finished granules exhibited good flow properties, but were cooled to room temperature before filling into the final packaging to prevent agglomeration or blocking.
  • a final product yield of 36.0 kg and a fine fraction of 12.0 kg were achieved.
  • Figure 4 shows the microscopic analysis of the resulting particles.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Emergency Medicine (AREA)
  • Molecular Biology (AREA)
  • Detergent Compositions (AREA)

Abstract

L'invention concerne un procédé de séchage, en particulier un procédé de séchage par pulvérisation, pour produire un mélange fluide comprenant des alkylpolyglycosides et des sels d'acide iminodisuccinique, et un mélange fluide obtenu à partir de celui-ci. Les alkylpolyglycosides et les sels d'acide iminodisuccinique sont biodégradables, bien tolérés par l'homme et peuvent être utilisés dans un grand nombre de produits quotidiens, par exemple des détergents et des liquides vaisselle, des savons à main et des produits cosmétiques. Le problème à résoudre par la présente invention est donc de fournir un procédé de séchage par pulvérisation au moyen duquel un mélange fluide d'alkylpolyglycosides et de sels d'acide iminodisuccinique peut être produit. La solution selon l'invention porte sur un procédé comprenant les étapes suivantes consistant à : fournir un réacteur à lit fluidisé, introduire des alkylpolyglycosides et des sels d'acide iminodisuccinique dans le réacteur à lit fluidisé, la proportion d'alkylpolyglycosides étant au moins égale à la proportion de sels d'acide iminodisuccinique, et sécher et/ou agglomérer les alkylpolyglycosides et les sels d'acide iminodisuccinique dans le réacteur à lit fluidisé à des températures allant jusqu'à 150 °C, de préférence jusqu'à 50 °C.
PCT/DE2025/100308 2024-03-28 2025-03-25 Procédé de séchage Pending WO2025201605A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102024109023.5A DE102024109023A1 (de) 2024-03-28 2024-03-28 Trocknungsverfahren
DE102024109023.5 2024-03-28

Publications (1)

Publication Number Publication Date
WO2025201605A1 true WO2025201605A1 (fr) 2025-10-02

Family

ID=95558862

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE2025/100308 Pending WO2025201605A1 (fr) 2024-03-28 2025-03-25 Procédé de séchage

Country Status (2)

Country Link
DE (1) DE102024109023A1 (fr)
WO (1) WO2025201605A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19702845A1 (de) * 1997-01-27 1998-07-30 Henkel Kgaa Verfahren zur Herstellung von Tensidgranulaten
WO2005023975A1 (fr) 2003-09-03 2005-03-17 Henkel Kommanditgesellschaft Auf Aktien Agent cosmetique a phases multiples pour laver les cheveux et nettoyer la peau
CN107325891A (zh) * 2017-06-16 2017-11-07 中原工学院 一种特效去除重金属的全天然绿色果蔬洗涤盐
WO2020104231A1 (fr) 2018-11-19 2020-05-28 Basf Se Poudres et granulés contenant un agent chélatant et une enzyme

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4209339A1 (de) * 1992-03-23 1993-09-30 Henkel Kgaa Verfahren zur Herstellung rieselfähiger Wasch- und Reinigungsmittelgranulate und/oder -teilgranulate
JP4175674B2 (ja) * 1995-08-11 2008-11-05 株式会社日本触媒 粉末およびその製造方法、ならびに該粉末を含む粒状洗剤組成物
PL4073217T3 (pl) * 2019-12-11 2024-11-18 Basf Se Granulki mgda i homo- lub kopolimer kwasu (met)akrylowego; sposób ich wytwarzania

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19702845A1 (de) * 1997-01-27 1998-07-30 Henkel Kgaa Verfahren zur Herstellung von Tensidgranulaten
WO2005023975A1 (fr) 2003-09-03 2005-03-17 Henkel Kommanditgesellschaft Auf Aktien Agent cosmetique a phases multiples pour laver les cheveux et nettoyer la peau
CN107325891A (zh) * 2017-06-16 2017-11-07 中原工学院 一种特效去除重金属的全天然绿色果蔬洗涤盐
WO2020104231A1 (fr) 2018-11-19 2020-05-28 Basf Se Poudres et granulés contenant un agent chélatant et une enzyme

Also Published As

Publication number Publication date
DE102024109023A1 (de) 2025-10-02

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