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Method for producing spherial polysilsesquioxane particles

A technology of polysilsesquioxane and granules, which is used in pharmaceutical formulations, preparations for skin care, medical preparations containing active ingredients, etc., can solve the problems of loss of materials, methods of not reporting the agglomeration properties of granules, etc. Material loss reduction effect

Active Publication Date: 2018-11-09
WACKER CHEM GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This means further loss of material and additionally protective measures must be taken to protect co-workers from non-toxic but very finely divided dust-like material
Further loss of material in mills due to harsher conditions through attrition or broken particles
[0004] No method has been reported to allow control of the agglomeration properties of the particles

Method used

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  • Method for producing spherial polysilsesquioxane particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] 1328 grams of demineralized water with a conductivity of 0.1 μS / cm was initially charged into a glass flask, and the temperature was controlled to 20°C. The contents of the flask were stirred at 300 rpm. The pH was adjusted to a value of 4.40 by adding 0.1 M hydrochloric acid. 291.6 g of methyltrimethoxysilane were metered in over 1 hour and the temperature was kept at 20°C. After the metered addition had ceased, the contents of the flask were stirred at 20° C. for 1 hour. Add 65.49 grams of 0.1 molar KOH in methanol over 1 minute at 20°C and mix for a total of 3 minutes to form a homogeneous mixture. Then turn off the mixer. After 21 hours, the precipitated particles were filtered off, washed with DM water and redispersed with DM water to give a 15% suspension. The suspension was then dried using a Niro Mobile Minor laboratory spray dryer at an inlet temperature of 260° C. and an outlet temperature of 155 to 160° C. using nitrogen as drying gas.

Embodiment 2

[0080] This example was carried out according to the method of Example 1, except that 85.14 grams of 0.1 molar KOH methanol solution was added to cause precipitation.

Embodiment 3

[0082] This example was carried out according to the method of example 1, except that 7.96 g of 1 molar ammonia solution was added to cause precipitation.

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Abstract

The invention relates to a method for producing spherial polysilsesquioxane particles, in which: in a first step, trialkoxysilane of general formula (I) RSiOR1 3 (I), where R is a hydrocarbon radicalwith between 1 and 16 carbon atoms, the carbon chain thereof being able to be broken by non-adjacent groups -O-, and R1 is a C1- to C4 alkoxy radical, is reacted with acidified water having a maximumpH value of 6, and mixed to form a hydrolysate; in a second step, the hydrolysate is mixed with a solution of a base in water or C1- to C4-alkanol; in a third step, the mixture is stored for at least2 hours; and in a fourth step, the polysilsesquioxane particles are spray-dried. The invention also relates to the polysilsesquioxane particles that can be produced according to said method.

Description

technical field [0001] The present invention relates to a process for the production of spherical polysilsesquioxane particles by hydrolysis of trialkoxysilanes, condensation of hydrolyzed products and spray drying of the particles, and also to polysilsesquioxane particles. Background technique [0002] The prior art, eg JP3970449B2, JPH06248081A and JPH0488023A, discloses different methods of producing spherical polymethylsilsesquioxane particles. JP3970449B2 describes optimization of space-time yield and control of particle size. Drying causes the particles to melt and form a network structure. The fused granules obtained are conveniently subsequently ground to provide a powdered product. [0003] The expensive and laborious processing steps required for grinding are disadvantageous. After drying, the very loose and dusty polysilsesquioxane granules first have to be dispensed. This means loss of material and cleaning costs for the dispensing equipment. The material mu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/06C08G77/08A61K8/89A61K8/891C08G77/18
CPCA61K8/891C08G77/045A61Q19/00A61K8/025A61K2800/10C08G77/06C08J3/122C08G77/32C08G77/70
Inventor S·克内尔
Owner WACKER CHEM GMBH
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