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Preparation method of isooctyltriethoxysilane oligomer

A technology of isooctyltriethoxysilane and oligomers, which is applied in the field of preparation of isooctyltriethoxysilane oligomers, can solve the problem of difficulty in controlling the reaction process, affecting product application effects, uneven molecular weight distribution, etc. problems, to achieve low production costs, good storage stability, and long service life

Inactive Publication Date: 2021-07-09
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acid-catalyzed method is usually to add hydrochloric acid to catalyze the hydrolysis reaction of silane, and free chlorine will inevitably be introduced during the preparation process, which will affect the application effect of the product; while the base-catalyzed method is usually to add inorganic bases such as sodium hydroxide and sodium carbonate or tetramethyl hydroxide Ammonium and other organic bases are used as catalysts, but under alkaline conditions, the hydrolysis rate of silane is faster, and the polycondensation and hydrolysis are carried out at the same time. The reaction process is difficult to control, which can easily lead to excessive polycondensation of the product and uneven molecular weight distribution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 500 g of isooctyltriethoxysilane, 20 g of ethanol, styrene divinylbenzene, Take 2g of sulfonic acid resin, weigh 55g of deionized water and add it to the dropping funnel to wait for dropwise addition. Turn on the stirring and oil bath heating device, and when the temperature of the system rises to 62°C, start to add deionized water slowly and uniformly, and the dropping time is controlled at 1.5h; after the dropwise addition, control the reaction temperature at 78~80°C, and continue aging 6h, make the deionized water in the system react completely; then gradually raise the temperature of the system to 100°C, distill out the ethanol in the system under normal pressure, until no more material is discharged, under the condition of vacuum degree of 0 to -0.09MPa , and continue to distill off the residual ethanol under reduced pressure to obtain the crude product of isooctyltriethoxysilane oligomer. After the material was cooled, the styrene divinylbenzenesulfonic acid ...

Embodiment 2

[0024] Into a 2000mL four-necked flask equipped with mechanical stirring, a spherical condenser (passing cooling water), a thermometer, and a constant pressure dropping funnel, 1000g of isooctyltriethoxysilane, 48g of ethanol, and styrene divinylbenzene were sequentially added. 3.5g of sulfonic acid resin, weighed 110g of deionized water and added to the dropping funnel to wait for dropwise addition. Turn on the stirring and oil bath heating device, and when the temperature of the system rises to 62°C, start to add deionized water slowly and uniformly, and the dropping time is controlled at 1.5h; after the dropwise addition, control the reaction temperature at 78~80°C, and continue aging 6h, make the deionized water in the system react completely; then gradually raise the temperature of the system to 100°C, distill out the ethanol in the system under normal pressure, until no more material is discharged, under the condition of vacuum degree of 0 to -0.09MPa , and continue to d...

Embodiment 3

[0026] Add 1000 g of isooctyltriethoxysilane, 48 g of isopropanol, and styrene divinyl to a 2000 mL four-neck flask equipped with mechanical stirring, a spherical condenser (through cooling circulating water), a thermometer, and a constant pressure dropping funnel. Base benzene sulfonic acid resin 4g, weigh 118g deionized water and join in the dropping funnel and wait for dropping. Turn on the stirring and oil bath heating device, and when the temperature of the system rises to 62°C, start to add deionized water slowly and uniformly, and the dropping time is controlled at 1.5h; after the dropwise addition, control the reaction temperature at 78~80°C, and continue aging 6h, make the deionized water in the system react completely; then gradually raise the temperature of the system to 100°C, distill out the ethanol and isopropanol in the system at normal pressure until no more materials are discharged, then the vacuum degree is from 0 to - Under the condition of 0.09MPa, continue...

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Abstract

The invention relates to a preparation method of an isooctyltriethoxysilane oligomer, and belongs to the field of fine chemical engineering. The preparation method comprises the following steps: by taking isooctyltriethoxysilane and deionized water as raw materials, alcohol as a solvent and ion exchange resin as a catalyst, carrying out hydrolysis reaction according to a certain proportion under stirring and heating conditions, distilling out alcohol after the reaction is completed, so as to obtain an isooctyltriethoxysilane oligomer crude product; and filtering and separating out the catalyst according to a conventional method, and recycling to obtain a colorless and transparent isooctyltriethoxysilane oligomer product. The product isooctyltriethoxysilane oligomer has the advantages of controllable molecular weight, low volatility, high stability, long service life, low VOC emission and the like, the used ion exchange resin catalyst can be recycled without activity reduction, the process is simple, the equipment requirement is low, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of isooctyltriethoxysilane oligomer, belonging to the technical field of fine chemicals. Background technique [0002] Silane oligomer is a kind of polysiloxane with relatively low degree of polymerization. It is a kind of polymer with repeated Si-O-Si bonds as the main chain and organic groups directly connected to silicon atoms. Because its structure contains both organic groups and inorganic structures, it has the characteristics of both organic and inorganic substances, so it is the most researched and most widely used category of organosilicon materials. [0003] Silane oligomers have excellent high and low temperature resistance, weather resistance, low surface tension, physiological inertness and easy processing, so they are widely used in various fields such as electronics, electrical appliances, construction, transportation, textiles, papermaking, medical treatment and hygiene , is a new type of "...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
CPCC07F7/0874Y02P20/584
Inventor 文少卿胡江华陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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