A kind of method for preparing propyl silicate

A technology of propyl silicic acid and silicate, applied in the direction of silicon organic compounds, etc., can solve the problems of low production efficiency, inability to industrialize production, low product yield, etc., and achieve high production efficiency, moderate size, and improved reaction yield. Effect

Active Publication Date: 2019-09-10
江西宏柏新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defects of low product yield and low production efficiency in the existing method for preparing propyl silicate, and the direct hydrolysis of propyl trichlorosilane is easy to cross-link with the reaction vessel and cannot be produced industrially, and provides a The method for preparing propyl silicate with high product yield, high production efficiency, environmental protection and benefit to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) A 1000ml four-necked flask is equipped with stirring, a thermometer, a condenser and a constant pressure dropping funnel. Under stirring, add 400g of water and 400g of sodium-type cation exchange resin into the four-necked flask, and control the temperature at 55 ℃, and then add 100g of propyltrichlorosilane into the constant pressure dropping funnel and drop it into a four-neck flask for hydrolysis reaction. The time for adding propyltrichlorosilane is 2 hours. After the addition, keep the temperature and continue the reaction for 15 minutes , The upper layer of the reaction solution was filtered to obtain propyl silicic acid particles with an average particle diameter of 3.1 mm.

[0029] (2) The propyl silicic acid particles obtained in step (1) were washed with water until the pH was 6, and 64 g of propyl silicic acid granules were obtained.

[0030] (3) Add the propylsilicic acid particles obtained by washing in step (2), 32g of water and 50g of sodium hydroxide...

Embodiment 2

[0032](1) A 1000ml four-necked flask is equipped with stirring, a thermometer, a condenser and a constant pressure dropping funnel. Under stirring, add 300g of water and 400g of sodium-type cation exchange resin into the four-necked flask, and control the temperature at 65 ℃, then add 100g of propyltrichlorosilane into the constant pressure dropping funnel and drop it into a four-neck flask for hydrolysis reaction. The time for adding propyltrichlorosilane is 1.5 hours. After the addition, keep the temperature and continue the reaction for 15 minutes , The upper layer of the reaction solution was filtered to obtain propyl silicic acid particles with an average particle diameter of 4 mm.

[0033] (2) The propyl silicic acid particles obtained in the step (1) were washed with water until the pH was 8, and 78 g of propyl silicic acid particles were obtained.

[0034] (3) Add the propylsilicic acid particles obtained by washing in step (2), 63g of water and 78g of potassium hydrox...

Embodiment 3

[0036] (1) A 1000ml four-necked flask is equipped with stirring, a thermometer, a condenser and a constant pressure dropping funnel. Under stirring, add 500g of water and 350g of sodium-type cation exchange resin into the four-necked flask, and control the temperature at 45 ℃, and then add 100g of propyltrichlorosilane into the constant pressure dropping funnel and drop it into a four-neck flask for hydrolysis reaction. The time for adding propyltrichlorosilane is 2.5 hours. After the addition, keep the temperature and continue the reaction for 15 minutes , and filter the upper layer of the reaction solution to obtain propyl silicic acid particles with an average particle diameter of 2 mm.

[0037] (2) The propyl silicic acid particles obtained by washing in step (1) were washed with water until the pH was 5, and 74 g of propyl silicic acid granules were obtained.

[0038] (3) Add the propylsilicic acid particles obtained in step (2), 74g of water and 90g of sodium hydroxide i...

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Abstract

The invention discloses a method of preparing propyl silicate. The method includes the steps of: 1) mixing propyl trichlorosilane, water and Na-type cation exchange resin to perform a hydrolysis reaction, and filtering an upper layer after the reaction is finished to prepare propyl silicic acid particles, wherein the weight ratio of the propyl trichlorosilane, the water to the Na-type cation exchange resin is 1:2-7:2-5 and the temperature of hydrolysis is 20-70 DEG C; 2) washing the propyl silicic acid particles until the pH value is 5-8; 3) performing contact reaction to the propyl silicic acid particles with water and NaOH / KOH, and filtering the mixture to obtain a propyl silicate solution being 25-50% in content, wherein the weight ratio of the propyl silicic acid particles, water to the NaOH / KOH is 1:0.5-1:0.5-1.5, the reaction temperature is 90-120 DEG C and the reaction time is 0.5-2 h of the contact reaction. The method is high in product yield and production efficiency, is environment-friendly and is especially suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing organic silicate, in particular to a method for preparing propyl silicate. Background technique [0002] Organosilicates, as building material waterproofing agents, have attracted widespread attention due to their excellent water resistance, acid and alkali resistance, high temperature resistance and low price. [0003] At present, the most commonly used organic silicate waterproofing agent is sodium methyl silicate. However, with the development of modern buildings and changes in environmental factors, higher requirements are placed on the performance of waterproofing agents. Propyl silicates have attracted attention due to their superior water repellency properties over methyl silicates. [0004] CN102633826A discloses a method for preparing an aqueous propyl silicate solution by using propyl trichlorosilane, the method includes hydrolyzing and condensing propyl trichlorosilane, a by-product of silane,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
Inventor 齐官军叶科文田丹李明生甘高翔
Owner 江西宏柏新材料股份有限公司
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