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The preparation method of propyl silicate waterproofing agent

A technology of propyl silicate and water repellent, which is applied in the direction of chemical instruments and methods, silicon organic compounds, and other chemical processes, and can solve problems such as lack of waterproof effect, pollution of the environment, and inability to use normally, so as to achieve waterproof Good effect, inhibition of self-polymerization, long effective time

Active Publication Date: 2016-06-15
淄博市临淄齐泉工贸有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main component of silicone water repellent is methyl silicate. The preparation of methyl silicate is relatively simple, and the side reaction is less, but the waterproof effect is lacking, which is worse than that of propyl silicate.
Propyl silicate has the same waterproof principle and better waterproof effect, but its production has the disadvantages of polluting the environment and many by-products, so it cannot be used normally

Method used

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  • The preparation method of propyl silicate waterproofing agent

Examples

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Comparison scheme
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Embodiment 1

[0019] 1. Preparation of propyltrimethoxysilane: Add 200g of propyltrichlorosilane into a container with stirring, condenser and thermometer, start stirring, and add 160g of methanol dropwise under negative pressure -0.05Mpa vacuum condition to carry out esterification reaction. After the dropwise addition, continue to stir and pump negative pressure until the pH of the esterification solution is 5.6, and the reaction stops to obtain propyltrimethoxysilane, and the by-product hydrogen chloride produced by the reaction is absorbed by water to obtain hydrochloric acid.

[0020] 2. Preparation of aqueous solution of sodium propyl silicate: add 50g of sodium hydroxide (99% by mass) solid in a container with stirring, condenser and thermometer, add 400g of water and 32g of methanol during the stirring process, stir and mix until sodium hydroxide ( Mass percentage 99%) solid dissolved, sodium hydroxide dissolved and heated up, keeping the temperature at about 40°C, 164g of propyltrim...

Embodiment 2

[0022] 1. Preparation of propyltrimethoxysilane: Add 200g of propyltrichlorosilane into a container with stirring, condenser and thermometer, start stirring, and add 160g of methanol dropwise under negative pressure -0.05Mpa vacuum condition to carry out esterification reaction. After the dropwise addition, continue to stir and pump negative pressure until the pH of the esterification solution is 5.6, and the reaction stops to obtain propyltrimethoxysilane, and the by-product hydrogen chloride produced by the reaction is absorbed by water to obtain hydrochloric acid.

[0023] 2. Preparation of aqueous solution of potassium propyl silicate: add 70g of potassium hydroxide (99% by mass) solid into a container with stirring, condenser and thermometer, add 400g of water and 32g of methanol during stirring, and stir until potassium hydroxide ( Mass percentage 99%) solid dissolved, potassium hydroxide dissolved and heated up, keeping the temperature at about 40°C, 164g of propyltrimet...

Embodiment 3

[0025] 1. Preparation of propyltrimethoxysilane: Add 200g of propyltrichlorosilane into a container with stirring, condenser and thermometer, start stirring, and add 150g of methanol dropwise under negative pressure -0.06Mpa vacuum condition to carry out esterification reaction. After the dropwise addition, continue to stir and pump negative pressure until the ph of the esterification solution is at 6, and the reaction stops to obtain propyltrimethoxysilane, and the by-product hydrogen chloride produced by the reaction is absorbed by water to obtain hydrochloric acid.

[0026] 2. Preparation of aqueous solution of sodium propyl silicate: Add 45g of sodium hydroxide (99% by mass) solid in a container with stirring, condenser and thermometer, add 400g of water and 39g of methanol during stirring, and stir until sodium hydroxide ( Mass percentage 99%) solid dissolved, sodium hydroxide dissolved and heated up, keeping the temperature at about 40°C, 164g of propyltrimethoxysilane wa...

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Abstract

The invention discloses a preparation method for a propyl silicate waterproof agent and belongs to the technical field of waterproof agents. According to the preparation method disclosed by the invention, a by-product, namely, propyltrichlorosilane in a process for producing a silane coupling agent, namely, gamma-chloropropyl trichlorosilane, is reacted with methanol in a molar ratio of 1: (3 to 5) to prepare propyltrimethoxysilane, then the propyltrimethoxysilane is hydrolyzed to obtain propylsilanol, and the propylsilanol is reacted with strong base under the suppression protection of methanol to prepare the propyl silicate aqueous solution-type waterproof agent. The preparation method disclosed by the invention is simple in preparation process, short in reaction time, and adequate in reaction; the yield of propyl silicate is greater than 75%; the generation of wastewater and solid wastes in the preparation process is avoided, so that pollution to environment is avoided.

Description

technical field [0001] The invention discloses a preparation method of a propyl silicate waterproofing agent, which belongs to the technical field of waterproofing agents. Background technique [0002] In the process of using silicon trichloride and chloropropene to prepare silane coupling agent γ-chloropropyl trichlorosilane, it is unavoidable that the by-product propyl trichlorosilane will be generated due to the reaction of impurity propylene and silicon trichloride, the by-product The output is not very large, because there is no specific application outlet or difficult to deal with, it is often discharged directly to pollute the environment and cause waste of resources. [0003] In the prior art, propyl trichlorosilane is directly hydrolyzed to produce propyl silicate aqueous solution. The process needs to use a large amount of water to remove acid, which will inevitably produce a large amount of production wastewater and pollute the environment. There is also direct h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C09K3/18
Inventor 张宇峰孔德强齐峰全杨义会齐泮锋
Owner 淄博市临淄齐泉工贸有限公司