Method for preparing ethyl silicate hydrolysate capable of being stored for long time

A technology of ethyl silicate and hydrolyzate, applied in coatings, anti-corrosion coatings, etc., can solve problems such as short storage period, inconvenient production and application process, and achieve fast drying speed, short storage period and good adhesion Effect

Inactive Publication Date: 2016-03-16
SHANDONG GOLDENCELL ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the prepared ethyl silicate hydrolyzate will undergo further (2) (3) condensation reactions during storage, resulting in a gradual increase in the viscosity of the hydrolyzate until it gels, resulting in a shorter storage period, which is difficult for actual production. , The application process brings a lot of inconvenience

Method used

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  • Method for preparing ethyl silicate hydrolysate capable of being stored for long time
  • Method for preparing ethyl silicate hydrolysate capable of being stored for long time
  • Method for preparing ethyl silicate hydrolysate capable of being stored for long time

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a glass four-necked reaction flask equipped with mechanical stirring, reflux condenser, thermometer and water bath heating, 180g of ethyl silicate (40% silicon content) and 90g of absolute ethanol were sequentially added to the four-necked flask, and opened Stir and heat up to 40°C, the stirring speed is 300 rpm, then add 0.3g of 98% concentrated sulfuric acid into 30g of deionized water and stir evenly, then dropwise into a four-necked flask for hydrolysis reaction, the dropping time is controlled at 1 hour, After the dropwise addition, heat up to 70°C and continue the reaction for 2 hours. After the reaction is completed, when the temperature is cooled to below 30°C, filter the ethyl silicate hydrolyzate into the container, and seal it with a cover.

[0021] The Raman spectrum of ethyl silicate hydrolyzate is as follows figure 1 shown by figure 1 It can be known: 656cm after hydrolysis of ethyl silicate -1 The characteristic peak of the Si-O-C bond in ethyl silic...

Embodiment 2

[0027] In a glass four-necked reaction flask with mechanical stirring, reflux condenser, thermometer and water bath heating, 5Kg ethyl silicate (silicon content is 28%) and 4.5Kg absolute ethanol were successively added to the four-necked flask, Turn on the stirring and heat up to 30°C, the stirring speed is 400 rpm, then add 0.03Kg 98% concentrated sulfuric acid into 0.5Kg deionized water and stir evenly, then drop them into a four-necked flask for hydrolysis reaction, and the dropping time is controlled at 1.5 After the dropwise addition, heat up to 60°C and continue the reaction for 3 hours. After the reaction is completed, when the temperature is cooled to below 30°C, filter the ethyl silicate hydrolyzate into the container and seal it with a cover.

[0028] The ethyl silicate hydrolyzate prepared in Example 2 and the solvent-type inorganic zinc-rich paint main agent A (its composition is mainly polyvinyl butyral, polyamide wax, phosphorus iron powder, zinc powder, precipit...

Embodiment 3

[0032] In a glass four-necked reaction flask equipped with mechanical stirring, reflux condenser, thermometer and water bath heating, 4Kg of ethyl silicate (32% silicon content) and 5Kg of absolute ethanol were sequentially added to the four-necked flask, and opened Stir and heat up to 20°C with a stirring speed of 200 rpm, then add 0.02Kg of 98% concentrated sulfuric acid into 1Kg of deionized water and stir evenly, then dropwise into a four-necked flask for hydrolysis reaction, the dropping time is controlled at 2 hours, After the dropwise addition, heat up to 80°C and continue the reaction for 2 hours. After the reaction is completed, when the temperature is cooled to below 30°C, filter the ethyl silicate hydrolyzate into the container, and seal it with a cover.

[0033] The ethyl silicate hydrolyzate prepared in Example 2 and the solvent-type inorganic zinc-rich paint main agent A (its composition is mainly polyvinyl butyral, polyamide wax, phosphorus iron powder, zinc powd...

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Abstract

The invention relates to a method for preparing ethyl silicate hydrolysate capable of being stored for a long time. By means of the technical scheme, ethyl silicate and anhydrous ethanol are sequentially added into a four-mouth glass reaction flask which is provided with a mechanical stirring device, a backflow condensation pipe and a thermometer and is heated through a water bath, stirring is started, and the temperature is raised; then, concentrated sulfuric acid is added into deionized water, evenly stirred and added into the four-mouth flask dropwise for a hydrolysis reaction, and dropwise adding time is controlled to be 1-2 hours; after dropwise adding, the temperature is raised to 60-80 DEG C, the reaction continues for 2-3 hours, when the temperature is reduced to 30 DEG C or below after the reaction is finished, the mixture is filtered into a container, and is the contained is covered with a cover for sealing. The ethyl silicate hydrolysate prepared through the method can be stored for as long as 12 months at normal temperature. When the ethyl silicate hydrolysate prepared through the method serves as an adhesive and is used for solvent type inorganic zinc-rich paint, a painting film is high in drying speed, good in adhesion force and excellent in corrosion resistance.

Description

technical field [0001] The invention relates to a preparation method of a long-storage ethyl silicate hydrolyzate, which belongs to the technical field of fine chemicals. Background technique [0002] Solvent-based inorganic zinc-rich paint is a two-component paint prepared from a main agent and a binder. The main agent is metal zinc powder as the main anti-rust pigment, which reacts with the binder to form a silicate-zinc- The three-dimensional network structure of iron is closely attached to the steel surface. The binder is ethyl silicate hydrolyzate, its function is that after the coating is applied, it will further undergo hydrolysis and polymerization by absorbing moisture in the air to play a bonding role, and react with the active iron on the surface of the steel to form zinc-silicate-iron The compound also reacts with the surface of the zinc particles, eventually forming a hard zinc silicate varnish film. Because solvent-based inorganic zinc-rich coatings have the ...

Claims

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Application Information

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IPC IPC(8): C08G77/06C09D129/14C09D183/04C09D7/12C09D5/10
CPCC08G77/06C08L2205/03C09D5/106C09D7/61C09D129/14C09D183/04
Inventor 关成善宗继月孟博李冲杜显振
Owner SHANDONG GOLDENCELL ELECTRONICS TECH
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