Industrial synthesis method for acetoxylpropyltrimethoxysilane

A technology of acetoxypropyltrimethoxysilane and trichlorosilane, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problem of many addition by-products, Eye irritation, environmental pollution and other problems, to achieve the effect of high yield, simple synthesis process, no environmental pollution

Active Publication Date: 2018-05-22
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The first three-step method is the most commonly used method in industry at present, and the process is very mature, but there are two problems: one is that there are many by-products in the step of obtaining chloropropyl trichlorosilane by addition of chloropropene and trichlorosilane , resulting in a low yield of the target addition product and an increase in production cost
The second is that when chloropropyltrimethoxysilane reacts with anhydrous sodium acetate, a large amount of by-product sodium chloride solid will be generated. There are 263 kilograms of sodium chloride salt in theory per ton of product, which contains a small amount of acetyl Oxypropyltrimethoxysilane is difficult to clean and cause environmental pollution
[0012] The second method is the simplest method, but the process is immature, and there are some problems as follows: First, the raw material trimethoxysilane is prone to self-disproportionation reaction during production, transportation, storage and use, and emits flammable and explosive The dangerous gas hydrogen has a great potential safety hazard. There have been safety accidents of trimethoxysilane flash explosion in many domestic manufacturers who produce and use trimethoxysilane
Moreover, trimethoxysilane vapor is extremely irritating to human eyes, making eyes red and swollen or even blind
Second, the quality of the raw material trimethoxysilane is unstable
The metal copper catalyst may remain in the trimethoxysilane synthesized by the direct method, and hydrogen chloride may remain in the trimethoxysilane synthesized by the esterification method. These two substances will poison the platinum catalyst and make the production unstable; the third is the addition of by-products Many, the yield is not high; the fourth is the need to use solvents, the consumption and treatment of solvents, increase production costs and reduce production capacity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add a tetrafluoromagnetic stirring bar into a 500 ml four-neck flask, connect the -10~0°C brine reflux condenser at the middle port, and connect the tail gas to the drying tower. Mix 138.2 g (1.02 mol) trichlorosilane and 100.1 g (1.0 mol) ) allyl acetate is mixed evenly and put into a 250 milliliter constant pressure funnel, put 20 milliliters of mixed raw materials in the flask, then add 0.02 milliliters of prepared main catalyst and co-catalyst to the flask mixed material, turn on the magnetic stirring, and slowly The temperature of the kettle rises to 75°C, open the discharge valve of the constant pressure funnel and start to drop the mixed material. Controlled at 75°C. After the dropwise addition, the temperature of the kettle was raised to 85°C for aging for 2 hours, then the reaction equipment was connected to a distillation device, and 2.7 grams of unreacted excess raw material trichlorosilane was distilled out, and the addition product acetoxysilane was contain...

Embodiment 2

[0041] Add a tetrafluoromagnetic stirring bar into a 2000 ml four-neck flask, connect the -10~0°C brine reflux condenser at the middle port, and connect the tail gas to the drying tower, mix 711.4 grams (5.25 mol) of trichlorosilane and 500.5 grams (5.0 mol) ) allyl acetate is mixed evenly and put into a 250 milliliter constant pressure funnel, put 40 milliliters of mixed raw materials in the flask, then add 0.1 milliliters of the prepared main catalyst and co-catalyst to the flask mixed material, turn on the magnetic stirring, and slowly The temperature of the kettle rises to 75°C, open the discharge valve of the constant pressure funnel and start to drop the mixed material. Controlled at 85°C. After the dropwise addition, the temperature of the kettle was raised to 90°C for 2 hours of heat preservation and aging, then the reaction equipment was connected to a distillation device, and 31.8 grams of unreacted excess raw material trichlorosilane was distilled out, and the addit...

Embodiment 3

[0044] Add a PTFE magnetic stirrer in a 2000ml four-neck flask, connect the -10~0°C brine reflux condenser at the middle port, connect the tail gas to the drying tower, and distill out the unreacted excess raw material trichlorosilane in Example 2 31.8 grams and 679.6 grams of new trichlorosilane, a total of 711.4 grams (5.25mol) of trichlorosilane and 500.5 grams (5.0mol) of allyl acetate are mixed evenly, then put into a 250 ml constant pressure funnel, put 20-40 ml and mix Put the raw materials into the flask, then add 0.1 ml each of the prepared main catalyst and co-catalyst to the mixture in the flask, turn on the magnetic stirring, slowly raise the temperature of the kettle to 75°C, open the discharge valve of the constant pressure funnel and start adding the mixture dropwise. During the addition process, the temperature of the kettle will rise, and there will be a small amount of reflux in the reflux condenser pipe. The dropping rate is controlled for 6 hours with the di...

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PUM

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Abstract

The invention relates to an industrial synthesis method for acetoxylpropyltrimethoxysilane, which belongs to the technical field of fine chemical engineering. According to the industrial synthesis method, trichlorosilane and allyl acetate first undergo hydrosilylation under catalyst, so that acetoxylpropyltrichlorosilane is obtained, and methanol is then used for esterifying acetoxylpropyltrichlorosilane so that acetoxylpropyltrimethoxysilane and hydrochloric acid are obtained. The yield of acetoxylpropyltrimethoxysilane disclosed by the invention is high, the synthesis process is simple and safe, and the environment is not polluted.

Description

technical field [0001] The invention relates to an industrial synthesis method of acetoxypropyltrimethoxysilane, which belongs to the technical field of fine chemicals. Background technique [0002] Acetoxypropyltrimethoxysilane is a widely used silane coupling agent product. Its molecular structure contains an acetoxy functional group with an unsaturated double bond structure and three hydrolyzable methoxy functional groups. Its dual reactivity allows them to improve the degree of bonding, bonding and compatibility between the two through two-way chemical reactions with inorganic materials such as glass, metals, fillers, and organic polymers such as thermosetting resins, plastics, and elastomers. Then improve the mechanical properties of the resin-based composite material or improve the adhesive strength and water resistance of the resin coating. At the same time, acetoxypropyltrimethoxysilane can also be copolymerized with monomers such as acrylic acid, methacrylic acid, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/14C07F7/18
CPCC07F7/14C07F7/188
Inventor 胡江华秦传俊汤艳阮少阳陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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