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Technology for preparing double-amino silane and treating by-product

A bisaminosilane and treatment process technology, which is applied in the field of preparation and by-product treatment process, can solve the problems of reduced product yield, low product yield, high cost, etc., to improve product yield, shorten reaction time, The effect of reducing energy consumption

Active Publication Date: 2015-03-11
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above patents all describe the preparation method of bisaminosilane: using a tower reactor, the reaction temperature is 120-160°C, and the feed ratio is 3-10:1; however, there are problems of low product yield and high energy consumption. problem; and its by-product ethylenediamine hydrochloride is not described and dealt with
[0004] In recent years, with the rapid development of the economy, the cost of raw materials and production has become higher and higher, and the requirements for environmental protection and energy consumption have become more and more stringent. The treatment methods of acid salts are roughly divided into three categories: one is not treated, and it is directly disposed of as waste; the other is distilled after treatment with a strong alkali solution such as KOH and NaOH, but 70% ethylenediamine is obtained after treatment. If the water content is too high, all silane products will be hydrolyzed and polymerized and deteriorated, so they cannot be reused as raw materials for production; the third type is treated with sodium alkoxide, such as sodium methoxide, sodium ethoxide, etc. This method is not only costly, but also expensive. The ethylenediamine product obtained by this method contains methanol or ethanol. If it is reused as a raw material in production, a small amount of alcohol will affect the stratification of the crude product and reduce the product yield.

Method used

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  • Technology for preparing double-amino silane and treating by-product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 12mol (721.2g) of ethylenediamine into the reaction kettle, press 1mol (198.7g) of chloropropyltrimethoxysilane into the metering tank, raise the temperature of ethylenediamine to 120°C under the stirring condition of 100 rpm, and drop Add the chloropropyltrimethoxysilane in the metering tank dropwise to the ethylenediamine in the reaction kettle within 4 hours from the liquid funnel. After the dropwise addition, continue the heat preservation reaction at 120°C for 2 hours, and the reaction will generate N-(β- Aminoethyl)-3-aminopropyltrimethoxysilane and ethylenediamine hydrochloride, then lower the temperature of the kettle to 80°C, and simultaneously turn on the water circulation vacuum pump to recover ethylenediamine 8mol (480.8 grams), after the recovery is completed, the temperature of the kettle is lowered to 40°C, and then the materials in the kettle are introduced into a conical settling kettle under normal pressure and statically stratified for 4 hours. Af...

Embodiment 2

[0024] Add 114.4 grams of ethylenediamine to the reaction kettle, and simultaneously add 480.8 grams of ethylenediamine recovered from the reaction in Example 1 and 126.0 grams of ethylenediamine recovered from ethylenediamine hydrochloride, and 1mol (198.7 grams) of chloropropyl trimethyl Press oxysilane into the metering tank, raise the temperature of ethylenediamine in the reactor to 125°C under stirring at 100 rpm, and then add chloropropyltrimethoxysilane dropwise to the ethylenediamine in the reactor within 4 hours through the dropping funnel. In the diamine, after the dropwise addition, the reaction was continued at 125°C for 2 hours to generate N-(β-aminoethyl)-3-aminopropyltrimethoxysilane and ethylenediamine hydrochloride. When the temperature drops to 80°C, turn on the water circulation vacuum pump to recover 8 mol (480.8 grams) of ethylenediamine under the condition of -0.08MPa. After the recovery is completed, lower the temperature of the kettle to 40°C and introdu...

Embodiment 3

[0027] Add 12mol (721.2 grams) of ethylenediamine into the reaction kettle, press 1mol (240.5 grams) of chloropropyltriethoxysilane into the metering tank, and raise the temperature of the ethylenediamine in the kettle to 122 ℃, within 4 hours through the dropping funnel, add 1 mol (240.5 g) of chloropropyltriethoxysilane dropwise to the reaction tank with the dropping funnel within 4 hours. In the ethylenediamine in the kettle, after the dropwise addition, the reaction was continued at 122°C for 2 hours, and the reaction produced N-(β-aminoethyl)-3-aminopropyltriethoxysilane and ethylenediamine hydrochloride After the reaction is completed, the temperature of the kettle is lowered to 80°C, and at the same time, the water circulation vacuum pump is turned on to recover 8mol (480.8 grams) of ethylenediamine under the condition of -0.08MPa. After the recovery is completed, the temperature of the kettle is lowered to 40°C and the The inner material is introduced into the conical ...

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Abstract

The invention relates to a technology for preparing double-amino silane and treating by-product, belonging to the field of chemical technology. By adopting a reaction way of dripping chloropropylated silane, the technology reduces the energy consumption and shortens the reaction time. Meanwhile, the technology can be used for treating the by-product ethylenediamine hydrochloride, so that the production cost is lowered, the environmental pollution is reduced, and the problem that the existing by-product ethylenediamine hydrochloride is treated by distilling through strong alkali solution, so that the treated by-product can not be reused as raw material can be solved; and the problems that the cost is high when the by-product is treated by sodium alcoholate, and the product yield is reduced after the treated by-product is reused as raw material can be solved. After the technology is adopted, the product yield is improved, and the treated by-product can be reused, so that the technology is suitable for industrial production and has higher economic effect and environmental protection effect.

Description

technical field [0001] The invention relates to the preparation of bisaminosilane and the treatment process of its by-products, belonging to the technical field of chemical industry. Background technique [0002] Diaminosilane, especially N-(β-aminoethyl)-3-aminopropyltrimethoxysilane and N-(β-aminoethyl)-3-aminopropylmethyldimethoxysilane is a An important industrial additive, it can be used to couple organic high polymers and inorganic substances, can be used as a glass fiber finishing agent, can be used as a crosslinking agent and curing agent for silicone rubber and silicone resin, and can be used as a textile Finishing agent can also be made into amino-modified silicone oil and so on. [0003] Regarding the preparation method of diaminosilane, there are quite a lot of patent reports abroad, such as U.S. Patent US2971864, Polish Patent 145671, Japanese Patent Publication No. 40-1185, JP-5-194550.1993, JP-6-11878.1994, German Patent No. 595488.1994, etc. . The above pa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 胡江华陈圣云秦传俊阮少阳王欣王灿甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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