Method for preparing oxane trisilicate of containing glucosyacylamino

A technology of glucosamide group and aminotrisiloxane, applied in the direction of sugar derivatives, organic chemistry, etc., can solve the problems of expensive chloroplatinic acid and high toxicity of allylamine, achieve cheap catalyst and avoid toxicity , reduce the effect of the reaction process

Inactive Publication Date: 2005-08-31
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The siloxanes synthesized by these methods all have a hydrosilation reaction in the synthesis process, and the catalyst chloroplatinic acid used in this reaction is more expensive; and the toxicity of allylamine is very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 1.62kg of hexamethyldisiloxane, 2.06kg of aminoethylaminopropyldimethoxymethylsilane, and 1.82g of tetramethylammonium hydroxide into the reaction kettle, heat to dissolve, and control the temperature at 100°C. After 4 hours, the temperature was raised to 130° C. to deactivate the catalyst. Evaporate aminoethylaminopropyl trisiloxane under reduced pressure, add equimolar gluconolactone, use methanol as solvent, heat to reflux, and react for 8 hours. The solvent methanol is evaporated to obtain the product. The minimum surface tension of its aqueous solution measured with a K12 surface tension meter is 21.1mN / m, and the critical micelle concentration is 5.4×10 -4 mol / L, the minimum contact angle on the quartz surface is 14°.

Embodiment 2

[0017] Add 8.10kg of hexamethyldisiloxane, 1.91kg of aminopropyldiethoxymethylsilane, and 168g of potassium hydroxide into the reaction kettle, heat to dissolve, and control the temperature at 120°C. After 5 hours of reaction, add acetic acid and catalyst to deactivate it, and then evaporate unreacted hexamethyldisiloxane. Evaporate aminopropyl trisiloxane under reduced pressure, add equimolar gluconolactone, use methanol as solvent, heat to reflux, and react for 10 hours. The solvent methanol is evaporated to obtain the product. The minimum surface tension of its aqueous solution measured by K12 surface tension meter is 21.2mN / m, and the critical micelle concentration is 6.4×10 -4 mol / L, the minimum contact angle on the quartz surface is 13°.

Embodiment 3

[0019] Add 16.20kg of hexamethyldisiloxane, 1.63kg of aminopropyldimethoxymethylsilane, and 151.8g of tetrabutylphosphonium hydroxide into the reaction kettle, heat to dissolve, and control the temperature at 80°C. After 4 hours of reaction, heat up Heating to 110°C deactivates the catalyst while distilling off unreacted hexamethyldisiloxane. Evaporate aminopropyl trisiloxane under reduced pressure, add equimolar gluconolactone, use methanol as solvent, heat to reflux, and react for 8 hours. The solvent methanol is evaporated to obtain the product. The minimum surface tension of its aqueous solution measured by a K12 surface tension meter is 21.3mN / m, and the critical micelle concentration is 6.3×10 -4 mol / L, the minimum contact angle on the quartz surface is 16°.

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Abstract

A process for preparing trisiloxane containing glucosylamido used as the assistant of agricultural chemical to decrease the surface tension of water includes catalytic reaction between hexamethyl disiloxane and aminosilane to obtain aminotrisiloxane, and reacting on lacton gluconate in methanol.

Description

technical field [0001] The invention relates to a compound obtained by forming silicon-containing bonds in molecules with or without nitrogen, oxygen or carbon bond reactions, in particular to a preparation method of trisiloxane containing glucosamide groups. Background technique [0002] There are existing methods for preparing sugar amidosiloxanes, such as German Patent DE 4,318,539, which discloses a method for preparing sugar amidosiloxanes. The product is obtained by reacting aminosiloxane with sugar lactone. But aminosiloxanes are obtained by hydrosilylation of allylamines. Wagner R. (Applied Organometallic Chemistry, 1996,10,421) reported a method for preparing sugar amidotrisiloxane, which obtained hydrogen-containing trisiloxane by reacting hydrogen-containing silane with hexamethyldisiloxane, Then use chloroplatinic acid as a catalyst to react with allylamine to obtain aminotrisiloxane, and then react with sugar lactone to obtain the product. [0003] The siloxan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H23/00
Inventor 韩富张高勇张越谷惠先张国栋
Owner CHINA RES INST OF DAILY CHEM IND
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