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Solid super acid and method for catalyzing and preparing chloracetate by using same

A technology of solid superacid and chloroacetic acid, which is applied in the field of pesticide chemical industry, can solve the problems of difficult recycling and high cost, etc., and achieve the effect of low toxicity and harmless products, good stability and simple preparation process

Inactive Publication Date: 2013-03-13
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing solid superacid catalysts are difficult to recycle and reuse, and the cost is high

Method used

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  • Solid super acid and method for catalyzing and preparing chloracetate by using same
  • Solid super acid and method for catalyzing and preparing chloracetate by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 60 mL of absolute ethanol to the three-neck flask, add 30 mL of tetrabutyl titanate dropwise under vigorous stirring at about 25 ° C, and continue stirring for 30 min to obtain a uniform and transparent light yellow solution A; add 12 mL of glacial acetic acid and 20 mL of distilled water into 40mL of absolute ethanol and stirred for 30min to obtain solution B. Under vigorous stirring, add solution B dropwise to solution A at a rate of 1-2 drops / second. After dropping, continue stirring for 1 hour to obtain uniform and transparent light yellow TiO 2 Sol. The gel was dried at 80°C for about 10 h, and ground into xerogel powder. The powder was calcined at 325°C for 2h and cooled naturally to room temperature to prepare TiO 2 powder. 6.0g of La 2 o 3 Dissolved in 1.85mol / L dilute sulfuric acid solution to make 0.07mol / L La 3+ solution, and then TiO 2 Soak the powder in it for 14 hours, then filter it with suction, dry it by infrared, activate it at 450℃~500℃ for...

Embodiment 2

[0031] Add 80 mL of absolute ethanol to a three-neck flask, add 30 mL of tetrabutyl titanate dropwise under vigorous stirring at about 25°C, and continue stirring for 30 minutes to obtain a uniform and transparent light yellow solution A; add 23 mL of glacial acetic acid and 27 mL of distilled water into 50mL of absolute ethanol and stirred for 30min to obtain solution B. Under vigorous stirring, add solution B dropwise to solution A at a rate of 1-2 drops / second. After dropping, continue stirring for 1 hour to obtain uniform and transparent light yellow TiO 2 Sol. The gel was dried at 80°C for about 10 h, and ground into xerogel powder. The powder was calcined at 325°C for 2h and cooled naturally to room temperature to prepare TiO 2 powder. 6.0g of La 2 o 3 Dissolved in 1.85mol / L dilute sulfuric acid solution to make 0.07mol / L La 3+ solution, and then TiO 2 Soak the powder in it for 14 hours, then filter it with suction, dry it by infrared, activate it at 450℃~500℃ for...

Embodiment 3

[0035]Add 70mL of absolute ethanol to the three-neck flask, add 30mL of tetrabutyl titanate dropwise under vigorous stirring at about 25°C, and continue stirring for 30min to obtain a uniform and transparent light yellow solution A; add 18mL of glacial acetic acid and 25mL of distilled water into 50mL of absolute ethanol and stirred for 30min to obtain solution B. Under vigorous stirring, add solution B dropwise to solution A at a rate of 1-2 drops / second. After dropping, continue stirring for 1 hour to obtain uniform and transparent light yellow TiO 2 Sol. The gel was dried at 80°C for about 10 h, and ground into xerogel powder. The powder was calcined at 325°C for 2h and cooled naturally to room temperature to prepare TiO 2 powder. 6.0g of La 2 o 3 Dissolved in 1.85mol / L dilute sulfuric acid solution to make 0.07mol / L La 3+ solution, and then TiO 2 Soak the powder in it for 14 hours, then filter it with suction, dry it by infrared, activate it at 450℃~500℃ for 3 hours...

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Abstract

The invention relates to a method for preparing solid super acid and a method for catalyzing and synthetizing chloracetate by using the solid super acid. The method comprises the following steps of: adding tetrabutyl titanate, ethanol, acetic acid and water according to the proportion, reacting at the room temperature, continuously stirring for one hour, standing for two days after the end of the reaction, heating to obtain pale yellow dry solid particles by an oil bath, grinding and sieving with a 150-mesh screen, soaking for 14 hours by lanthanum sulfate solution prepared by dissolving lanthanum oxide in sulfuric acid, and placing in a muffle furnace for calcining for 3 hours at 500 DEG C after suction filtration to obtain pale yellow solid which is a catalyst product. According to the method for preparing the chloracetate, azeotropic with-water performance of toluene is utilized, and a solvent secondary adding method is adopted to ensure anhydrous performance of the catalytic process. The solid super acid provided by the invention has good stability and can be repeatedly used. For the method for preparing the chloracetate, the process is simple, by-products do not exist, and the product is less toxic and harmless.

Description

technical field [0001] The invention relates to a solid superacid and its use for catalyzing the preparation of chloroacetate, which belongs to the field of pesticide chemical industry. Background technique: [0002] Fluroxypyr acetate is developed from the improvement of fluroxypyr acetic acid, a fluorine-containing heterocyclic herbicide. In the synthesis process, the synthesis of the raw material chloroacetate adopts the method of condensation of chloroacetyl chloride and the corresponding alcohol. The raw material, chloroacetyl chloride, is highly toxic and will be violently hydrolyzed in the air to produce hydrogen chloride gas, so this method is not environmentally friendly and the follow-up treatment is troublesome. Such as using a solid superacid catalyst to catalyze the synthesis, the yield is high, the operation is simple, the catalyst is easy to separate, and there is no environmental pollution. It is an environmentally friendly method that is currently recommende...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C67/08C07C69/63
Inventor 潘志权糜昊程清蓉周红黄齐茂
Owner WUHAN INSTITUTE OF TECHNOLOGY
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