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Method of using solid acid catalyst to synthesize amide-type cooling agent

A solid acid catalyst and cooling agent technology, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of waste acid discharge, non-compliance with green and environmental protection production, etc. Promote the effect of high application value and slowing down the corrosion of production equipment

Pending Publication Date: 2019-09-20
濮阳天源生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The object of the present invention is to provide a method for synthesizing amide cooling agents using solid acid catalysts in view of the waste acid discharge in the synthesis method of amide cooling agents in the prior art, which does not conform to the environmental protection production

Method used

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  • Method of using solid acid catalyst to synthesize amide-type cooling agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Preparation of wetted solid acid catalyst

[0038] Take 72g SiO 2 Heat to reflux in 100ml, 0.1mol / L HCI solution for 1 hour, filter, wash with water until neutral, and dry at 120°C for 2 hours. Treated SiO 2 Dispersed in 100g HClO 4 in ethyl acetate, stirred evenly, concentrated by heating, and activated under nitrogen protection at 80~100°C for 30h to obtain activated HClO 4 -SiO 2 Wetted solid acid catalyst.

[0039] (2) Catalytic synthesis of WS-23

[0040] Take 70g of activated HClO 4 -SiO 2 Load the wetted solid acid catalyst evenly into the fixed bed reactor 1, then mix 140g of 2,2-diisopropylpropionitrile, 256g of methanol and 1.4g of water mixture evenly through the mixer 2, and open the feed valve 3. The raw material liquid enters the fixed bed reactor 1, after the raw material liquid removes the air in the pipeline, open the discharge pump 4 and the second valve 6, so that the raw material liquid circulates in the fixed bed reactor 1, and open the ...

Embodiment 2

[0044] (1) Preparation of wetted solid acid catalyst

[0045] HClO 4 -SiO 2 The preparation of the loaded solid acid catalyst is as in Example 1, so no further details are given.

[0046] (2) Catalytic synthesis of N-ethyl-2,3-dimethyl-2-isopropylbutanamide

[0047] Take 70g of activated HClO 4 -SiO 2 Load the wet-loaded solid acid catalyst evenly into the fixed-bed reactor 1, then mix 140g of 2,2-diisopropylpropionitrile, 300g of ethanol and 1.4g of water in the mixer 2, and open the feed valve 3. The raw material liquid enters the fixed bed reactor 1, after the raw material liquid removes the air in the pipeline, open the discharge pump 4 and the second valve 6, so that the raw material liquid circulates in the fixed bed reactor 1, and open the sleeve type The heating device is used to maintain a constant temperature of 80°C for alcoholysis cycle reaction for 3h.

[0048] Sampling and analysis, after the content of 2,2-diisopropylpropionitrile in the reaction liquid is...

Embodiment 3

[0051] (1) Preparation of wetted solid acid catalyst

[0052] Take 72g SiO 2 Heat to reflux in 100ml, 0.1mol / L HCI solution for 1 hour, filter, wash with water until neutral, and dry at 120°C for 2 hours. Treated SiO 2 Dispersed in 100g H 3 PO 4 in ethyl acetate, stirred evenly, concentrated by heating, and activated under the protection of nitrogen at 80~100°C for 30 hours to obtain activated H 3 PO 4 -SiO 2 Wetted solid acid catalyst.

[0053] (2) Catalytic synthesis of WS-23

[0054] Take 65g of activated H 3 PO 4 -SiO 2 Load the wetted solid acid catalyst evenly into the fixed bed reactor 1, then mix 140g of 2,2-diisopropylpropionitrile, 256g of methanol and 1.4g of water mixture evenly through the mixer 2, and open the feed valve 3. The raw material liquid enters the fixed bed reactor 1, after the raw material liquid removes the air in the pipeline, open the discharge pump 4 and the second valve 6, so that the raw material liquid circulates in the fixed bed rea...

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Abstract

The invention belongs to the technical field of compound preparation, and discloses a method of using a solid acid catalyst to synthesize an amide-type cooling agent. According to the method, 2,2-diisopropyl propane nitrile, C1-C6 lower aliphatic alcohols, and water are taken as the raw materials; and under the action of a solid acid catalyst, thermostatic alcoholysis circular reactions are carried out in a fixed bed reactor. Solid acids are used to replace liquid acids, the problem that a large amount of low concentration acidic wastewater is generated in conventional cooling agent production is solved, the discharge of waste solid, waste gas, and wastewater is reduced, at the same time, the corrosion on production equipment is largely reduced; the method is green and environmentally friendly; a fixed bed reactor is adopted, an outer circulation type reaction technology is used, the alcoholysis process of converting cyano groups into N-alkyl amide is smoothly carried out, the lower aliphatic alcohols can be circularly used after being separated by a gas-liquid separator; the raw material waste is reduced, and continuous production is realized.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and relates to a method for synthesizing an amide-type cooling agent by using a solid acid catalyst. Background technique [0002] WS-23 (N,2,3-trimethyl-2-isopropylbutanamide) is a new type of cooling agent that can replace the traditional cooling agent menthol. Compared with menthol, WS-23 has clear Pleasant, long-lasting, fresh, non-irritating spicy taste, no bitter taste, low dosage, and no strong smell, less irritating to eyes, mucous membranes and skin, can be widely used in chewing gum, toothpaste, candy, jelly, jam, Starch food, dairy products, meat products, cigarettes, medicines and other products. [0003] Most of the production of WS-23 at home and abroad uses propionitrile and halogenated isopropane as raw materials to synthesize WS-23 through two-step reactions of condensation and alcoholysis addition. The reaction equation is as follows: [0004] . [0005] The fi...

Claims

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Application Information

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IPC IPC(8): C07C231/06C07C233/05B01J27/06B01J27/16
CPCB01J27/06B01J27/16C07C231/06C07C233/05C23F11/145
Inventor 文教刚姚彦涛冯乙巳付敬超刘仁欢陈永装李新正
Owner 濮阳天源生物科技有限公司
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