Method for industrially improving production efficiency of N,2,3-trimethyl-2-isopropyl butyramide

A technology of isopropyl butyramide and production efficiency, applied in the preparation of carboxylic acid amide, chemical instruments and methods, separation/purification of carboxylic acid amide, etc., can solve the company's economic loss, waste, long reaction time and other problems, achieve good Economic and environmental benefits, the effect of improving the reaction efficiency and improving the reaction yield

Inactive Publication Date: 2016-12-14
ANHUI FENGLE PERFUME
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this method are: the reaction must be carried out under strong acid gas and high pressure conditions, which requires strict quality requirements for production equipment and operators; Relatively low yield
The main problems of this scheme are: 1. The reaction is not complete. After the reaction, the residual amount of 2,3-dimethyl-2-isopropylbutyronitrile is 3-8%, which causes the intermediates to fail to fully participate in the reaction, resulting in the Waste; ②The reaction time is long, the original process needs heat preservati

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 139kg of 2,3-dimethyl-2-isopropyl-butyronitrile and 436kg of polyphosphoric acid with a content of 80% into the reactor, heat and stir, and slowly add dimethyl carbonate dropwise when the temperature rises to 100°C 90kg, after the end, add 6kg of water (accounting for 1 / 3 of the total dropping amount) for the first time and keep warm at 120°C for 3 hours, then add 12kg of water (accounting for 2 / 3 of the total dropping amount) for the second time, and continue to keep warm 9 hours, turn off the heat. The temperature of the reactor was lowered to 60° C., and a 30% aqueous sodium hydroxide solution was slowly added dropwise until the pH value of the system reached 7. Add 170kg of ethyl acetate, stir well, and separate the water phase. Cool down and crystallize to obtain the finished product of N,2,3-trimethyl-2-isopropylbutyramide. The residual amount of 2,3-dimethyl-2-isopropyl-butyronitrile in the reaction was 1.14%, and the product yield was 91.14%.

Embodiment 2

[0024] Add 278kg of 2,3-dimethyl-2-isopropyl-butyronitrile and 845kg of polyphosphoric acid with a content of 80% into the reactor, heat and stir, and slowly add dimethyl carbonate dropwise when the temperature rises to 120°C 216kg, after the end, add 12kg of water (accounting for 1 / 3 of the total dropping amount) for the first time and keep warm for 3 hours at 150°C, and add 12kg of water (accounting for 1 / 3 of the total dropping amount) for the second time to keep warm for 3 hours Hour, drip 12kg water (accounting for 1 / 3 of total dropwise amount) for the third time and insulate for 6 hours, stop heating. The temperature of the reaction kettle was lowered to 70 degrees Celsius, and 30% aqueous sodium hydroxide solution was slowly added dropwise until the pH value of the system reached 7. Add 400kg of ethyl acetate, stir well, and separate the water phase. Cool down and crystallize to obtain the finished product of N,2,3-trimethyl-2-isopropylbutyramide. The residual amount ...

Embodiment 3

[0026] Add 278kg of 2,3-dimethyl-2-isopropyl-butyronitrile and 930kg of polyphosphoric acid with a content of 80% into the reactor, heat and stir, and slowly add dimethyl carbonate dropwise when the temperature rises to 120°C 198kg, after the end, add 9kg of water dropwise for the first time (accounting for 1 / 4 of the total dropping amount) at 160°C for 3 hours, then add 9kg of water dropwise for the second time (accounting for 1 / 4 of the total dropping amount) and continue to keep warm for 3 hours Hour, drip 9kg water (accounting for 1 / 4 of total dripping amount) for the third time and insulate for 3 hours, drip 9kg water (accounting for 1 / 4 of total dropping amount) for the fourth time and insulate for 3 hours and stop heating. The temperature of the reaction kettle was lowered to 60 degrees Celsius, and 30% aqueous sodium hydroxide solution was slowly added dropwise until the pH value of the system reached 7. Add 420kg of ethyl acetate, stir well, and separate the water pha...

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PUM

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Abstract

The invention provides a method for industrially improving the production efficiency of N,2,3-trimethyl-2-isopropyl butyramide. The method comprises the following steps: (1) adding 2,3-dimethyl-2-isopropyl-butyronitrile and polyphosphoric acid, which are reaction materials, into a reaction kettle, slowly adding dimethyl carbonate dropwise under the conditions of heating and stirring, adding water dropwise in batches after finishing dropwise adding, continuing to preserve the heat at the temperature of 110-180 DEG C for 12 hours, stopping heating; (2) reducing the temperature of the reaction kettle to lower than 90 DEG C after finishing the reaction, slowly adding a sodium hydroxide aqueous solution of 30% dropwise until the PH value of a system reaches 7, adding ethyl acetate, fully stirring, removing an aqueous phase, cooling, crystalizing to obtain a finished product of the N,2,3-trimethyl-2-isopropyl butyramide. The adding mode of the dimethyl carbonate is changed to slowly adding dropwise, proper amount of water is added in batches after finishing adding the dimethyl carbonate dropwise, so that the reaction speed and the conversion efficiency of the 2,3-dimethyl-2-isopropyl-butyronitrile are both greatly improved.

Description

technical field [0001] The invention relates to the technical field of synthetic cooling agent production, in particular to a method for industrially improving the production efficiency of N,2,3-trimethyl-2-isopropylbutanamide. Background technique [0002] N,2,3-Trimethyl-2-isopropylbutanamide is also known as synthetic cooling agent WS-23, which is characterized by refreshing, long-lasting, fresh, non-irritating spicy taste, no bitter taste, and low dosage. It is one of the more popular synthetic cooling agents in the market in recent years. Its market usage is increasing year by year. [0003] For example, the scheme reported by Li Jiayu and Zhang Chi in the No. 6 issue of "The Synthesis of New Cooling Agent N,2,3-trimethyl-2-isopropylbutanamide (WS-23)" in December 2007, such as fragrance flavor cosmetics, is The intermediate 2,3-dimethyl-2-isopropylbutyronitrile is produced by alkylation of propionitrile and 2-bromopropane, and the intermediate is synthesized in two s...

Claims

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Application Information

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IPC IPC(8): C07C231/06C07C231/24C07C233/05
CPCC07C231/06C07C231/24
Inventor 赵彬金劲松王广强赵国平郭希凯朱俊峰张翼轸赵以梅刘军王亮
Owner ANHUI FENGLE PERFUME
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