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Preparation method of azodicarbonamide

A technology of azodicarbonamide and dimethylformyl, which is applied in the field of preparation of azodicarbonamide, can solve the problems of long steps and low production efficiency, and achieve the effect of less three wastes and high safety

Pending Publication Date: 2021-12-03
安徽昊帆生物有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation method of TMAD is to use ethyl chloroformate or phenyl chloroformate to synthesize the active ester and then replace it with methylamine. This method has long steps and low production efficiency.

Method used

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  • Preparation method of azodicarbonamide
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  • Preparation method of azodicarbonamide

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preparation example Construction

[0024] The preparation method according to the embodiment of the present invention comprises the following steps:

[0025] Step S1, reacting hydrazine hydrochloride and dimethyl formyl chloride to generate an intermediate, the chemical structural formula of the intermediate is shown in the following formula (I):

[0026]

[0027] That is to say, first, using hydrazine hydrochloride and dimethylformyl chloride as raw materials, the intermediate TMDA-1 having the chemical structural formula as shown in the above formula (I) is obtained.

[0028] Specifically, its chemical reaction formula is as shown in the following formula (1):

[0029]

[0030] Wherein, in order to promote the progress of the reaction, the hydrazine hydrochloride can be reacted with dimethylformyl chloride under the action of the first organic base in a tetrahydrofuran solution of hydrazine hydrochloride.

[0031] The existence of the first organic base removes hydrogen ions and chloride ions at the en...

Embodiment 1

[0051] (1) Preparation of compound TMAD-1

[0052]Take a 250mL reaction bottle and add 39.25g of hydrazine hydrochloride, 0.233mol, 2.5eq) and tetrahydrofuran (100mL, 5P), and add triethylamine (51.6g, 0.326mol, 3.5eq) dropwise in an ice-water bath with temperature controlled at 10-15°C, and continue to maintain Dimethylformyl chloride (10 g, 0.093 mol, 1.0 eq) was added dropwise at high temperature, and the reaction was completed after 4 hours of heat preservation. The reaction solution was washed with water (50mL*2), dried over anhydrous sodium sulfate, filtered, and concentrated to obtain 13.1g of TMAD-1 with a yield of 81%.

[0053] (2) Preparation of compound TMAD

[0054] Add TMAD-1 (13.1g, 0.075mol, 1.0eq), NBS (13.4g, 0.075mmol, 1.0eq) into dichloromethane (100mL, 8P), add pyridine (5.9g , 0.075mol, 1.0eq), and incubated for 3 hours. The reaction solution was washed with 50 mL of water and 50 mL of saturated brine, dried over anhydrous sodium sulfate, filtered, and ...

Embodiment 2

[0058] (1) Preparation of compound TMAD-1

[0059] Take a 10L reaction bottle and add hydrazine hydrochloride (1.963kg, 28.65mol, 2.5eq) and tetrahydrofuran (5L, 5P), add triethylamine (2.58kg, 16.3mol, 3.5eq) dropwise in an ice-water bath with temperature controlled at 10-15°C, and continue to maintain Dimethylformyl chloride (500 g, 4.65 mol, 1.0 eq) was added dropwise at high temperature, and the reaction was completed after 6 hours of heat preservation. The reaction solution was washed with water (2.5L*2), dried over anhydrous sodium sulfate, filtered, and concentrated to obtain 701g of TMAD-1 with a yield of 86.5%.

[0060] (2) Preparation of compound TMAD

[0061] Add TMAD-1 (701g, 4.02mol, 1.0eq), NBS (715.6g, 4.02mol, 1.0eq) into dichloromethane (5.6L, 8P), and add pyridine (317.6g , 4.02mol, 1.0eq), and incubated for 3 hours. The reaction solution was washed with 2L of water and 2L of saturated brine, dried over anhydrous sodium sulfate, filtered, and concentrated ...

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Abstract

The invention provides a preparation method of azodicarbonamide, which comprises the following steps: S1, reacting hydrazine hydrochloride with dimethylformyl chloride to generate an intermediate; and S2, carrying out an azo reaction on the intermediate, so as to obtain the azodicarbonamide. According to the preparation method disclosed by the embodiment of the invention, the used raw materials are high in safety, few three wastes are formed in the production, and the obtained product can be obtained only by effectively separating and drying, and pure TMDA can be obtained without re-purification.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of azodicarbonamide. Background technique [0002] Azodicarbonamide (TMAD) is a non-toxic, odorless foaming agent. Because of the -N=N- bond in its molecular structure, it can release up to 200-250mL / g of nitrogen when heated, so it is compared widely used. [0003] At present, the preparation method of TMAD is to use ethyl chloroformate or phenyl chloroformate to first synthesize an active ester and then replace it with methylamine. This method has long steps and low production efficiency. Contents of the invention [0004] In view of this, the present invention provides a reaction raw material with high safety, strong operability, less waste, and can obtain pure TMAD without further purification, which is more suitable for industrial production. [0005] In order to solve the problems of the technologies described above, the present invention...

Claims

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Application Information

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IPC IPC(8): C07C281/20C07C281/06
CPCC07C281/20C07C281/06
Inventor 王桂春刘炼骆浩
Owner 安徽昊帆生物有限公司
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