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Preparation method of N,N-dimethyl glycine ester based on silica gel sulfonic acid serving as catalyst

A technology of dimethylglycine ester and dimethylglycine, which is applied in the field of chemical industry, can solve the problems of cumbersome operation and increased synthesis reaction cost, and achieve the effects of simple treatment, reduction of waste generation, and production cost saving

Inactive Publication Date: 2013-11-20
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the cost of the synthesis reaction increases and the operation is cumbersome.

Method used

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  • Preparation method of N,N-dimethyl glycine ester based on silica gel sulfonic acid serving as catalyst
  • Preparation method of N,N-dimethyl glycine ester based on silica gel sulfonic acid serving as catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Example 1: Synthesis of N,N-dimethylglycine

[0031] Hydroxyacetonitrile method: at room temperature, add 1000 grams of 40% hydroxyacetonitrile aqueous solution to the autoclave, then pass through 1435 grams of 33% dimethylamine aqueous solution, then raise the temperature to 60°C, and the pressure reaches 7 kg (mPa), and react for 30 After 12 minutes, stop the reaction, transfer the reaction solution to a 3000ml flask, add 786 grams of 50% potassium hydroxide aqueous solution in the reaction solution, and incubate at 80°C for 5 hours to obtain N,N-dimethylglycinate Ammonia solution, deamination to obtain N,N-dimethylglycine salt solution, and then add 37% hydrochloric acid to adjust the pH to 5.0 to obtain a mixture of N,N-dimethylglycine and potassium chloride. Add 8 grams of activated carbon for decolorization, filter the activated carbon with suction, cool the filtrate to 10°C, crystallize, and centrifuge to remove potassium chloride crystals, and crystallize and pu...

Embodiment 2

[0032] Embodiment two N, the synthesis of N-dimethylglycine

[0033]Formaldehyde, sodium cyanide and dimethylamine three-component Strecker method: add 1000 grams of 37% formaldehyde aqueous solution and 2215 grams of 30% sodium cyanide aqueous solution to the reactor, and then slowly add 3363 grams of 33% dimethylamine aqueous solution dropwise, After the dropwise addition, raise the temperature to 80°C and react for 5 hours to obtain an ammonia solution of N,N-dimethylglycine sodium salt, deamination to obtain a solution of N,N-dimethylglycine sodium salt, and then add 98% sulfuric acid to adjust pH to 5.0, to obtain a mixture of N,N-dimethylglycine and sodium sulfate. Add 6 grams of activated carbon for decolorization, filter the activated carbon with suction, cool the filtrate to 10°C, crystallize, centrifuge to remove sodium sulfate crystals, and crystallize and purify the filtrate according to conventional methods to obtain 646 grams of N,N-dimethylglycine solid with a p...

Embodiment 3

[0034] Embodiment three: the preparation of catalyst silica gel sulfonic acid

[0035] Add 1000 grams of 200-300 mesh dry silica gel into the reactor, then add 2000 grams of dichloromethane, stir at room temperature, and slowly add a certain amount of chlorosulfonic acid. After the addition was complete, stirring was continued at room temperature for 2 hours, and the hydrogen chloride gas released was absorbed with water. Stand still and remove dichloromethane to obtain silica gel sulfonic acid with a certain amount of immobilized sulfonic acid, dry and analyze the immobilized amount of sulfonic acid to obtain catalyst silica gel sulfonic acid for future use. The mass ratio of the sulfonic acid to the silica gel by weight of chlorosulfonic acid is 15-40%.

[0036] catalyst Chlorosulfonic acid (g) Solid loading (mmol / g) Silica sulfonic acid A 150 1.28 Silica sulfonic acid B 250 2.14 Silica sulfonic acid C 400 3.40

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Abstract

The invention relates to preparation of N, N-dimethyl glycine ester chemical products, particularly relates to a preparation method of N,N-dimethyl glycine ester based on silica gel sulfonic acid serving as a catalyst, and belongs to the field of chemical industries. The preparation method is characterized in that carboxylic acid and alcohol are used as raw materials for carrying out esterification reaction so as to obtain the N,N-dimethyl glycine ester, the catalyst for esterification reaction is the silica gel sulfonic acid, the carboxylic acid is N,N-dimethyl glycine, and the alcohol is fatty alcohol with 1-12 carbon atoms. The synthesis of the silica gel sulfonic acid serving as the catalyst involved in the invention is simple, raw materials for synthesis of the catalyst are cheap and easily available, and the catalyst has high catalytic activity; the catalyst is recycled and reused through simple filtration, so that the production cost is saved; the corrosion of sulfuric acid, phosphoric acid and the like to equipment is avoided; by adopting the technology, the yield is high, and the conversion rate can reach above 95%; after completion of reaction, the follow-up treatment is simple; the atom economy in the whole reaction process is good, and no other waste products are generated except for water.

Description

technical field [0001] The invention aims at the field of chemical industry and relates to the preparation of N,N-dimethylglycine ester chemical products. Background technique [0002] Esterification reaction is a kind of organic chemical reaction, which is the reaction of alcohol and carboxylic acid / oxygen-containing inorganic acid to form ester and water. The esterification reaction is divided into two categories, one is the reaction of carboxylic acid and alcohol, and the other is the reaction of inorganic oxyacid / inorganic strong acid and alcohol. The first type of esterification reaction is reversible, and the reaction is slow, and concentrated sulfuric acid is often used as a catalyst. [0003] N,N-Dimethylglycinate, also known as N,N-Dimethylaminoacetate, is a new type of skin penetration enhancer. This type of compound can be applied to creams, ointments and liniments in medicines and cosmetics to enhance the penetration and absorption of medicines on the skin and ...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/12
CPCY02P20/584
Inventor 吴传隆龙晓钦郑道敏姚如杰丁永良秦岭朱丽利王用贵杨帆
Owner CHONGQING UNISPLENDOUR CHEM
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