Preparation method of morpholine ethanesulfonic acid

A technology of morpholineethanesulfonic acid and sodium morpholineethanesulfonate, which is applied in the field of ethanesulfonic acid derivative products, can solve the problems of high COD of crystallization centrifuged mother liquor, corrosion damage of production equipment, high cost of biochemical treatment, etc., and achieves improved acidification removal Effects of salt method, increased equipment life, and improved synthesis conditions

Pending Publication Date: 2019-09-27
XZL BIO TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis technology has the following disadvantages: first, the synthesis process of the raw material sodium vinyl sulfonate generates a large amount of polymerized impurities, resulting in high COD of the crystallization centrifuged mother liquor, and high biochemical treatment costs; second, the resin column adsorption acidification needs to dilute the reaction solution After 5-10 times, the analysis of the resin column will produce a large amount of acidic wastewater and washing wastewater, which will cause high production cost and large environmental pollution; thirdly, the collected morpholine ethanesulfonic acid solution will be concentrated and the water will contain acidic substances, which will easily affect the production. Corrosion damage to equipment

Method used

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  • Preparation method of morpholine ethanesulfonic acid
  • Preparation method of morpholine ethanesulfonic acid
  • Preparation method of morpholine ethanesulfonic acid

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Effect test

preparation example Construction

[0037] A kind of reaction formula of the preparation method of morpholineethanesulfonic acid is:

[0038] (1) Sulfonation

[0039] Main response:

[0040] side effects:

[0041] (2) Neutralization

[0042] Main response:

[0043] HSO 3 -CH 2 -CH 2 -O-SO 3 H+2NaOH→NaSO 3 -CH 2 -CH 2 -O-SO 3 Na+2H 2 o

[0044] side effects:

[0045] NaSO 3 -CH 2 -CH 2 -O-SO 3 Na+NaOH→NaSO 3 -CH=CH 2 +NaSO 4 +H 2 o

[0046] h 2 SO 4 +2NaOH→Na 2 SO 4 +2H 2 o

[0047] (3) Addition

[0048] Main response:

[0049]

[0050] side effects:

[0051]

[0052] (4) Acidification

[0053] Main response:

[0054]

[0055] side effects:

[0056]

[0057] Infrared Qualitative Analysis figure 1 and figure 2 The match is 99.86%.

Embodiment 1

[0059] (1) Add 64.4g of absolute ethanol, and feed 224g of sulfur trioxide gas at 0-50°C under stirring and cooling to generate ethanedisulfonic acid;

[0060] (2) Add 284.4g of deionized water and drop ethanedisulfonic acid at 35-40°C to dilute;

[0061] (3) Add dropwise 30% liquid caustic soda 373.3g at 35-40°C under stirring and cooling down to generate sodium edisulphonate solution, add morpholine 121.8g under stirring, add 30% liquid caustic soda 186.7g dropwise at 60°C, control The pH of the reaction solution is 12.5-13.5. After the dropwise addition is completed, the temperature is kept at 60°C for 4 hours, the temperature is raised to 100°C and the temperature is kept at reflux for 4 hours, and the temperature is lowered to below 40°C;

[0062] (4) Add 142g of 49% dilute sulfuric acid dropwise to acidify to PH=4.3, add 400g of deionized water to dilute to a material content below 15%, cool to 10-20°C and centrifuge 386.4g of crystallized sodium sulfate decahydrate;

...

Embodiment 2

[0066] (1) Add 64.4g of absolute ethanol, and feed 224g of sulfur trioxide gas at 0-50°C under stirring and cooling to generate ethanedisulfonic acid;

[0067] (2) Add 284.4g of deionized water and drop ethanedisulfonic acid at 10-20°C to dilute;

[0068] (3) Add 30% liquid caustic soda 373.3g dropwise at 10-20°C under stirring and cooling to generate sodium edisulphonate solution, add morpholine 121.8g under stirring, add 30% liquid caustic soda 186.7g dropwise at 60°C, control The pH of the reaction solution is 12.5-13.5. After the dropwise addition is completed, the temperature is kept at 60°C for 8 hours, the temperature is raised to 100°C and the temperature is kept at reflux for 4 hours, and the temperature is lowered to below 40°C;

[0069] (4) Add 142g of 49% dilute sulfuric acid dropwise to acidify to PH=4.3, add 400g of deionized water to dilute to a material content below 15%, cool down to 10-20°C and centrifuge 382g of crystallized sodium sulfate decahydrate;

[0...

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Abstract

The invention discloses a preparation method of morpholine ethanesulfonic acid, and relates to the field of ethanesulfonic acid derivative products. The preparation method comprises the following steps that 1, sulfonation is conducted, wherein anhydrous ethanol is introduced into sulfur trioxide gas under stirring and cooling conditions to generate ethionic acid; the ethionic acid is dropwise added into deionized water for dilution; 2, neutralizing is carried out, wherein liquid alkali is dropwise added into the ethionic acid solution under stirring and cooling conditions to generate a sodium ethanedisulphonate solution; 3, addition is performed, wherein morpholine is added into the sodium ethanedisulphonate solution during stirring, heating is conducted, liquid alkali is added dropwise, the PH value of a reaction solution is controlled, heat preservation is conducted for a period of time, and sodium 4-morpholin-1-ylethylsulphonate is generated; 4, acidifying is carried out; 5, a sodium 4-morpholin-1-ylethylsulphonate solution enters an electrodialysis membrane device to further separate sodium sulfate salt, negative-pressure concentrating and dehydrating are carried out, cooling crystallization and centrifugal separation are conducted to obtain a 2-(N-morpholino)ethanesulfonic acid monohydrate product, and centrifugal liquid can be circularly sleeved and concentrated to extract the product. According to the method, synthesis conditions are improved, generation of a reaction polymer is reduced, and the reaction conversion rate is increased to 95% from 70% of the original process according to ethanol.

Description

technical field [0001] The invention relates to the field of ethanesulfonic acid derivative products, in particular to a preparation method of morpholineethanesulfonic acid. Background technique [0002] The synthesis of morpholine ethanesulfonic acid adopts ethanol stirring and cooling to pass through sulfur trioxide gas (molar ratio 1:2) at 0-50 ℃ to generate ethanedisulfonic acid, and add 30% liquid caustic soda (molar ratio 1:3) and ether polymerization inhibitor (molar ratio 1:0.005) to 50-60°C, add ethylene disulfonic acid dropwise to react to form a mixture of sodium vinylsulfonate, sodium sulfate and sodium polyvinylsulfonate, freeze and centrifuge to separate sodium sulfate Salt to obtain sodium vinylsulfonate solution, addition reaction of morpholine and sodium vinylsulfonate solution (molar ratio 1:1) to generate sodium morpholineethanesulfonate, sodium morpholineethanesulfonate adsorbs sodium ions through a cationic resin column After collecting the morpholine e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/088
CPCC07D295/088
Inventor 邓新基石晶王超刘景亮张华田园李秀秀
Owner XZL BIO TECHNOLOGY CO LTD
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