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Method for synthesizing 3-alkenyl-1, 6-diacid by using electrochemical reaction

A chemical reaction and diacid technology, applied in the electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problems of poor selectivity, difficult separation, unsuitable for industrialization, etc., and achieve low cost, good catalysis, and easy purification and separation. Effect

Inactive Publication Date: 2010-04-07
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

People such as J.Bringmann react with cheap butadiene and carbon dioxide, use Ni ligand as a catalyst, and in a container without a diaphragm, the method of sacrificing the anode to synthesize 3-hexenedioic acid has a higher yield, but the choice of reaction Very poor, difficult to separate, not suitable for industrialization

Method used

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  • Method for synthesizing 3-alkenyl-1, 6-diacid by using electrochemical reaction
  • Method for synthesizing 3-alkenyl-1, 6-diacid by using electrochemical reaction
  • Method for synthesizing 3-alkenyl-1, 6-diacid by using electrochemical reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Put 5.0mmol of tetramethylammonium bromide and 35mL of acetonitrile into a high-pressure electrolytic cell without a diaphragm lined with polytetrafluoroethylene, and feed 1,3-butadiene gas with a pressure of 2 standard atmospheres , when 7.0mmol 1,3-butadiene is dissolved into the high-pressure electrolyte (tetramethylammonium bromide and acetonitrile), the solution is saturated, and then carbon dioxide gas is introduced to make the pressure of the electrolytic cell 3MPa, with silver as the cathode, Aluminum is used as the anode, connected with 0.06A direct current, and the reaction stops when 2F of electricity per mole of 1,3-butadiene is passed through, and the reaction lasts for 6.3 hours.

[0047] (2) Filter the liquid in the electrolytic cell, keep the filtrate for recycling, vacuum-dry the filter residue at 80°C for 1 hour, add 50ml of hydrochloric acid solution with a mass fraction of 35% for acidification, stir for 4 hours, extract 3 times with 30ml of ether...

Embodiment 2

[0050] (1) Put 5.0mmol tetramethylammonium bromide, 35mL dimethyl sulfoxide, and 6.9mmol 2-methyl-1,3-butadiene into a high-pressure electrolytic cell without a diaphragm lined with polytetrafluoroethylene In the process, carbon dioxide gas is introduced again so that the pressure of the electrolytic cell is 1MPa, silver and aluminum are used as the cathode and anode, and a 0.06A direct current is connected, and the reaction stops when 2F of electricity is introduced per mole of 1,3-butadiene, and the reaction It took 6.2 hours.

[0051] (2) Filter the liquid in the electrolytic cell, keep the filtrate for recycling, vacuum-dry the filter residue at 80°C for 1 hour, add 50ml of hydrochloric acid solution with a mass fraction of 35% for acidification, stir for 6 hours, extract 3 times with 30ml of ether, and combine the extractions The final solution was evaporated to dryness to obtain the crude product, and the mixed solution of 50ml of dichloromethane and ethanol (20:1 by vol...

Embodiment 3

[0053] (1) Put 5.0mmol of tetramethylammonium bromide, 35mL of acetonitrile, and 6.9mmol of 2,3-dimethyl-1,3-butadiene into a high-pressure electrolytic cell without a diaphragm lined with polytetrafluoroethylene , and then pass in carbon dioxide gas, so that the pressure of the electrolytic cell is 3MPa, with silver and aluminum as the cathode and anode, connected with 0.06A direct current, and stop the reaction when 1F of electricity per mole of 1,3-butadiene is passed in, and the reaction is complete. 3 hours.

[0054] (2) Filter the liquid in the electrolytic cell, keep the filtrate for recycling, vacuum-dry the filter residue at 80°C for 1 hour, add 50ml of hydrochloric acid solution with a mass fraction of 35% for acidification, stir for 3 hours, extract 3 times with 30ml of ether, and combine the extractions The final solution was evaporated to dryness to obtain the crude product, and the mixed solution of 30ml dichloromethane and ethanol (20:1 by volume) was heated to ...

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Abstract

The invention discloses a method for synthesizing 3-alkenyl-1, 6-diacid by using electrochemical reaction, which comprises the following steps of: adding organic ammonium salt and organic solvent into a diaphragm-free high pressure electrolytic cell, adding a 1, 3-diolefin compound into the electrolytic cell, then introducing carbon dioxide into the electrolytic cell, filtering the liquid in the high pressure electrolytic cell after the electrochemical reaction, drying filter residues, then acidifying the filter residues, extracting the acidified filter residues by ether, evaporating the extracted solution to obtain a coarse product of the 3-alkenyl-1, 6-diacid, and re-crystallizing the coarse product to obtain a pure product. The method is performed under mild electrochemical conditions, so the method is environment-friendly; the raw materials are cheap and easy to be obtained, need no additional catalyst, have high selectivity and are applicable to industrialization; and the method can efficiently convert and utilize the carbon dioxide, and has double values of economy and environmental protection.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a method for synthesizing 3-ene-1,6-dioic acid by electrochemical reaction. Background technique [0002] Adipic acid is an important chemical raw material, mainly used in the production of nylon 66, polyurethane, synthetic resin and plasticizer. [0003] The synthesis process of adipic acid can be divided into the following four methods according to the raw materials: ①KA oil (a mixture of cyclohexanol and cyclohexanone) method; ②C 4 olefin method; ③cyclohexene method; ④biological method. [0004] ① KA oil (a mixture of cyclohexanol and cyclohexanone) method: KA oil method is the main process of adipic acid synthesis. This method generally synthesizes KA oil first, and then oxidizes KA oil to synthesize adipic acid. The raw material for synthetic kA oil is generally cyclohexane (88%), and benzene (5%) or phenol (7%) can also be used [0005] The oxidation of KA oil i...

Claims

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Application Information

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IPC IPC(8): C25B3/00
Inventor 江焕峰李传华袁高清戚朝荣姬小趁
Owner SOUTH CHINA UNIV OF TECH
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