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A kind of method that bipolar membrane electrodialysis prepares 1-10-camphorsulfonic acid

A bipolar membrane electrodialysis, L-10- technology, applied in the preparation of sulfonic acid, chemical instruments and methods, membrane technology, etc., to achieve the effect of avoiding the generation of secondary pollutants, avoiding the consumption of chemical reagents, and important industrial application value

Active Publication Date: 2021-11-12
HEFEI CHEMJOY POLYMER MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is currently no report on the conversion of L-10-ammonium camphorsulfonate to prepare L-10-camphorsulfonic acid by bipolar membrane electrodialysis

Method used

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  • A kind of method that bipolar membrane electrodialysis prepares 1-10-camphorsulfonic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] This embodiment adopts as figure 1 In the bipolar membrane electrodialysis device shown, the arrangement of the membrane stack is anode electrode-anode chamber-bipolar membrane-[acid chamber-anion exchange membrane-salt chamber-cation exchange membrane-alkali chamber-bipolar membrane] n -cathode compartment-cathode electrode, the number n of repeating units is 5. The anode and cathode materials in the membrane stack are corrosion-resistant titanium coated with ruthenium, and the compartments between adjacent ion exchange membranes, including acid chambers and alkali chambers, are composed of gaskets with flow channels and grids. is 0.8mm. The cation exchange membrane, anion exchange membrane and bipolar membrane used in the membrane stack are CJMC-3, CJMA-3, and CJBPM-2 produced by Hefei Science and Technology Polymer Material Technology Co., Ltd. The effective area of ​​a single membrane is 189cm 2 (9cm×21cm).

[0024] The anode chamber and the cathode chamber are c...

Embodiment 2

[0027] The bipolar membrane electrodialysis device used in this embodiment is the same as that in Embodiment 1.

[0028] The anode chamber and the cathode chamber are connected in series, and 500mL 0.3mol / L Na 2 SO 4 The aqueous solution is used as a strong electrolyte, and 1000mL of 200g / L L-10-ammonium camphorsulfonate solution (conductivity 26mS / cm) is passed into the salt chamber in the bipolar membrane electrodialysis membrane stack to the bipolar membrane electrodialysis membrane stack 800mL of deionized water was passed into the acid chamber and alkali chamber respectively. During the experiment, the linear flow velocity of each compartment solution flowing in the membrane stack was 4cm / s, operated at constant voltage, the membrane stack voltage was set to 15V, and the upper limit of the current density was set to 50mA / cm 2 .

[0029] The experiment runs until the conductivity of the salt chamber drops to 500 μS / cm, and the conversion rate of L-10-ammonium camphorsul...

Embodiment 3

[0031] The bipolar membrane electrodialysis device used in this embodiment is the same as that in Embodiment 1.

[0032] The anode chamber and the cathode chamber are connected in series, and 500mL 0.3mol / L Na 2 SO 4 The aqueous solution is used as a strong electrolyte, and 1000mL of 200g / L L-10-ammonium camphorsulfonate solution (conductivity 26mS / cm) is passed into the salt chamber in the bipolar membrane electrodialysis membrane stack to the bipolar membrane electrodialysis membrane stack 800mL of deionized water was passed into the acid chamber and alkali chamber respectively. During the experiment, the linear flow velocity of each compartment solution flowing in the membrane stack was 4cm / s, operated at constant voltage, the membrane stack voltage was set to 20V, and the upper limit of the current density was set to 50mA / cm 2 .

[0033] The experiment runs until the conductivity of the salt chamber drops to 300 μS / cm, and the conversion rate of L-10-ammonium camphorsul...

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Abstract

The invention discloses a method for preparing L-10-camphorsulfonic acid by bipolar membrane electrodialysis. A bipolar membrane electrodialysis device is used to first feed L-10-camphor into a salt chamber in a bipolar membrane electrodialysis membrane stack. The ammonium sulfonate solution is passed into deionized water respectively to the acid chamber and the alkali chamber in the bipolar membrane electrodialysis membrane stack, and the strong electrolyte solution is respectively passed into the anode chamber and the cathode chamber in the bipolar membrane electrodialysis membrane stack; then Applying a direct current to both ends of the bipolar membrane electrodialysis membrane stack can realize the conversion of L-10-ammonium camphorsulfonate to prepare L-10-camphorsulfonic acid. The conversion rate of L-10-ammonium camphorsulfonate in the bipolar membrane electrodialysis conversion process of the present invention can be as high as 98%, and the purity of the obtained product L-10-camphorsulfonic acid is as high as 99%. The preparation method is simple to operate, does not need to consume any chemical reagents, and avoids the problems of consumption of a large amount of chemical reagents and generation of secondary pollutants caused by the regeneration of the ion exchange resin after the use of the traditional ion exchange method.

Description

technical field [0001] The invention relates to a method for preparing L-10-camphorsulfonic acid by bipolar membrane electrodialysis, belonging to the technical field of organic acid production. Background technique [0002] Camphorsulfonic acid is a derivative of camphor and has a chiral counterpart structure. According to its chemical characteristics, it can be divided into left-handed and right-handed structures. Among them, left-handed camphorsulfonic acid (L-10-camphorsulfonic acid) is widely used in medicine, light industry and daily chemical industries. At present, the chemical synthesis of L-10-camphorsulfonic acid is mainly through first synthesizing ammonium camphorsulfonate solution, then obtaining L-10-ammonium camphorsulfonate through resolution, and then performing continuous ion exchange through a fixed bed to obtain L-10- Camphorsulfonic acid solution. This process often has a long production cycle, relatively low overall yield, poor product purity, and fur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/19C07C303/22B01D61/44
CPCB01D61/445C07C303/22C07C2602/42C07C309/19
Inventor 汪耀明颜海洋王晓林李为李传润吴亮徐铜文
Owner HEFEI CHEMJOY POLYMER MATERIALS CO LTD