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Method for recovering camphorsulfonic acid

A technology of camphorsulfonic acid and camphorsulfonate, which is applied in the field of medicine and chemical industry, can solve the problems of production process safety hazards, low recovery rate, air pollution, etc., and achieve the effects of low production cost, environmental friendliness and simple operation procedures

Active Publication Date: 2019-06-21
WUHAN WUYAO PHARMA
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0008] (1) the camphorsulfonic acid aqueous solution after the acidification will have a large amount of camphorsulfonic acid degradation in the concentration process, cause the camphorsulfonic acid recovery rate to be low, and the camphorsulfonic acid quality of reclaiming is not good;
[0009] (2) The acidified aqueous solution of camphorsulfonic acid will produce degraded acid gas sulfur dioxide during the concentration process, which will corrode equipment and pollute the air, and there are potential safety hazards in the production process
[0012] (1) The construction cost of ceramic membrane system, bipolar membrane electrodialysis system and ion exchange system is high, and the aqueous solution containing sodium camphorsulfonate is inefficient;
[0013] (2) A large amount of high-salt wastewater will be produced in the ion exchange process, and inorganic salts cannot be effectively recycled;
[0014] (3) Ceramic membrane system, bipolar membrane electrodialysis system and ion exchange system are easily polluted by polymer impurities, inorganic impurities and organic impurities, resulting in short service life and high recycling costs, which are not suitable for large-scale industrialization Recovery of camphorsulfonic acid
[0017] (1) Sodium camphorsulfonate is very soluble in water, and after cooling and crystallization, it will also dissolve in a large amount in the water phase, so the recovery rate is not high;
[0018] (2) After acidification of sodium camphorsulfonate, it is necessary to filter out the inorganic salts therein, otherwise, after cooling down and crystallizing, a large amount of inorganic salts will remain in the camphorsulfonic acid, causing the quality of the recovered camphorsulfonic acid to fail to meet the requirements, such as its optical rotation and melting point can not meet the commercial standard
[0019] Therefore, due to above-mentioned technical defect, according to the result of repeated experiment of this invention embodiment, can not obtain the camphorsulfonic acid that meets its described rate of recovery and quality standard

Method used

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  • Method for recovering camphorsulfonic acid
  • Method for recovering camphorsulfonic acid
  • Method for recovering camphorsulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0073] Add an aqueous solution containing camphorsulfonic acid to a 1L three-neck flask, and measure the pH. If the pH is not neutral, neutralize with concentrated hydrochloric acid or sodium carbonate. Add 0.01 (w / w) activated carbon, heat to 50-60°C and stir to react for 2 hours, then filter to remove activated carbon. The filtrate is concentrated under reduced pressure at 50-60°C to remove water, and the vacuum degree is ≤-0.08MPa. After the water is concentrated to dryness, lower the temperature to 20-30°C, add 3 times the concentrated solid weight of dichloromethane, beat the slurry and stir for 1 hour, then filter, and transfer the filter cake to an oven at 50-60°C to dry to constant weight. Transfer the dried solid to a 500ml three-neck flask, add 3 times the solid weight of absolute ethanol, dropwise add 1.1 times the equivalent of camphorsulfonate HCl / ethanol solution, control the temperature at 10-20°C, keep stirring for 1 hour, and pump After filtration, the filtr...

Embodiment 2

[0075] Add an aqueous solution containing camphorsulfonic acid to a 1L three-neck flask, and measure the pH. If the pH is not neutral, neutralize with concentrated hydrochloric acid or sodium carbonate. Add 0.02 (w / w) activated carbon, heat to 50-60°C and stir to react for 2 hours, then filter to remove activated carbon. The filtrate is concentrated under reduced pressure at 50-60°C to remove water, and the vacuum degree is ≤-0.08MPa. After the water is concentrated to dryness, lower the temperature to 20-30°C, add 3 times the concentrated solid weight of dichloromethane, beat the slurry and stir for 1 hour, then filter, and transfer the filter cake to an oven at 50-60°C to dry to constant weight. Transfer the dried solid to a 500ml three-neck flask, add 3 times the solid weight of absolute ethanol, dropwise add 1.1 times the equivalent of camphorsulfonate HCl / ethanol solution, control the temperature at 10-20°C, keep stirring for 1 hour, and pump After filtration, the filtr...

Embodiment 3

[0077] Add an aqueous solution containing camphorsulfonic acid to a 1L three-neck flask, and measure the pH. If the pH is not neutral, neutralize with concentrated hydrochloric acid or sodium carbonate. Add 0.10 (w / w) activated carbon, heat to 50-60°C and stir to react for 2 hours, and filter to remove activated carbon. The filtrate is concentrated under reduced pressure at 50-60°C to remove water, and the vacuum degree is ≤-0.08MPa. After the water is concentrated to dryness, lower the temperature to 20-30°C, add 3 times the concentrated solid weight of dichloromethane, beat the slurry and stir for 1 hour, then filter, and transfer the filter cake to an oven at 50-60°C to dry to constant weight. Transfer the dried solid to a 500ml three-neck flask, add 3 times the solid weight of absolute ethanol, dropwise add 1.1 times the equivalent of camphorsulfonate HCl / ethanol solution, control the temperature at 10-20°C, keep stirring for 1 hour, and pump After filtration, the filtra...

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Abstract

The present invention discloses a method for recovering camphorsulfonic acid. The method comprises: (1) neutralizing an aqueous solution containing camphorsulfonic acid; (2) decolorizing the aqueous solution containing camphorsulfonic acid after the neutralizing; (3) carrying out concentrating dewatering on the decolorized aqueous solution containing camphorsulfonic acid, beating with an organic solvent, filtering, and drying the filter cake to obtain camphor sulfonate; and (4) acidifying the camphor sulfonate obtained in the step (3) to obtain camphorsulfonic acid. According to the present invention, the process for recovering camphorsulfonic acid from the aqueous solution containing camphorsulfonic acid has characteristics of simple operation step, low production cost and environmental friendliness, and is suitable for the recovery of camphorsulfonic acid from aqueous solutions containing camphorsulfonic acid in the industrialization process.

Description

technical field [0001] The application relates to a method for recovering camphorsulfonic acid, which belongs to the field of medicine and chemical industry. Background technique [0002] Camphorsulphonic acid (Camphorsulphonic acid, CAS number: 3144-16-9, molecular formula: C 10 h 16 o 4 S) is a sulfonic acid derivative of camphor, which is mainly produced industrially by sulfonating camphor as a raw material. Camphorsulfonic acid has a chiral structure and has two optical isomers, L-camphorsulfonic acid and D-camphorsulfonic acid, and is an important chiral resolution agent. For example, US Pat. No. 4,847,265 reported that L-camphorsulfonic acid was applied to the resolution of the platelet aggregation inhibitor clopidogrel. In addition, camphorsulfonic acid can also be used as a chiral ion pair reagent for the separation and analysis of chiral drugs. The optical isomer structural formula of camphorsulfonic acid is shown in the following formula: [0003] [0004]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/44C07C303/32C07C303/02C07C309/19
Inventor 赵涛涛洪健张伟艾娇皮金红张琦张光槐谢国范吴鸣
Owner WUHAN WUYAO PHARMA
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