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A clean production process for converting sodium camphorsulfonate into camphorsulfonic acid

A technology of sodium camphorsulfonate and camphorsulfonic acid, which is applied in the fields of sulfonic acid preparation and organic chemistry, can solve the problems of low total yield, long production cycle, poor product purity, etc., and achieve the goal of reducing circulation volume and saving energy consumption Effect

Active Publication Date: 2017-03-15
厦门欣赛科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the chemical industry synthesizes camphorsulfonic acid mainly by first synthesizing sodium camphorsulfonate or sodium camphorsulfonate solution, and then carrying out continuous ion exchange by fixed bed to obtain camphorsulfonic acid solution; often there is a long production cycle and relatively low total yield. Low, poor product purity needs further separation and purification, etc.

Method used

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  • A clean production process for converting sodium camphorsulfonate into camphorsulfonic acid
  • A clean production process for converting sodium camphorsulfonate into camphorsulfonic acid
  • A clean production process for converting sodium camphorsulfonate into camphorsulfonic acid

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Experimental program
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Effect test

Embodiment 1

[0040] Wherein: the raw material liquid in the step 1 adopts 25% sodium camphorsulfonate solution, adopts the ceramic membrane that aperture is 50nm; Hydrochloric acid and sodium hydroxide are 4% sodium hydroxide;

Embodiment 2

[0042] Wherein: the raw material solution in the step 1 adopts 15% sodium camphorsulfonate solution, and adopts the ceramic membrane that the aperture is 100nm; Hydrochloric acid and sodium hydroxide are 4% sodium hydroxide;

Embodiment 3

[0044] Wherein: the raw material liquid in the step 1 adopts 30% sodium camphorsulfonate solution, adopts the ceramic membrane that aperture is 200nm; Hydrochloric acid and alkali are 4% sodium hydroxide.

[0045] The result is as follows:

[0046]

[0047] It can be seen from the above table that the positive calculation yields of the three batches of experiments are all above 100%. Excluding the error in weighing, it can be seen that there is basically no loss in the product. At the same time, it can be seen from the color change of the resin on site The conversion is very thorough.

[0048] The camphorsulfonic acid solution obtained by continuous ion exchange is concentrated by reverse osmosis, concentrated by MVR, crystallized, centrifuged, and crystals are dried. After the crystals of camphorsulfonic acid are tested, the purity of camphorsulfonic acid crystals can reach more than 99.7%, reaching pharmaceutical grade camphor Sulfonic acid levels.

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Abstract

The invention discloses a clear production technology for converting sodium camphorsulfonate into camphorsulfonic acid. The clear production technology comprises the following steps of step one, carrying out ceramic membrane filtration on a feed solution, and obtaining ceramic membrane dialysate; step two, enabling the ceramic membrane dialysate to enter a bipolar membrane electrodialysis system to carry out bipolar membrane electrodialysis, and obtaining a crude camphorsulfonic acid solution; step three, enabling the ceramic membrane dialysate to enter a continuous ion exchange system to carry out continuous ion exchange, and obtaining a camphorsulfonic acid solution; step four, carrying out reverse osmosis concentration on the camphorsulfonic acid solution, and obtaining a camphorsulfonic acid concentrated solution; step 5, obtaining camphorsulfonic acid crystals through crystallizing, centrifugal separation and crystal drying after carrying out mechanical vapor recompression concentration on the camphorsulfonic acid concentrated solution. According to the camphorsulfonic acid crystals produced by adopting the clear production technology disclosed by the invention, the purity can be more than 99.5 percent, and the crystals reach the pharmaceutical-grade camphorsulfonic acid level; meanwhile, a one-step recovery rate of materials can be more than 95 percent, the cycling volume is reduced, and energy consumption is reduced.

Description

technical field [0001] The invention relates to the field of camphorsulfonic acid production, in particular to a production process for converting sodium camphorsulfonate into camphorsulfonic acid. Background technique [0002] Camphor mainly exists in camphor plant camphor wood, zingiberaceae and alpiniae seeds, and is an indispensable raw material for medicine, daily use and national defense industry. According to its source, camphor is mainly divided into two categories: natural and synthetic. Natural camphor is mainly extracted from the essential oils of Lauraceae plants, and generally has dextrorotatory optical activity; synthetic camphor is made from turpentine through major chemical reactions such as isomerization, acetic acid addition esterification, hydrolysis and dehydrogenation, and is racemized. body. [0003] Camphorsulfonic acid is a derivative of camphor and has a chiral counterpart structure. According to its optical properties, it can be divided into left-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/19C07C303/22
CPCC07C303/22C07C309/19
Inventor 卢伯福
Owner 厦门欣赛科技有限公司
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