Clean production process for converting camphor ammonium sulfonate into camphorsulfonic acid

A technology of ammonium camphorsulfonate and camphorsulfonic acid, which is applied in the preparation of sulfonic acid, preparation of organic compounds, organic chemistry, etc., can solve the problems of long production cycle, low total yield, poor product purity, etc. Small size, simple process and compact equipment

Active Publication Date: 2016-04-06
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 ammonium camphorsulfonate solution, and then making camphorsulfonic acid solution through continuous ion exchange in a fixed bed; Low, poor product purity needs further separation and purification, etc.

Method used

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  • Clean production process for converting camphor ammonium sulfonate into camphorsulfonic acid
  • Clean production process for converting camphor ammonium sulfonate into camphorsulfonic acid
  • Clean production process for converting camphor ammonium sulfonate into camphorsulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Wherein: the raw material liquid in step 1 adopts 25% ammonium camphorsulfonate solution, adopts the ceramic membrane that aperture is 50nm; Hydrochloric acid and sodium hydroxide are 4% sodium hydroxide;

Embodiment 2

[0041] Wherein: the raw material solution in step 1 adopts 15% ammonium camphorsulfonate solution, adopts the ceramic membrane that aperture is 100nm; Hydrochloric acid and sodium hydroxide are 4% sodium hydroxide;

Embodiment 3

[0043] Wherein: the raw material liquid in the step 1 adopts 30% ammonium camphorsulfonate solution, adopts the ceramic membrane that aperture is 200nm; Hydrochloric acid and alkali are 4% sodium hydroxide.

[0044] The result is as follows:

[0045]

[0046]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.

[0047] 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 camphorsulfonic acid crystals are tested, the purity of the camphorsulfonic acid crystals can reach more than 99.5%, reaching pharmaceutical grade camphor. Sulfonic acid levels.

[0048] In addit...

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Abstract

The invention discloses a clean production process for converting camphor ammonium sulfonate into camphorsulfonic acid. The clean production process comprises the following steps of step 1, filtering a feed solution by a ceramic membrane to obtain a ceramic membrane dialysate; step 2, enabling the ceramic membrane dialysate to enter into a continuous ion exchange system for performing continuous ion exchange to obtain a camphorsulfonic acid solution, and filling a separation unit of the continuous ion exchange system with strong acid cation exchange resin; step 3, performing reverse osmosis concentration on the camphorsulfonic acid solution to obtain a camphorsulfonic acid concentrated solution; step 4, performing mechanical steaming and compressive concentration on the camphorsulfonic acid concentrated solution, and then performing crystallization, centrifugal separation and crystal drying to obtain a camphorsulfonic acid crystal. The camphorsulfonic acid crystal produced by the clean production process for converting the camphor ammonium sulfonate into the camphorsulfonic acid, disclosed by the invention, can reach 99.5 percent or over 99.5 percent in purity, reaches the pharmaceutical grade level of the camphorsulfonic acid, and has the advantages of high yield, simple working procedure, good conversion effect, high purity of product, compact equipment, small occupied area and the like.

Description

technical field [0001] The invention relates to the field of camphorsulfonic acid production, in particular to a clean production process for converting ammonium 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 in...

Claims

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Application Information

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IPC IPC(8): C07C303/02C07C303/44C07C309/19
CPCC07C303/02C07C303/44C07C309/19
Inventor 卢伯福
Owner 厦门欣赛科技有限公司
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