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Prepn of 2-naphthylamine-3,6,8-trisulfonic acid

A technology of trisulfonic acid and naphthylamine, applied in chemical instruments and methods, azo dyes, organic dyes, etc., can solve the problems of preparation that have not been reported, and achieve the effects of easy availability of raw materials, wide application range, and high yield

Inactive Publication Date: 2007-01-03
浙江海晨化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Also have report 2-naphthylamine-1,5, the separation method of 7-trisulfonic acid in addition, and the preparation of 2-naphthylamine-3,6,8-trisulfonic acid of the present invention has no report

Method used

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  • Prepn of 2-naphthylamine-3,6,8-trisulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Add 2200 parts (parts by weight, the same below) of 65% oleum into the sulfonation pot, and add 656 parts of dried amino G salt in batches under stirring. The feeding temperature does not exceed 70°C. After the addition, close the sulfonation pot, heat it to 125°C, and keep it at 125-140°C for 6 hours, with a pressure of 1-2 kg / cm2. Cool down to 100°C, and dilute the sulfonated compound into a dilution pot filled with 3000 parts of water. Dilution time is about 1-2 hours, the temperature after dilution is 110-120° C., the concentration of sulfuric acid is in the range of 40-50%, and it is incubated under this condition for 1-2 hours. Cool down to 25-35°C, filter to obtain 770 parts of amino acid K. The yield was 92.88%, and the purity by liquid chromatography analysis was 99.8%.

Embodiment 2

[0020] Add 2200 parts (parts by weight, the same below) of 65% oleum into the sulfonation pot, and add 656 parts of dried amino R salt in batches under stirring. The feeding temperature should not exceed 70°C. After the addition, the sulfonation pot should be closed and heated to 125°C for 6 hours, with a pressure of 1-2 kg / cm2. Cool down to 100°C, and dilute the sulfonated compound into a dilution pot filled with 3000 parts of water. The dilution time is about 2-3 hours, the temperature after dilution is 110-120° C., the concentration of sulfuric acid is in the range of 35-50%, and the temperature is kept for 1-2 hours under this condition. Cool down to 25-35°C, filter to obtain 770 parts of amino acid K. Yield 88%, liquid chromatography analysis purity 99.64%

Embodiment 3

[0022] Add 2300 parts (parts by weight, hereinafter the same) 65% oleum into the sulfonation pot, add the mixture formed by mixing the dried amino G salt, amino R salt and Bronic acid in batches with a stirring rate of 710.5% Among them, 576 parts of amino G salt; 108 parts of amino R salt; 26.5 parts of bronnic acid. The feeding temperature does not exceed 70°C. After the addition, close the sulfonation pot, heat it to 125°C, and keep it at 125-140°C for 6 hours, with a pressure of 1-2 kg / cm2. Cool down to 100°C, and dilute the sulfonated compound into a dilution pot filled with 3000 parts of water. The dilution time is about 1-2 hours. Cool down to 25-35°C, filter to obtain 871.7 parts of amino acid K. The yield was 95.8%, and the purity by liquid chromatography analysis was 99.63%.

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Abstract

The present invention discloses preparation process of 2-naphthylamine-3, 6, 8-trisulfonic acid. Amino G acid or its salt, Amino R acid or its salt, bulcoxic acid or its salt, or their mixture is reacted with fuming sulfuric acid with high concentration of SO3 at certain temperature and pressure for certain time to obtain high purity 2-naphthylamine-3, 6, 8-trisulfonic acid. The present invention is suitable for industrial production.

Description

technical field [0001] The present invention relates to the preparation method of compound in organic synthesis, more specifically refer to the preparation method of improved 2-naphthylamine-3,6,8-trisulfonic acid (ie amino K acid). Background technique [0002] Amino K acid is widely used as an important intermediate in the dye industry to prepare acid dyes and reactive dyes, usually using reaction steps such as sulfonation, salting out, amination, acid precipitation and then sulfonation. [0003] U.S. Patent 4,551,283 once mentioned the method that amino acid is separated from sulfonated mixture. In addition, the separation method of 2-naphthylamine-1,5,7-trisulfonic acid is also reported, but the preparation of 2-naphthylamine-3,6,8-trisulfonic acid of the present invention has not been reported. Contents of the invention [0004] The purpose of the present invention is to provide a preparation method for preparing 2-naphthylamine-3,6,8-trisulfonic acid, so as to overc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/35C09B62/00
Inventor 张七男李洪林颜晓明赵强
Owner 浙江海晨化工有限公司
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