A kind of preparation technology of 2-aminonaphthalenesulfonic acid mixture

A technology for preparing aminonaphthalenesulfonic acid and its preparation technology is applied in the field of preparation technology of 2-aminonaphthalenesulfonic acid mixture, which can solve the problems of low utilization rate of 2-naphthol, great difficulty in environmental protection treatment, large amount of waste acid, etc., and achieve improvement Utilization rate, less waste acid, and simple process

Active Publication Date: 2020-11-06
SHANDONG CHUANGLAN YAOSHI ENVIRONMENTAL PROTECTION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that the amount of waste acid is large, the environmental protection treatment is difficult, the utilization rate of 2-naphthol is low, and less than 60% of 2-naphthol is finally converted into 2-amino-3,6,8-naphthalenetrisulfonic acid

Method used

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  • A kind of preparation technology of 2-aminonaphthalenesulfonic acid mixture
  • A kind of preparation technology of 2-aminonaphthalenesulfonic acid mixture
  • A kind of preparation technology of 2-aminonaphthalenesulfonic acid mixture

Examples

Experimental program
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Effect test

Embodiment 1

[0057] In a stirring four-neck flask, add 110g of 98% sulfuric acid, add 100g of 2-naphthol under stirring and cooling, stir for half an hour, then add 190g of 105% sulfuric acid and react at about 80°C for 12 hours. After the reaction, Put the sulfonated compound into 500g of 22% ammonia water, add ammonia water to adjust the ammonia value to about 4.5%, add 60g of ammonium sulfite, react at a temperature of 180°C for 16 hours, cool down, deammoniate, neutralize with 50% sulfuric acid, remove sulfur dioxide, cool down, Suction filtration and drying to obtain 268g of the product, which is a mixture of 2-aminonaphthalenesulfonic acid, with an amino value of 72.3% (calculated as 2-amino-6,8-naphthalenedisulfonic acid)

Embodiment 2

[0059] Add 1000 parts of 100% sulfuric acid to the sulfonation tank, add 1000 parts of 2-naphthol under stirring and cooling, stir for half an hour after adding, then add 1650 parts of 105% sulfuric acid, react at about 80 ° C for 10 hours, and sulfonate Put in 25% ammonia water, finally adjust and neutralize the liquid ammonia value to about 4.5%, add 600 parts of ammonium sulfite, react at 170°C for 18 hours, cool down, deammoniate, neutralize with 50% sulfuric acid, remove sulfur dioxide, cool down, and filter with suction , oven dry, obtain 2968 parts of products, be 2-amino naphthalene sulfonic acid mixture, amino value 68.3%. (calculated as 2-amino-6,8-naphthalene disulfonic acid)

Embodiment 3

[0061] Take 1300 parts of the dried 2-aminonaphthalenesulfonic acid mixture and sulfonate it in 2650 parts of 65% oleum at a temperature of 135-140°C for 12 hours. Dilute the sulfonated solution in 1800 parts of water to adjust the reaction solution The concentration of sulfuric acid is 38-40%. After cooling down, filter to obtain 1426 parts of the product with a content of 72.6%. Based on 2-naphthol, the yield of 2-amino-3,6,8-naphthalenetrisulfonic acid is 88.94%, and the chromatographic purity of the product is 99.58%.

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Abstract

The invention discloses a preparation technology for a 2-sulfonaphtine mixture. The preparation technology comprises the following steps: enabling 2-naphthol to be subjected to sulfonation in sulfuricacid of which the mass fraction is 98-100% and fuming sulphuric acid of which the mass fraction of the sulfuric acid is 105%, to obtain sulfonation liquid of a mixture containing 2-hydroxyl-6,8-naphthalene disulfonic acid, 2-hydroxyl-3,6-naphthalene disulfonic acid and 2-naphthol monosulfonic acid, adding ammonia water to the sulfonation liquid for regulating an ammonia value, adding ammonium sulfite for catalytic-aminolysis, and adding dilute sulphuric acid for acidizing, to obtain a mixture of 2-amino-6,8-naphthalene disulfonic acid, 2-amino-3,6-naphthalene disulfonic acid and 2-amino monosulfonic acid, namely the 2-sulfonaphtine mixture. The mixture is capable of sulfonating in 115% of the fuming sulphuric acid so as to obtain 2-amino-3,6,8-naphthalene trisulfonic acid. The preparationtechnology is capable of greatly improving the utilization ratio of the 2-naphthol.

Description

technical field [0001] The invention relates to a production process of 2-amino-3,6,8-naphthalenetrisulfonic acid, in particular to the preparation of a raw material for preparing 2-amino-3,6,8-naphthalenetrisulfonic acid-2-aminonaphthalenesulfonic acid mixture craft. Background technique [0002] 2-Amino-3,6,8-naphthalenetrisulfonic acid, also known as K acid, is an important dye intermediate, mainly used in the fields of azo dyes, reactive dyes and organic pigments, and the use of K acid in industrial production The demand is high. [0003] The traditional production process of 2-amino-3,6,8-naphthalene trisulfonic acid is to produce 2-hydroxy-6.8-naphthalene disulfonic acid potassium after sulfonation of 2-naphthol, and then produce 2-amino- 6.8-naphthalene disulfonic acid, and then sulfonated to produce 2-amino-3.6.8-naphthalene trisulfonic acid. The disadvantage of this process is that the amount of waste acid is large, the environmental protection treatment is diffi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/47C07C303/06C07C303/22
CPCC07C303/06C07C303/22C07C309/43C07C309/47
Inventor 王在军任帅昌刘文静杨海军李宗泉张克宏
Owner SHANDONG CHUANGLAN YAOSHI ENVIRONMENTAL PROTECTION TECH CO LTD
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