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Preparation technique of 2-amido-3,6,8-naphthalenetrisulphonic acid

A technology for the preparation of naphthalene trisulfonic acid, which is applied in the fields of sulfonic acid preparation and organic chemistry, and can solve problems such as environmental hazards, high cost, and difficult wastewater treatment

Active Publication Date: 2011-06-15
青岛奥盖克化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] During the production of 2-amino-3,6,8-naphthalenetrisulfonic acid, a large amount of waste acid is produced, 8 tons of 15-20% waste acid per ton of product, 6.5 tons of 40% waste acid, potassium sulfate and ammonium sulfate 3.5 tons of waste water, waste water treatment is difficult and costly, some manufacturers directly discharge, causing great harm to the environment
[0004] Chinese patent CN1887863A reports the method for preparing 2-amino-3,6,8-naphthalene trisulfonic acid from 6,8-naphthalene disulfonate, and the present invention reclaims 2-naphthol through hydrolysis from sulfonation mother liquor and applies mechanically to The method for preparing 2-amino-3,6,8-naphthalenetrisulfonic acid has not been reported

Method used

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  • Preparation technique of 2-amido-3,6,8-naphthalenetrisulphonic acid
  • Preparation technique of 2-amido-3,6,8-naphthalenetrisulphonic acid
  • Preparation technique of 2-amido-3,6,8-naphthalenetrisulphonic acid

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Experimental program
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Embodiment 1

[0018] In the four-necked flask equipped with stirring, add 88g of 98% sulfuric acid, add 100g of 2-naphthol under stirring and cooling, stir for 30 minutes, then add 190g of 105% sulfuric acid, and react for 6 hours after the addition. After the reaction, the The sulfonate was added to a solution of 170 g of potassium sulfate dissolved in 600 ml of water, stirred for 2 hours after the addition, and filtered to obtain 240 g of the product, wherein the content of potassium 6,8-naphthalene disulfonate was 71%.

[0019] The above-mentioned potassium 6,8-naphthalene disulfonate was dissolved in a mixed solution of 260ml of ammonia water and 62ml of ammonium bisulfite, added to an autoclave, heated to 140°C, kept for 12 hours, cooled, the mother liquor was decolorized by activated carbon, acidified, and filtered , oven dry, obtain product 155g, wherein 7-amino-1,3-naphthalenedisulfonic acid (amino G acid) content is 82.6%.

[0020] Sulfonate 155g of the above-mentioned dried produc...

Embodiment 2

[0023] In a 3000L glass-lined reactor, add 88kg of 98% sulfuric acid. Add 1000kg of 2-naphthol under stirring and cooling. After the addition, stir for 30 minutes, then add 1900kg of 105% sulfuric acid, and react at 80-85°C for 6 hours after the addition. After the reaction, the sulfonate was added to a solution of 1700kg of potassium sulfate dissolved in 600kg of water at a temperature not exceeding 90°C, stirred for 2 hours after the addition, and filtered to obtain 6,8-naphthalene disulfonic acid with a content of 72.3%. Potassium 2458kg.

[0024] The above-mentioned potassium 6,8-naphthalene disulfonate was dissolved in a mixed solution of 2650L of ammonia water and 650L of ammonium bisulfite, added into an autoclave, heated to 140°C, and kept for reaction for 12 hours. The temperature was lowered, the mother liquor was decolorized by active carbon, acidified, filtered, and dried to obtain 1612 kg of 7-amino-1,3 naphthalene disulfonic acid with a content of 81.3%.

[002...

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Abstract

The present invention discloses a preparation technics for 2-amino-3,6,8-naphthalenesulfonic acid, which solves the problem of the large volume of wasted water drained by the technics in the prior art, and decreases the individual cost of the raw material of 2-naphthol, thereby decreasing the cost. The fabrication technics includes that 2-naphthol is sulfonated in sulphuric acid or oleum to produce 6,8-naphthalin-disulfuric acid (G acid), 3,7- naphthalin-disulfuric acid (R acid), and the other sulfuric acid derivatives of 2-naphtalins, then potassium sulphuric is added for crystallization to obtain 6,8-naphthalin-potassium disulfuric (G salt), the stock solution undergoes high-temperature hydrolysis, in which 3,7- naphthalin-disulfuric acid (R acid) and the other sulfuric acid derivativesof 2-naphtalins are hydrolyzed into 2-naphthalin, then the stock liquid is extracted, oxidized, decolored and condensed to retrieve the potassium sulphuric, which is recycled to procedure involved inthe production of 6,8-naphthalin-potassium disulfuric (G salt), which undergoes ammonolysis and sulfonation to produce 2-amino-3,6,8-naphthalintrisulfuric acid.

Description

technical field [0001] The invention relates to a preparation process of 2-amino-3,6,8-naphthalenetrisulfonic acid. technical background [0002] 2-Amino-3,6,8-naphthalenetrisulfonic acid is an important raw material for the production of reactive yellow M-3RE, which is one of the ternary colors of the color, and its dosage is more than 80,000 tons, requiring 2- Amino-3,6,8-naphthalene trisulfonic acid is about 15,000 tons. The direct dyes are not fast enough to the fabric and are easy to fade when washing. They have been gradually replaced by reactive dyes. Therefore, 2-amino-3,6 , The demand for 8-naphthalenetrisulfonic acid will also increase significantly. [0003] During the production of 2-amino-3,6,8-naphthalenetrisulfonic acid, a large amount of waste acid is produced, 8 tons of 15-20% waste acid per ton of product, 6.5 tons of 40% waste acid, potassium sulfate and ammonium sulfate The amount of waste water is 3.5 tons. Waste water treatment is difficult and costly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/47C07C303/06
Inventor 王在军沈允涛侯卫波李宗泉林国栋
Owner 青岛奥盖克化工股份有限公司
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