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Novel environment-friendly production process of 1-naphthol-4-sulfonic acid

A new process, sulfonic acid technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of difficult separation of isomers, waste of energy and environment, and many by-products, so as to reduce SO2 pollution and resource waste, and save acid resources. , the effect of increasing the conversion rate

Inactive Publication Date: 2015-06-24
叶良梅
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are mainly two synthetic methods of nivinic acid: one is prepared by sulfonation of methyl naphthol as a raw material, but this method has many by-products and isomer separation is difficult; the other is based on 4-amino Sodium sulfonate is used as a raw material, and it undergoes an addition reaction with sodium bisulfite in the presence of hydrochloric acid, and further hydrolyzes and acid precipitates to obtain the finished product. When this process is used to produce Nivinic acid dyes, it consumes more acid and needs to be heated to 90°C for 8 hours. Hours to get rid of sulfur dioxide, waste more energy and easily cause environmental pollution

Method used

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  • Novel environment-friendly production process of 1-naphthol-4-sulfonic acid
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  • Novel environment-friendly production process of 1-naphthol-4-sulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 600kg of sodium 4-sulfamate into the dissolving pot, add 1200kg of water, heat up to 95°C, then add 73.5kg of liquid caustic soda, stir to dissolve completely, then put it into a sealed enamel reaction pot with a volume of 3000L, and heat up to 100°C , feed SO at a flow rate of 10kg / h 2 After 1 hour, samples were taken to determine the end point of the reaction. Then put 450kg of liquid caustic soda with a mass concentration of 40% in the ammonia release concentration pot, heat up to 100°C, press in a certain amount of hydrolyzate to make the pH of the solution reach 12, heat up to 100°C to drive out the ammonia gas, and inject the above A batch of acid analysis of all the mother liquor, concentrated to d = 1.21g / cm 3 , filter to remove impurities. The filtrate was blown dry with steam, poured into an acid analysis kettle, added hydrochloric acid while it was hot until the pH value of the solution was 3, filtered to take the filter cake, blown dry to obtain 391 kg...

Embodiment 2

[0027] Add 600kg of sodium 4-sulfamate into the dissolving pot, add 1200kg of water, heat up to 95°C, then add 73.5kg of liquid caustic soda, stir to dissolve completely, then put it into a sealed enamel reaction pot with a volume of 3000L, and heat up to 100°C , feed SO at a flow rate of 10.5kg / h 2 After 1 hour, samples were taken to determine the end point of the reaction. Then put 450kg of liquid caustic soda with a mass concentration of 40% in the ammonia release concentration pot, heat up to 100°C, press in a certain amount of hydrolyzate to make the pH of the solution reach 12, heat up to 100°C to drive out the ammonia gas, and inject the above A batch of acid analysis of all the mother liquor, concentrated to d = 1.22g / cm 3 , filter to remove impurities. The filtrate was blown dry with steam, poured into an acid analysis kettle, added hydrochloric acid while it was hot until the pH value of the solution was 3, filtered to take the filter cake, blown dry to obtain 395k...

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Abstract

The invention relates to a novel environment-friendly production process of 1-naphthol-4-sulfonic acid. The production process comprises the following steps: adding 4-sodium sulfamate into a dissolving pot; adding water; heating and adding liquid caustic soda; stirring until the liquid caustic soda is completely dissolved; pumping the solution into an enamel reaction kettle; circulating in a sealed system; heating and introducing SO2 to perform hydrolysis reaction; putting the liquid caustic soda in an ammonia discharging concentration kettle; heating to the temperature of 100 DEG C; charging a hydrolyzing solution; regulating the pH of the solution; heating to completely dispel ammonia gas; charging all mother solution of the last batch of acid eduction; concentrating; filtering to remove impurities; blowing away filtrate by steam; pumping into an acid eduction kettle; adding hydrochloric acid to regulate the pH of the solution when the filtrate is hot; filtering and taking a filter cake; and drying the filter cake by blowing air to obtain NW acid and packaging. By adopting SO2 as a raw material, the production process disclosed by the invention has the advantages of greatly increasing the conversion ratio of the 4-sodium sulfamate to be as high as 100%, also saving about 50% of sulfur resources, lowering the production cost and causing small environmental pollution.

Description

technical field [0001] The invention relates to providing a new environmentally friendly production process of 1-naphthol-4-sulfonic acid, which belongs to the technical field of fine chemicals. Background technique [0002] 1-Naphthol-4-sulfonic acid, referred to as Nivenic acid for short, is an important dye intermediate, such as used in the manufacture of direct copper blue BR and 2R, direct violet RB, acid red B and acid medium bordeaux B and other dyes. At present, there are mainly two synthetic methods of nivinic acid: one is prepared from methyl naphthol by sulfonation, but this method has many by-products and isomer separation is difficult; the other is based on 4-amino Sodium sulfonate is used as a raw material, and it undergoes an addition reaction with sodium bisulfite in the presence of hydrochloric acid, and further hydrolyzes and acid precipitates to obtain the finished product. When this process is used to produce Nivinic acid dyes, it consumes more acid and n...

Claims

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Application Information

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IPC IPC(8): C07C303/02C07C309/43
Inventor 叶良梅
Owner 叶良梅
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