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Recycling method of alkali fusion solution of 1-amino-8-naphthol-3,6-disulfonic acid

A technology of resource utilization and molten solution, which is applied in the field of resource utilization of H acid-base molten solution, can solve the problems of serious environmental pollution, difficult treatment, consumption of sulfuric acid, etc., and achieve the effects of reducing emissions, reducing consumption and saving costs

Active Publication Date: 2017-01-11
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process step (5) adds a large amount of liquid caustic soda or solid caustic soda for alkali fusion, and the alkali molten liquid contains more free alkali, but step (6) needs to add sulfuric acid to adjust the pH value to strong acidity, consume a large amount of sulfuric acid, and produce a large amount of free alkali at the same time Salt wastewater is difficult to treat and causes serious environmental pollution

Method used

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  • Recycling method of alkali fusion solution of 1-amino-8-naphthol-3,6-disulfonic acid
  • Recycling method of alkali fusion solution of 1-amino-8-naphthol-3,6-disulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 99% dichloropropanol 199g (1.527mol) in the 1000ml reactor, with negative pressure-0.085MPa, stir and heat up to 60°C, start to drop 500g of H acid-base solution, free alkali content 11% (converted to NaOH1. 375mol), H acid content 13.8%, dropwise addition time 90min, dropwise process keep kettle temperature 60 ~ 62 ℃, dropwise end, continue distillation 5min; The oil layer is 130.76g, and the gas spectrum analysis contains ECH85.26%, DCH13.23%, and the water separation layer is 201g, and the gas spectrum analysis contains ECH5.6%, DCH1.15%. Yield 96.5% (based on converted DCH).

Embodiment 2

[0022] Add 99% dichloropropanol 376.3g (2.888mol) in 1000ml reactor, bring negative pressure-0.095MPa, stir and heat up to 50 ℃, begin to dropwise add H acid-base solution 350g, free alkali content 16.5% (reduce NaOH1 .444mol), H acid content 13.8%, drop time 90min, dropwise process keep kettle temperature 49~52 ℃, dropwise finish, continue distillation 5min; Analysis; oil layer 368.9g, gas spectrum analysis contains ECH32.4%, DCH48.99%, water separation layer 175.5g, gas spectrum analysis contains ECH6.1%, DCH3.15%, according to the analysis calculation DCH conversion rate is 50%, ECH yield 97.5% (based on converted DCH).

Embodiment 3

[0024] Add 268.4g (2.06mol) of 99% dichloropropanol in a 1000ml reactor, stir and heat up to 45°C, start to add 350g of H acid-base solution dropwise, the free alkali content is 20% (NaOH1.75mol), and the H acid content 20%, adding time for 10 minutes, keep the temperature of the kettle at 45-50°C during the dropping process, continue to keep warm for 10 minutes after the dropping is completed; cool down the feed liquid, let it stand for 10 minutes, pour the clear liquid into the separatory funnel to separate layers, and separate the oil layer ①189. 3g, the brine layer was divided into the reaction kettle, stripped with negative pressure -0.09MPa until no oil drops were distilled, the distillate was poured into the separatory funnel to separate layers, the oil separation layer ② 6.93g, the water separation layer 97.5g, gas spectrometry analysis Contains 3.56% ECH and 1.98% DCH, combined two oil layer gas spectrometry analysis contains 79.1% ECH, 19.4% DCH; saponification kettle...

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Abstract

The invention relates to the field of organic chemistry, and concretely relates to a recycling method of an alkali fusion solution of 1-amino-8-naphthol-3,6-disulfonic acid. The recycling method of the alkali fusion solution of 1-amino-8-naphthol-3,6-disulfonic acid has the advantages of reduction of the sulfuric acid consumption in the acid precipitation process, cost saving, reduction of the discharge amount of salt-containing wastewater, and realization of production of a chemical product benefiting economy through recycling free alkalis in the alkali fusion solution.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a resource utilization method of H acid-base solution. Background technique [0002] H acid is an important naphthalene dye intermediate, widely used in printing and dyeing, textile, chemical and other industries. At present, the production process of most manufacturers mainly includes the following steps: (1) sulfonation of refined naphthalene to obtain naphthalene 1,3,6-trisulfonic acid, (2) nitration of naphthalene 1,3,6-trisulfonic acid to obtain nitrate (3) Alkaline neutralization, (4) Nitro acid is reduced by iron powder or hydrogenation reduction to obtain amino acid, (5) Alkali-melted amino acid is obtained H acid, (6) acid is precipitated H acid Products; patents JP50142546, DE3020441, GB1576608, CN101367753A, CN101381331A, etc. all disclose related processes. The production process step (5) adds a large amount of liquid caustic soda or solid caustic soda for alkali fu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/50C07C303/32C07D303/08C07D301/26
Inventor 史雪芳丁克鸿徐林田宇张晓谕谢峰聂庆超
Owner JIANGSU YANGNONG CHEM GROUP
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