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Recovery comprehensive utilization method of disperse red 60 byproduct

A technology of disperse red and by-products, applied in the directions of alkali metal bromide, amino-hydroxyanthraquinone dyes, organic chemistry, etc., can solve the problems of high energy consumption, inability to change environmental pollution, and high consumption of phenol.

Active Publication Date: 2008-07-23
浙江长征化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing treatment of mother liquor water is to reclaim phenol through vacuum distillation, still contain phenol, disperse red 60, potassium bromide etc. in the distillation residue, product yield is low, phenol consumption is big, vacuum distillation process is complicated, energy consumption is big, The single-step condensation yield is only about 85-88%, the production cost is relatively high, and a large amount of hazardous solid waste is generated, which causes great environmental pollution.
There is also methanol added after the condensation reaction for separation, and the product quality has improved, but because the condensation reaction itself has not been improved, the yield is still low, the unit consumption of phenol is still high, and the boiling point of methanol is too low and is flammable. Explosive dangerous goods, there are serious safety hazards in the use process, and in the invention patent of CN 101003691A, 1-amino-2-bromo-4-hydroxyanthraquinone is used as a wet product filter cake as a condensation raw material, and solvents and antioxidants are also added , although the problem of drying the hydrolyzate has been solved, the comprehensive recovery and utilization of phenol in mother liquor water, disperse red 60 soluble in phenol, and potassium bromide cannot be solved, and the problem of high unit consumption of phenol and low yield cannot be solved. The status quo of environmental pollution
And the recovery and comprehensive utilization of the by-product potassium bromide in the condensation mother liquor water have not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the 4M 3 Condensation mother liquid water is poured into a 6300L enamel kettle with a pump, and stirring is started, and 60kg of 98% sulfuric acid and 50kg of sodium sulfate are slowly added. After the addition, stir for half an hour, and then separate layers to obtain an upper layer solution containing phenol and disperse red 60 dissolved in phenol, and a lower layer solution containing potassium bromide and phenol. Add alkali to the upper layer solution to adjust the pH to 6-9, which is the treated mother liquor water, which is used for the condensation reaction of Disperse Red 60. Pump the lower layer solution into a 5000L enamel kettle, start stirring, add 30kg of butyl acetate, add After completion, static stratification, the upper layer is phenol and butyl acetate layer, the lower layer of potassium bromide solution is pumped into the bromine recovery tower, through 47kg of chlorine gas and steam, until the temperature at the top of the tower reaches...

Embodiment 2

[0025] Embodiment 2: the 4M 3 Condensation mother liquid water is pumped into the enamel kettle of 6300L, starts stirring, slowly adds 250kg of 50% waste sulfuric acid and 90kg of sodium chloride, and the following process steps are the same as in Example 1. Pump the lower layer solution into a 5000L enamel kettle, start stirring, add 100kg of butyl acetate, after the addition is complete, let it stand for stratification, the upper layer is phenol and butyl acetate layer, and the lower layer of potassium bromide solution is pumped into the bromine recovery tower In the process, 47kg of chlorine gas and steam are used to steam bromine when the temperature of the tower top reaches 60-110°C. The steamed bromine is collected in a bromine altar after being condensed, and 97kg of bromine is recovered, with a content of 98.5%.

Embodiment 3

[0026] Embodiment 3: the 4M 3 Condensation mother liquor water is pumped into the enamel kettle of 6300L, starts to stir, slowly adds 25% sulfuric acid 240kg and sodium sulfate 200kg, following process steps are the same as embodiment 1. The lower layer solution was pumped into a 5000L enamel kettle, started stirring, and 100kg of butyl acetate was added, and the following process steps were the same as in Example 2. Recover bromine to be 96kg, content is 98.5%.

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PUM

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Abstract

The invention discloses a recovery method and comprehensive utilization of disperse red 60 by-products, belonging to the comprehensive treatment technical field of the chemical dyes and auxiliaries by-products, which comprises the following process steps: (1) acidification: the condensation mother liquid water obtained by condensation reaction of the 1-amino-2- bromine-4- hydroxyl anthraquinone and the phenol is acidi-regulated to the acid pH value, and sulfate or hydrochloride is added for acidulating; (2) standing stratification: the acidulated mother liquid water is kept still for more than a half hour, upper solution of disperse red sixty with phenol and dissolved in the phenol, and lower solution with potassium bromide and phenol are obtained; (3) separation: the lower solution is put in the potassium bromide catch trough, and then is derived into the potassium bromide extraction boiler; (4) extraction: organic solvent is put into the potassium bromide extraction boiler, after extracting, standing and stratification, the upper layer is phenol which can dissolve in the organic solvent, the lower layer is potassium bromide solution. The recovery method and comprehensive utilization of disperse red 60 by-products has the advantages of reducing production cost and environmental pollution effectively.

Description

technical field [0001] The invention relates to a recovery and comprehensive utilization method of by-products of disperse red 60, which belongs to the technical field of comprehensive treatment of by-products of chemical dyes and chemicals. Background technique [0002] In the current production process of Disperse Red 60, the condensed mother liquor obtained by condensation reaction of 1-amino-4-hydroxyanthraquinone and phenol, which is filtered, contains a large amount of phenol, Disperse Red 60 and potassium bromide. Existing treatment of mother liquor water is to reclaim phenol through vacuum distillation, still contain phenol, disperse red 60, potassium bromide etc. in the distillation residue, product yield is low, phenol consumption is big, vacuum distillation process is complicated, energy consumption is big, The single-step condensation yield is only about 85-88%, the production cost is relatively high, a large amount of hazardous solid waste is generated, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/50C07C39/04C07C19/075C01D3/10
Inventor 金永辉阮国涛赵锋莫琰杜伟丰
Owner 浙江长征化工有限公司
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