3,3'-dichlorobenzidine hydrochloride waste water reclaiming method and apparatus thereof

A technology of dichlorobenzidine hydrochloride and treatment method, which is applied in water/sewage treatment, chemical instruments and methods, water/sewage multi-stage treatment, etc. High economic value, low treatment cost, and the effect of eliminating environmental pollution

Inactive Publication Date: 2009-02-25
SHANDONG AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two methods can effectively degrade toxic substances in dye macromolecules, but neither of them has utilized resources, and ...

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  • 3,3'-dichlorobenzidine hydrochloride waste water reclaiming method and apparatus thereof

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Embodiment 1

[0051] 500mL of 3,3'-dichlorobenzidine hydrochloride production mother liquor wastewater containing 8% (mass fraction) of hydrochloric acid, 24% (mass fraction) of sulfuric acid and about 1.5% (mass fraction) of organic matter was added in a three-necked flask of 1000mL , evacuate to 0.09MPa, heat the electric heating mantle to boiling, and condense the evaporated HCl and water with a condenser tube. When the sulfuric acid was concentrated to about 50% (mass fraction), the temperature was about 69°C, and the heating was stopped. At this time, the condensate contained about 14% (mass fraction) of hydrochloric acid average concentration. If the condensate is received in sections, hydrochloric acid with a concentration of 17% (mass fraction) can be obtained. Add 9 g of activated carbon into the three-necked flask, and decolorize it by slight boiling for 1 h. Filtrate while hot to remove activated carbon to obtain almost colorless sulfuric acid concentrate. The filtrate was plac...

Embodiment 2

[0053] Use a pump to add 3,3'-dichlorobenzidine hydrochloride production mother liquor wastewater containing 8% (mass fraction) of hydrochloric acid, 24% (mass fraction) of sulfuric acid and about 1.5% (mass fraction) of organic matter to the external heating natural circulation In the evaporator, vacuumize to 0.09MPa, heat to boiling with saturated water vapor, and continuously add waste water to keep the liquid level in the evaporator constant. The steamed HCl and water enter the bottom of the rectification tower with packing, adjust the reflux ratio to 1.2, and obtain hydrochloric acid with an average content of about 20% (mass fraction) at the bottom of the tower, and the water vapor at the top of the tower enters the condensation tube to condense, and the condensate hydrochloric acid The average content is about 4% (mass fraction). When the sulfuric acid concentration reaches about 50% (mass fraction), stop heating, pump the concentrated waste water into the decolorization...

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Abstract

The invention discloses a method for resourceful treatment of 3,3'-dichlorobenzidine hydrochloride wastewater, in which a chemical technology is adopted for the resourceful treatment of 3, 3'-dichlorobenzidine hydrochloride wastewater, in order that hydrochloric acid and sulphuric acid in the wastewater can be recycled, a by-product of o-chloroaniline sulfate is obtained, and the environment pollution caused by waste discharge is prevented. The method for resourceful treatment comprises that (1) first, the wastewater is evaporated, so that the chlorine hydride in the wastewater is separated and the wastewater is concentrated; (2) the chlorine hydride and water evaporated is rectified and separated, so that the chlorine hydride can be concentrated and reused, the vapor containing little chlorine hydride is recycled by condensing; (3) the wastewater concentrated by evaporating is decolored, and the colored substances contained are removed; (4) the wastewater is cooled for crystallization after being decolored, so that the o-chloroaniline sulfate is separated, and the purified sulphuric acid is obtained and reused. The invention discloses the structure of a device for resourceful treatment technique at the same time.

Description

1. Technical field [0001] The invention relates to a waste water containing hydrochloric acid, sulfuric acid and refractory and toxic aniline organic matter, especially a resource treatment method and device for the mother liquor waste water of 3,3'-dichlorobenzidine hydrochloride production, which belongs to chemical treatment, chemical technology field. 2. Background technology [0002] 3,3'-dichlorobenzidine (DCB) hydrochloride (C 12 h 10 Cl 2 N 2 2HCl) is an important pigment and dye intermediate. The benzidine yellow, Uerkang fast red, and azo dyes produced from this intermediate have good acid resistance, bright and firm color, and are made from it as the main body. A series of organic pigments account for about 27% of the total organic pigments. The production of 3,3′-dichlorobenzidine hydrochloride generally uses o-nitrochlorobenzene as a raw material, and is produced through reduction, transposition, salt formation, crystallization, filtration, and drying. At ...

Claims

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Application Information

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IPC IPC(8): C02F9/10C02F1/04C02F1/58C01B17/90
Inventor 贾寿华周杰裘立群
Owner SHANDONG AGRICULTURAL UNIVERSITY
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