CN1752032A - Treatment and recovery technology for mixed acid from industrial waste water 3,3-dichlorobenzidine hydrochloride - Google Patents
Treatment and recovery technology for mixed acid from industrial waste water 3,3-dichlorobenzidine hydrochloride Download PDFInfo
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- CN1752032A CN1752032A CN 200510090608 CN200510090608A CN1752032A CN 1752032 A CN1752032 A CN 1752032A CN 200510090608 CN200510090608 CN 200510090608 CN 200510090608 A CN200510090608 A CN 200510090608A CN 1752032 A CN1752032 A CN 1752032A
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- dichlorobenzidine hydrochloride
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Abstract
A process for reclaiming the acid mixture generated by industrial sewage and 3.3-dichlorobiphenylamin hydrochloride features the ore containing Mg is used to react on the sulfuric acid in said acid mixture to obtain magnesium sulfate while decrease the acidity of sewage.
Description
Technical field
The present invention relates to a kind of treatment process of trade effluent, especially a kind of to dyeing waste water 3, the 3-dichlorobenzidine hydrochloride produces the technology that associated products was handled and therefrom extracted to nitration mixture
Background technology
Wastewater treatment promptly is to utilize various technical measures that the pollutent of various forms is separated from waste water, or it is decomposed, is converted into harmless and stable material, thus the process that waste water is purified.For processing method of industrial waste water, can be divided into physical treatment process, method of chemical treatment and biological treatment three major types at present.3, the 3-dichlorobenzidine hydrochloride produces nitration mixture and belongs to dyeing waste water, and its water quality is special, and pollution intensity is big, is one of reluctant trade effluent, and its discharging and processing are that the current whole world is paid close attention to and problem demanding prompt solution.
Summary of the invention
The objective of the invention is to can't good treatment 3 at what exist in the prior art, and the 3-dichlorobenzidine hydrochloride produces the deficiency of nitration mixture, and a kind of treatment process that utilizes magnesium ore that waste water is handled and turned waste into wealth is provided.
The object of the present invention is achieved like this: a kind of trade effluent 3, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, employing contains the ore and 3 of magnesium elements, the sulfuric acid that the 3-dichlorobenzidine hydrochloride produces in the nitration mixture reacts, extract sal epsom simultaneously at reduction waste water tart, may further comprise the steps:
(1) magnesium ore and 3.3-dichlorobenzidine hydrochloride generation nitration mixture are stirred in neutralization tank by reaction ratio, fully the reaction back generates the neutralisation of sulphuric acid magnesium solution;
(2) add the capacity gac at the neutralizer that generates, adsorb the organic impurity in the neutralizer, the gac after absorption is finished is obtained the higher Adlerika of purity by the filter elimination;
(3) will filter the high temperature Adlerika that the back obtains and squeeze into crystallizer, the solution spontaneous nucleation of lowering the temperature in crystallizer carries out centrifugation wet feed crystal then in whizzer or suction filtration machine;
(4) the wet feed crystal is sent into drying machine, produce required magnesium sulfate crystals after the drying.
In the process of preferably underway and reaction, continue to add magnesium ore and add at interval and making reaction solution keep weakly acidic sulfuric acid.
The continuous potential of hydrogen of detection reaction liquid in N-process preferably, pH value is controlled at 4-6, and takes this as a foundation and regulate vitriolic and add speed.
Preferably control temperature of reaction in the neutralization reaction at 80 ℃-85 ℃.
The preferably used ore that contains magnesium elements is magnesia or magnesia calcining powder.
Preferably add silver hydroxide in the Adlerika after filtration.
Preferably the waste liquid after the centrifugation is sent into circulating reaction in the reaction solution again.
The invention has the beneficial effects as follows: utilize the comparatively cheap magnesium ore of price to handle trade effluent, simple to operate, cost is low, has both prevented pollution, can make full use of the spent acid in the waste liquid again, turns waste into wealth.
Embodiment
A kind of trade effluent 3, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, adopts the ore and 3 that contains magnesium elements, and the sulfuric acid that the 3-dichlorobenzidine hydrochloride produces in the nitration mixture reacts, extract sal epsom simultaneously at reduction waste water tart, may further comprise the steps:
(1) magnesium ore and 3.3-dichlorobenzidine hydrochloride generation nitration mixture are stirred in neutralization tank by reaction ratio, fully the reaction back generates the neutralisation of sulphuric acid magnesium solution;
(2) add the capacity gac at the neutralizer that generates, adsorb the organic impurity in the neutralizer, the gac after absorption is finished is obtained the higher Adlerika of purity by the filter elimination;
(3) will filter the high temperature Adlerika that the back obtains and squeeze into crystallizer, the solution spontaneous nucleation of lowering the temperature in crystallizer carries out centrifugation wet feed crystal then in whizzer or suction filtration machine;
(4) the wet feed crystal is sent into drying machine, produce required magnesium sulfate crystals after the drying.
First specific embodiment of the present invention, the 3.3-dichlorobenzidine hydrochloride produces that institute's sulfur acid is 30% in the nitration mixture in the reactant, and hydrochloric is 5%; Content of magnesia is 85% in the magnesia, and other contains small amounts iron.Magnesia and pending 3.3-dichlorobenzidine hydrochloride are produced nitration mixture add in the neutralization tank by 1: 7.5 ratio, add the water stirring it is fully reacted, resultant of reaction is that main solute is the solution of sal epsom.In neutralization tank, continue to add magnesia or its calcining powder in the neutralization reaction process, and add sulfuric acid successively as auxiliary agent, potential of hydrogen with the maintenance reaction solution is a slightly acidic, and can make itself and calcining powder continue neutralization reaction takes place, and constantly detect solution acid alkalinity in the reaction process, remaining on pH value is 5, and as standard, control sulfuric acid add-on, the temperature to neutralizer in the reaction process is controlled, and the temperature of neutralizer is controlled at 80 degrees centigrade.Above-mentioned steps is finished, composition is mainly sal epsom in the neutralizer that produces, because producing in the nitration mixture, the 3.3-dichlorobenzidine hydrochloride contains small amount of hydrochloric acid and organic impurity, and also contain the small amounts of iron ore in the magnesia ore, so in its resultant of reaction except sal epsom, also comprise ferric sulfate, iron(ic) chloride, magnesium chloride and other impurity, in order to remove the impurity that is comprised in this neutralizer, in reacted neutralization tank, add the capacity gac, stirred 80 minutes, and made iron ion compound and other organic solid impurity in the abundant absorption reaction liquid of gac.Fully after the absorption, solution is filtered by pressure filter, remove the gac after adsorbing fully.Through leaf-type filter the impurity solid is filtered, the purity of the liquid solute sal epsom after the filtration can reach more than 97%.High temperature sal epsom clear liquid after filtering is squeezed into crystallizer, be cooled to below 30 degree, the clear liquid spontaneous nucleation of in crystallizer, lowering the temperature.Solid-liquid mixture after the crystallization is carried out centrifugation, and use whizzer that it is washed into the wet feed crystal.Wet feed is sent into scale be controlled at vibrated fluidized bed about 200 square metres, temperature is controlled at 50 degrees centigrade and carries out drying, finally makes the magnesium sulfate heptahydrate crystal.
Second specific embodiment of the present invention is produced the 3.3-dichlorobenzidine hydrochloride and is produced that institute's sulfur acid is 33% in the nitration mixture in the reactant, hydrochloric is 7%; Content of magnesia is 90% in the magnesia, and other contains small amounts iron.Magnesia and pending 3.3-dichlorobenzidine hydrochloride are produced nitration mixture add in the neutralization tank by 1: 7.8 ratio, add the water stirring it is fully reacted, resultant of reaction is that main solute is the solution of sal epsom.In neutralization tank, continue to add magnesia or its calcining powder in the neutralization reaction process, and add sulfuric acid successively as auxiliary agent, potential of hydrogen with the maintenance reaction solution is a slightly acidic, and can make itself and calcining powder continue neutralization reaction takes place, and constantly detect solution acid alkalinity in the reaction process, remaining on pH value is 5, and as standard, control sulfuric acid add-on, the temperature to neutralizer in the reaction process is controlled, and the temperature of neutralizer is controlled at 85 degrees centigrade.Above-mentioned steps is finished, and adds the capacity gac in neutralization tank, stirs 90 minutes, makes iron ion compound and other organic solid impurity in the abundant absorption reaction liquid of gac.Fully after the absorption, solution is filtered by pressure filter, remove the gac after adsorbing fully.Through leaf-type filter the impurity solid is filtered, the purity of the liquid solute sal epsom after the filtration can reach more than 97%.High temperature sal epsom clear liquid after filtering is squeezed into crystallizer, be cooled to below 30 degree, the clear liquid spontaneous nucleation of in crystallizer, lowering the temperature.Solid-liquid mixture after the crystallization is carried out centrifugation, and use whizzer that it is washed into the wet feed crystal.Wet feed is sent into scale be controlled at vibrated fluidized bed about 200 square metres, temperature is controlled at 50 degrees centigrade and carries out drying, finally makes the magnesium sulfate heptahydrate crystal.
In order to expand the product scope of this invented technology, can in drying process, control effectively in addition,, satisfy different product needed to make the magnesium sulfate crystals of different crystal water to parameters such as temperature, times.
Claims (7)
1. trade effluent 3, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, adopts the ore and 3 that contains magnesium elements, and the sulfuric acid that the 3-dichlorobenzidine hydrochloride produces in the nitration mixture reacts, extract sal epsom simultaneously at reduction waste water tart, it is characterized in that: may further comprise the steps
(1) magnesium ore and 3.3-dichlorobenzidine hydrochloride are produced nitration mixture by reaction ratio 1～1.5: 7.5～8 stir in neutralization tank, fully reaction back generation neutralisation of sulphuric acid magnesium solution;
(2) add the capacity gac at the neutralizer that generates, adsorb the organic impurity in the neutralizer, the gac after absorption is finished is obtained the higher Adlerika of purity by the filter elimination;
(3) will filter the high temperature Adlerika that the back obtains and squeeze into crystallizer, the solution spontaneous nucleation of lowering the temperature in crystallizer carries out centrifugation wet feed crystal then in whizzer or suction filtration machine;
(4) the wet feed crystal is sent into drying machine, produce required magnesium sulfate crystals after the drying.
2. trade effluent 3 as claimed in claim 1,3-dichlorobenzidine hydrochloride produce treatment and recovery technology for mixed acid, it is characterized in that: in the process of underway and reaction, continue to add magnesium ore and add at interval making reaction solution keep weakly acidic sulfuric acid.
3. trade effluent 3 as claimed in claim 2, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, it is characterized in that: the potential of hydrogen of continuous detection reaction liquid in N-process, pH value is controlled at 4-6.
4. as claim 2 or 3 described trade effluents 3, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, it is characterized in that: the temperature of reaction in the control neutralization reaction is at 80 ℃-85 ℃.
5. as claim 1 or 2 or 3 described trade effluents 3, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, it is characterized in that: the used ore that contains magnesium elements is magnesia or magnesia calcining powder.
6. trade effluent 3 as claimed in claim 1, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, it is characterized in that: add silver hydroxide in the Adlerika after filtration.
7. trade effluent 3 as claimed in claim 1, the 3-dichlorobenzidine hydrochloride produces treatment and recovery technology for mixed acid, and it is characterized in that: the waste liquid after the centrifugation is sent into circulating reaction in the reaction solution again.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510090608 CN1752032B (en) | 2005-08-17 | 2005-08-17 | Treatment and recovery technology for mixed acid from industrial waste water 3,3-dichlorobenzidine hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510090608 CN1752032B (en) | 2005-08-17 | 2005-08-17 | Treatment and recovery technology for mixed acid from industrial waste water 3,3-dichlorobenzidine hydrochloride |
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| CN1752032A true CN1752032A (en) | 2006-03-29 |
| CN1752032B CN1752032B (en) | 2010-07-28 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880685A (en) * | 2012-12-20 | 2014-06-25 | 江苏道博化工有限公司 | Comprehensive recovery utilization method for 3,3-dichlorobenzidine |
| CN104843926A (en) * | 2015-05-21 | 2015-08-19 | 成都虹华环保科技股份有限公司 | Nitric acid stripping water treatment system |
| CN107827130A (en) * | 2017-12-13 | 2018-03-23 | 青岛锐丰源化工有限公司 | Utilize the production line for being alkylated spent acid and preparing magnesium sulfate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3937320A1 (en) * | 1989-11-09 | 1991-05-16 | Hoechst Ag | METHOD FOR THE CONTINUOUS PRODUCTION OF 3,3'-DICHLOR-BENZIDINE DIHYDROCHLORIDE |
| CN1280255C (en) * | 2004-08-31 | 2006-10-18 | 大连理工大学 | Process for comprehensive utilization of waste sulfuric acid from 3,3'-dichloro benzidine hydrochloride |
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2005
- 2005-08-17 CN CN 200510090608 patent/CN1752032B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880685A (en) * | 2012-12-20 | 2014-06-25 | 江苏道博化工有限公司 | Comprehensive recovery utilization method for 3,3-dichlorobenzidine |
| CN103880685B (en) * | 2012-12-20 | 2015-08-19 | 江苏道博化工有限公司 | 3, the recovery method of comprehensive utilization of 3 '-dichlorobenzidine |
| CN104843926A (en) * | 2015-05-21 | 2015-08-19 | 成都虹华环保科技股份有限公司 | Nitric acid stripping water treatment system |
| CN107827130A (en) * | 2017-12-13 | 2018-03-23 | 青岛锐丰源化工有限公司 | Utilize the production line for being alkylated spent acid and preparing magnesium sulfate |
| CN107827130B (en) * | 2017-12-13 | 2024-04-02 | 青岛锐丰源化工有限公司 | Production line for preparing magnesium sulfate by using alkylated waste acid |
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| CN1752032B (en) | 2010-07-28 |
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