CN102976541A - New technology for separating waste water containing zinc and nickel - Google Patents
New technology for separating waste water containing zinc and nickel Download PDFInfo
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- CN102976541A CN102976541A CN2012104529053A CN201210452905A CN102976541A CN 102976541 A CN102976541 A CN 102976541A CN 2012104529053 A CN2012104529053 A CN 2012104529053A CN 201210452905 A CN201210452905 A CN 201210452905A CN 102976541 A CN102976541 A CN 102976541A
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Abstract
The invention discloses a new technology for separating waste water containing zinc and nickel. The new technology is screened out mainly by comparing extraction, sediment, reduction and replacement. The new technology for separating waste water containing zinc and nickel is simple in operation, low in cost and environment-friendly. The new technology aims at handling the waste water generated in the synthesizing process of 2,2'-dipyridyl and is simple. According to the new technology, cost of the 2,2'-dipyridyl synthesis is greatly reduced and meanwhile the whole technological process is optimized.
Description
Technical field
The invention belongs to chemical industry and pesticide field, be specifically related to a kind ofly 2, what produce in the 2'-dipyridyl building-up process contains the novel process that zinc, nickel waste water separate.
Background technology
2,2'-dipyridyl is one of dipyridyl isomer, is a kind of important organic synthesis intermediate, is mainly used in medicine intermediate, organic synthesis etc.Simultaneously, it also is a kind of widely used sequestrant, paint additive, is widely used in the aspects such as DYE PRODUCTION, pesticide producing and spices.Therefore, it is synthesized and the research of industrialization aspect will have great importance.
The traditional method Raney's nickel of synthetic 2,2'-dipyridyl is that catalyzer is synthetic take pyridine as raw material.The catalyst life of this method is shorter, should not recycle, and also can't satisfy the requirement in the production.
Take the dihalo-pyridine as raw material, synthesizing 2,2'-dipyridyl with composite catalyst becomes the main method of producing at present 2,2'-dipyridyl both at home and abroad.Therefore, will certainly restrict whole technical process for the control of cost, particularly the aftertreatment of the waste water that contains catalyzer that produces in its production process seemed particularly important.
Summary of the invention
The present invention from reduce production costs, optimization technological process, energy-conserving and environment-protective equal angles, a kind of novel process that zinc, nickel waste water separate that contains has been proposed.
To achieve these goals, the present invention adopts following technical scheme:
A kind of novel process that contains zinc, nickel waste water separation, its processing step is as follows:
(1) alkaline hydrolysis: synthetic 2, after the coupling of 2'-dipyridyl finishes, be warming up to 40-60 ℃ of alkaline hydrolysis 4-5h to adding 900-1000kg 20% ammoniacal liquor and 150-250kg ammonium sulfate in precipitation gained 240-270kg solid, after the toluene extraction, obtain containing the waste water of catalyzer zinc, nickel;
(2) deamination: the waste water that step (1) is produced heats deamination to pH=7-8;
(3) displacement: waste water behind step (2) deamination is warming up to 60-80 ℃, adds 3-8kg zinc powder and 3-8kg antimonous oxide, insulation 1-3h;
(4) heavy zinc once: after step (3) insulation finishes, suction filtration while hot, filtrate adds 50-100kg bicarbonate of ammonia, stirs suction filtration behind the 4-8h under the room temperature, washing namely gets zinc subcarbonate;
(5) the heavy zinc of secondary: step (4) suction filtration rear filtrate adds sulfuric acid and transfers pH=1-4, namely gets zinc sulfate ammonia, applies mechanically to the once heavy zinc of next batch;
(6) concentrate: the waste water that the final waste water that step (5) produces and washing produce all goes to concentrated post, and the gained solid ammonium sulfate is as the raw material of producing chemical fertilizer after concentrating, and water also can be applied mechanically.
Beneficial effect of the present invention:
The inventive method is simple to operate, cost is lower, environmental friendliness, not only greatly reduces the synthetic cost of 2,2'-dipyridyl, has also optimized whole technical process simultaneously.
Embodiment
Embodiment 1
The novel process that contains zinc, nickel waste water separation may further comprise the steps:
(1) alkaline hydrolysis: after synthetic 2,2'-dipyridyl coupling finishes, be warming up to 40 ℃ of alkaline hydrolysis 4h to adding 900kg 20% ammoniacal liquor and 150kg ammonium sulfate in precipitation gained 240kg solid, after the toluene extraction, obtain containing the waste water of catalyzer zinc, nickel;
(2) deamination: the waste water that step (1) is produced heats deamination to pH=7;
(3) displacement: waste water behind step (2) deamination is warming up to 60 ℃, adds 3kg zinc powder and 3kg antimonous oxide, insulation 1h;
(4) heavy zinc once: after step (3) insulation finishes, suction filtration while hot, filtrate adds 50kg bicarbonate of ammonia, stirs suction filtration behind the 4h under the room temperature, washing namely gets zinc subcarbonate;
(5) the heavy zinc of secondary: step (4) suction filtration rear filtrate adds sulfuric acid and transfers pH=1, namely gets zinc sulfate ammonia, applies mechanically to the once heavy zinc of next batch;
(6) concentrate: the waste water that the final waste water that step (5) produces and washing produce all goes to concentrated post, and the gained solid ammonium sulfate is as the raw material of producing chemical fertilizer after concentrating, and water also can be applied mechanically.
Embodiment 2
The novel process that contains zinc, nickel waste water separation may further comprise the steps:
(1) alkaline hydrolysis: after synthetic 2,2'-dipyridyl coupling finishes, be warming up to 40 ℃ of alkaline hydrolysis 4h to adding 925kg 20% ammoniacal liquor and 175kg ammonium sulfate in precipitation gained 250kg solid, after the toluene extraction, obtain containing the waste water of catalyzer zinc, nickel;
(2) deamination: the waste water that step (1) is produced heats deamination to pH=7;
(3) displacement: waste water behind step (2) deamination is warming up to 60 ℃, adds 4kg zinc powder and 4kg antimonous oxide, insulation 2h;
(4) heavy zinc once: after step (3) insulation finishes, suction filtration while hot, filtrate adds 70kg bicarbonate of ammonia, stirs suction filtration behind the 4h under the room temperature, washing namely gets zinc subcarbonate;
(5) the heavy zinc of secondary: step (4) suction filtration rear filtrate adds sulfuric acid and transfers pH=2, namely gets zinc sulfate ammonia, applies mechanically to the once heavy zinc of next batch;
(6) concentrate: the waste water that the final waste water that step (5) produces and washing produce all goes to concentrated post, and the gained solid ammonium sulfate is as the raw material of producing chemical fertilizer after concentrating, and water also can be applied mechanically.
Embodiment 3
The novel process that contains zinc, nickel waste water separation may further comprise the steps:
(1) alkaline hydrolysis: after synthetic 2,2'-dipyridyl coupling finishes, be warming up to 60 ℃ of alkaline hydrolysis 4h to adding 950kg 20% ammoniacal liquor and 200kg ammonium sulfate in precipitation gained 260kg solid, after the toluene extraction, obtain containing the waste water of catalyzer zinc, nickel;
(2) deamination: the waste water that step (1) is produced heats deamination to pH=7.5;
(3) displacement: waste water behind step (2) deamination is warming up to 80 ℃, adds 5kg zinc powder and 5kg antimonous oxide, insulation 3h;
(4) heavy zinc once: after step (3) insulation finishes, suction filtration while hot, filtrate adds 80kg bicarbonate of ammonia, stirs suction filtration behind the 4h under the room temperature, washing namely gets zinc subcarbonate;
(5) the heavy zinc of secondary: step (4) suction filtration rear filtrate adds sulfuric acid and transfers pH=3, namely gets zinc sulfate ammonia, applies mechanically to the once heavy zinc of next batch;
(6) concentrate: the waste water that the final waste water that step (5) produces and washing produce all goes to concentrated post, and the gained solid ammonium sulfate is as the raw material of producing chemical fertilizer after concentrating, and water also can be applied mechanically.
Embodiment 4
The novel process that contains zinc, nickel waste water separation may further comprise the steps:
(1) alkaline hydrolysis: after synthetic 2,2'-dipyridyl coupling finishes, be warming up to 60 ℃ of alkaline hydrolysis 5h to adding 1000kg 20% ammoniacal liquor and 250kg ammonium sulfate in precipitation gained 270kg solid, after the toluene extraction, obtain containing the waste water of catalyzer zinc, nickel;
(2) deamination: the waste water that step (1) is produced heats deamination to pH=8;
(3) displacement: waste water behind step (2) deamination is warming up to 80 ℃, adds 8kg zinc powder and 8kg antimonous oxide, insulation 3h;
(4) heavy zinc once: after step (3) insulation finishes, suction filtration while hot, filtrate adds 100kg bicarbonate of ammonia, stirs suction filtration behind the 4h under the room temperature, washing namely gets zinc subcarbonate;
(5) the heavy zinc of secondary: step (4) suction filtration rear filtrate adds sulfuric acid and transfers pH=4, namely gets zinc sulfate ammonia, applies mechanically to the once heavy zinc of next batch;
(6) concentrate: the waste water that the final waste water that step (5) produces and washing produce all goes to concentrated post, and the gained solid ammonium sulfate is as the raw material of producing chemical fertilizer after concentrating, and water also can be applied mechanically.
Claims (1)
1. one kind contains the novel process that zinc, nickel waste water separate, and it is characterized in that its processing step is as follows:
(1) alkaline hydrolysis: synthetic 2, after the coupling of 2'-dipyridyl finishes, be warming up to 40-60 ℃ of alkaline hydrolysis 4-5h to adding 900-1000kg 20% ammoniacal liquor and 150-250kg ammonium sulfate in precipitation gained 240-270kg solid, after the toluene extraction, obtain containing the waste water of catalyzer zinc, nickel;
(2) deamination: the waste water that step (1) is produced heats deamination to pH=7-8;
(3) displacement: waste water behind step (2) deamination is warming up to 60-80 ℃, adds 3-8kg zinc powder and 3-8kg antimonous oxide, insulation 1-3h;
(4) heavy zinc once: after step (3) insulation finishes, suction filtration while hot, filtrate adds 50-100kg bicarbonate of ammonia, stirs suction filtration behind the 4-8h under the room temperature, washing namely gets zinc subcarbonate;
(5) the heavy zinc of secondary: step (4) suction filtration rear filtrate adds sulfuric acid and transfers pH=1-4, namely gets zinc sulfate ammonia, applies mechanically to the once heavy zinc of next batch;
(6) concentrate: the waste water that the final waste water that step (5) produces and washing produce all goes to concentrated post, and the gained solid ammonium sulfate is as the raw material of producing chemical fertilizer after concentrating, and water also can be applied mechanically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210452905.3A CN102976541B (en) | 2012-11-13 | 2012-11-13 | New technology for separating waste water containing zinc and nickel |
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| CN201210452905.3A CN102976541B (en) | 2012-11-13 | 2012-11-13 | New technology for separating waste water containing zinc and nickel |
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| CN102976541A true CN102976541A (en) | 2013-03-20 |
| CN102976541B CN102976541B (en) | 2014-06-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880061A (en) * | 2014-02-28 | 2014-06-25 | 安徽国星生物化学有限公司 | Method for separating and purifying zinc ions and nickel ions in ammonification catalytic waste liquor |
| CN108640390A (en) * | 2018-05-31 | 2018-10-12 | 阳谷祥光铜业有限公司 | A kind of processing method of stibium-containing wastewater |
| CN109608252A (en) * | 2018-12-11 | 2019-04-12 | 中山市承铭农业技术开发有限公司 | A kind of production method of akaline liquid fertilizer |
| CN110407279A (en) * | 2019-07-09 | 2019-11-05 | 安徽红太阳新材料有限公司 | A kind of diquat dibromide wastewater treatment method |
Citations (4)
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| JPH0490770A (en) * | 1990-08-02 | 1992-03-24 | Okayama Pref Gov | Automatic continuous room or low temperature decomposition of multihalogenated organic compound |
| CN1869199A (en) * | 2006-05-23 | 2006-11-29 | 北京未名凯拓农业生物技术有限公司 | A strain denitrogen paracoccus and its culturing method and application |
| CN101074211A (en) * | 2007-06-18 | 2007-11-21 | 浙江工业大学 | Process for treating high-purity pyridine solution |
| CN101074424A (en) * | 2006-05-19 | 2007-11-21 | 中国石油化工股份有限公司 | Xylose staphylocci for degrading 2-picoline and its use |
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2012
- 2012-11-13 CN CN201210452905.3A patent/CN102976541B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0490770A (en) * | 1990-08-02 | 1992-03-24 | Okayama Pref Gov | Automatic continuous room or low temperature decomposition of multihalogenated organic compound |
| CN101074424A (en) * | 2006-05-19 | 2007-11-21 | 中国石油化工股份有限公司 | Xylose staphylocci for degrading 2-picoline and its use |
| CN1869199A (en) * | 2006-05-23 | 2006-11-29 | 北京未名凯拓农业生物技术有限公司 | A strain denitrogen paracoccus and its culturing method and application |
| CN101074211A (en) * | 2007-06-18 | 2007-11-21 | 浙江工业大学 | Process for treating high-purity pyridine solution |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880061A (en) * | 2014-02-28 | 2014-06-25 | 安徽国星生物化学有限公司 | Method for separating and purifying zinc ions and nickel ions in ammonification catalytic waste liquor |
| CN108640390A (en) * | 2018-05-31 | 2018-10-12 | 阳谷祥光铜业有限公司 | A kind of processing method of stibium-containing wastewater |
| CN109608252A (en) * | 2018-12-11 | 2019-04-12 | 中山市承铭农业技术开发有限公司 | A kind of production method of akaline liquid fertilizer |
| CN110407279A (en) * | 2019-07-09 | 2019-11-05 | 安徽红太阳新材料有限公司 | A kind of diquat dibromide wastewater treatment method |
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| CN102976541B (en) | 2014-06-11 |
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