CN100497354C - Technique for extracting and recovering wastewater of acephate pesticide - Google Patents
Technique for extracting and recovering wastewater of acephate pesticide Download PDFInfo
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- CN100497354C CN100497354C CNB2007100522105A CN200710052210A CN100497354C CN 100497354 C CN100497354 C CN 100497354C CN B2007100522105 A CNB2007100522105 A CN B2007100522105A CN 200710052210 A CN200710052210 A CN 200710052210A CN 100497354 C CN100497354 C CN 100497354C
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- waste water
- acetate
- acephate
- solvent
- ammonium salt
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Abstract
This invention discloses a process for treating acephate-containing pesticide wastewater, and recovering acephate, inorganic ammonium salt, acetic acid and acetate. The process comprises: extracting wastewater with a solvent, sending the organic phase containing acephate to a solvent-removal apparatus, removing the solvent, separating, crystallizing to obtain acephate, sending extracted wastewater to a displacer, adding a strong acid to displace ammonium acetate into acetic acid and inorganic ammonium salt, or sending extracted wastewater to a neutralization apparatus, adding caustic alkali, and neutralizing to obtain acetate. The method is economic and environmentally friendly, and has such advantages as easy control and stable operation.
Description
Technical field
The invention belongs to a kind of wastewater treatment and reclaim novel process, particularly a kind of acephate agricultural chemicals waste water processing and recovery acephate and inorganic ammonium salt, acetate, acetate technology.
Background technology
The acephate agricultural chemicals waste water is the waste water that produces in a kind of higher effective and lower toxic pesticide acephate production process.This waste water is colourless or light yellow liquid, toughness slightly, the agricultural chemicals stink that tool is dense.Principal pollutant content in this waste water is respectively: acephate 2-4%, ammonium acetate 20-30%, ammonium sulfate 4-8%, other organism 2-4%, the comprehensive COD value of waste water is more than 500,000, and this waste water is very big to the contaminative of water body, just fish and microorganism is had great lethality under extremely low concentration.The generation of estimating this waste water in domestic every year is at 1.5-3 ten thousand tons, and along with the forbidding of methamidophos pesticide, the raising of acephate output, the amount of this waste water also can increase gradually.
The processing of this waste water is exactly the difficult problem of each acephate pesticide producing producer and environmental administration all the time, though have some units to adopt chemical process or biological method to handle, all finally abandoned processing because processing cost is high and treatment effect is not good.Also there is unit to adopt the simple fractionation by distillation organism and the method for ammonium acetate, but also because still have a large amount of dischargings of acetate and ammonia nitrogen and the thick ammonium acetate that obtains can't be re-refined and uses and fail to be applied to reality and come to an end.Therefore, present nearly all manufacturer all is unordered discharging or adopts a large amount of tap water dilution discharges.
Summary of the invention
The object of the present invention is to provide a kind of novel process of the waste water that produces in the acephate pesticide producing process being handled and reclaimed the former medicine of acephate and inorganic ammonium salt, acetate, acetate.
The object of the present invention is achieved like this: solvent and waste water are put into turntable extracting tower, with solvent waste water is extracted, extract the organic phase that contains acephate and send into precipitation device, get the former medicine of acephate through the precipitation fractional crystallization, turning back to extraction process after the solvent recuperation condensation recycles, to send into displacement apparatus through the waste water after the extraction, add sulfuric acid the ammonium acetate in the waste water is replaced as corresponding acetic acid and inorganic ammonium salt, further refining acetate, maybe will send into neutralising arrangement through the waste water after the extraction, add sodium hydroxide neutralize acetate.
The ratio of above-mentioned solvent and waste water is 1:1.
Waste water after the above-mentioned process extraction is sent into displacement apparatus, adding sulfuric acid replaces the ammonium acetate in the waste water, the displacement temperature is 30-60 ℃, by the 5000L reactor, throw about 1-1.5 hours of the time of acid, pH value is 3-5, is sent from center device and isolates inorganic ammonium salt and dilute acetic acid solution when displacement liquid is cooled to 10-20 ℃, again dilute acetic acid solution is carried out fractionation under 100-125 ℃ temperature and gets acetate and residual inorganic ammonium salt.
Waste water after above-mentioned process extracts is sent into neutralising arrangement, adds sodium hydroxide and carry out neutralization reaction under 60-80 ℃ temperature, and again that neutralization reaction is good acetate solution gets acetate after concentrated, cooling, separation.
The technology of a kind of acephate agricultural chemicals waste water processing provided by the invention and recovery acephate and inorganic ammonium salt, acetate, acetate, can solve the difficult problem that the acephate pesticide wastewater is handled, be a kind of economy, environmental protection, control easily can the novel process of moving steady in a long-term.Adopt technology of the present invention, can make this waste water obtain improvement in full force and effect, reach the safety dumping standard, can reclaim the tool value product again, waste water per ton can be made profits about 1500 yuan, reduces processing cost.Therefore, the present invention very easily applies.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
The processing step of processing of acephate agricultural chemicals waste water and recovery acephate and inorganic ammonium salt, acetate is:
1, with organic solvent lower halogenated hydrocarbon the acephate agricultural chemicals waste water is extracted, the ratio of solvent and waste water is 1:1, to extract the residual acephate agricultural chemicals in the waste water.This extraction equipment is a turntable extracting tower, after the organic phase that contains acephate of extraction is sent into precipitation still separation solvent, send into the crystallization kettle crystallization and get the former medicine of acephate, turning back to extraction process after the solvent recuperation condensation recycles, waste water after extraction contains acephate below 0.3%, is sent to acetic acid displacement operation again.
2, in waste water, slowly add quantitative sulfuric acid in proportion, travel out to form acetic acid with the acetate in the sulfuric acid displacement waste water, simultaneously the ammonium root is combined with inorganic acid and form inorganic ammonium salt, and separate, temperature during displacement is controlled at 30-60 ℃, by the 5000L reactor, throws 1-1.5 hours time of acid, pH value is 3-5, and chemical molecular formula is: 2CH
2COONH
4+ H
2SO
4==(NH
4)
2SO
4+ 2CH
4COOH.
3, after displacement is finished, when displacement liquid is cooled to 10-20 ℃, can the inorganic ammonium salt in the displacement liquid (cured article) be separated by whizzer, the mother liquor after the centrifugation is the dilute acetic acid solution (containing a spot of inorganic ammonium salt) of 20-95%.Dilute acetic acid is: the acetum of 20-95%; Acetic acid derivative is: various acetic esters, various acetate, aceticanhydride, acetylize material, halogenated acetic acids.
4. the dilute acetic acid solution with centrifugal gained carries out fractionation, further isolate acetic acid and residual inorganic ammonium salt, stop distillation when distillation temperature reaches 100-125 ℃, controlled temperature refluxes can get qualified acetic acid product, will get inorganic ammonium salt after the cooling of the material in the still.
Embodiment 2:
The processing step that acephate and acetate were handled and reclaimed to the acephate agricultural chemicals waste water is:
1, with organic solvent lower halogenated hydrocarbon methamidophos pesticide waste water is extracted, the ratio of solvent and waste water is 1:1, to extract the residual acephate agricultural chemicals in the waste water.This extraction equipment is a turntable extracting tower, and the organic phase that contains acephate of extraction is sent into the crystallization kettle crystallization and got the former medicine of acephate after sending into precipitation still separation solvent, turns back to extraction process after the solvent recuperation condensation and recycles.Waste water after extraction contains acephate below 0.3%, in being sent to and operation again.
2, will send into neutralising arrangement through the acephate waste water after the extraction, and add sodium hydroxide and carry out neutralization reaction under 60-80 ℃ temperature, chemical molecular formula is: CH
2COONH
4+ NaOH==CH
2COONa+H
2O+NH
3, the acetate solution of becoming reconciled in inciting somebody to action again gets the acetate product through concentrating the postcooling crystallization by centrifugation.Acetate solution turns back to dehydration back continuation cooling system acetate product in the dehydration still.
Claims (4)
1, technology is handled and reclaimed to the acephate agricultural chemicals waste water, it is characterized in that: solvent and waste water are put into turntable extracting tower, with solvent waste water is extracted, send extracting the organic phase that contains acephate into precipitation device, get the former medicine of acephate through the precipitation fractional crystallization, turning back to extraction process after the solvent recuperation condensation recycles, waste water after the extraction is sent into displacement apparatus, add sulfuric acid the ammonium acetate in the waste water is replaced as corresponding acetic acid and inorganic ammonium salt, further refining acetate, waste water after maybe will extracting is sent into neutralising arrangement, add sodium hydroxide neutralize acetate.
2, technology according to claim 1, the ratio that it is characterized in that described solvent and waste water is 1:1.
3, technology according to claim 1, it is characterized in that the waste water after the extraction is sent into displacement apparatus, adding sulfuric acid replaces the ammonium acetate in the waste water, the displacement temperature is 30-60 ℃, by the 5000L reactor, throw about 1-1.5 hours of the time of acid, pH value is 3-5, when displacement liquid is cooled to 10-20 ℃, be sent from center device and isolate inorganic ammonium salt and dilute acetic acid solution, again dilute acetic acid solution is carried out fractionation under 100-125 ℃ temperature and get acetate and residual inorganic ammonium salt.
4, technology according to claim 1, it is characterized in that and to send into neutralising arrangement through the waste water after the extraction, add sodium hydroxide and under 60-80 ℃ temperature, carry out neutralization reaction, again will in the acetate solution of becoming reconciled through concentrating, cooling, getting acetate after separating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100522105A CN100497354C (en) | 2007-05-21 | 2007-05-21 | Technique for extracting and recovering wastewater of acephate pesticide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100522105A CN100497354C (en) | 2007-05-21 | 2007-05-21 | Technique for extracting and recovering wastewater of acephate pesticide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101050224A CN101050224A (en) | 2007-10-10 |
| CN100497354C true CN100497354C (en) | 2009-06-10 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100522105A Expired - Fee Related CN100497354C (en) | 2007-05-21 | 2007-05-21 | Technique for extracting and recovering wastewater of acephate pesticide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100497354C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701490B (en) * | 2012-07-02 | 2013-11-06 | 江汉大学 | Treatment method of acephate production process wastewater |
| CN102989760A (en) * | 2012-11-21 | 2013-03-27 | 苏州科技学院 | Restoring method for soil polluted by acephate pesticide |
| CN108689541A (en) * | 2018-04-24 | 2018-10-23 | 江苏蓝丰生物化工股份有限公司 | The processing method of the waste water containing ammonium acetate |
| CN112850834B (en) * | 2021-01-14 | 2023-04-07 | 安道麦股份有限公司 | Treatment method of acephate extraction raffinate wastewater |
-
2007
- 2007-05-21 CN CNB2007100522105A patent/CN100497354C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 乙酰甲胺磷萃取工艺. 雄鹰等.农药，第44卷第8期. 2005 |
| 乙酰甲胺磷萃取工艺. 雄鹰等.农药，第44卷第8期. 2005 * |
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|---|---|
| CN101050224A (en) | 2007-10-10 |
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Owner name: SUZHOU DALING ENVIRONMENTAL PROTECTION TECHNOLOGY Free format text: FORMER OWNER: HAIFENG CHEMICAL IND CO., LTD., EZHOU Effective date: 20150821 |
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| C41 | Transfer of patent application or patent right or utility model | ||
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Effective date of registration: 20150821 Address after: Room 3, apartment 420, silk Plaza, Shengze Town, Wujiang Town, Suzhou District, Jiangsu, 215228 Patentee after: SUZHOU DA LING ENVIRONMENTAL TECHNOLOGY CO., LTD. Address before: 436034, Hubei, Ezhou province Ezhou Haifeng Chemical Industry Co., Ltd. Patentee before: Haifeng Chemical Ind Co., Ltd., Ezhou |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090610 Termination date: 20170521 |