CN102765841A - Method for recovering 3,5,6-Trichloropyridin-2-ol sodium from 3,5,6-Trichloropyridin-2-ol sodium alkaline hydrolysis wastewater - Google Patents
Method for recovering 3,5,6-Trichloropyridin-2-ol sodium from 3,5,6-Trichloropyridin-2-ol sodium alkaline hydrolysis wastewater Download PDFInfo
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- CN102765841A CN102765841A CN2012101483433A CN201210148343A CN102765841A CN 102765841 A CN102765841 A CN 102765841A CN 2012101483433 A CN2012101483433 A CN 2012101483433A CN 201210148343 A CN201210148343 A CN 201210148343A CN 102765841 A CN102765841 A CN 102765841A
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- sodium alcoholate
- trichloro pyridyl
- pyridyl sodium
- alkaline hydrolysis
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Abstract
The present invention relates to a method for recovering 3,5,6-Trichloropyridin-2-ol sodium from 3,5,6-Trichloropyridin-2-ol sodium alkaline hydrolysis wastewater, and belongs to the technical fields of chemical separation and water treatment. The method comprises processing steps of filtration, evaporation, sodium chloride removal and drying. The method provided by the invention can realize a high recovery rate of 3,5,6-Trichloropyridin-2-ol sodium, increase production yield of 3,5,6-Trichloropyridin-2-ol sodium by more than 3% with less investment and effectively reduce production cost of 3,5,6-Trichloropyridin-2-ol sodium, and has a high rate of return on investment. Wastewater treated by the method provided by the invention has salt reduced by more than 60%, COD reduced by more than 85%, BOD55 / COD ratio increased to higher than 0.3 and substantially enhanced wastewater biodegradability, and can be treated with ordinary biochemical method to reach discharge standards. A by-product sodium chloride produced by the method can be refined and used as an industrial salt.
Description
Technical field
The present invention relates to a kind of method that from trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water, reclaims trichloro pyridyl sodium alcoholate, belong to chemical separating and water-treatment technology field.
Background technology
Trichloro pyridyl sodium alcoholate is a kind of important chemical material, is mainly used in the production of agricultural chemicals Chlorpyrifos 94, first class Chlorpyrifos 94, is a kind of pesticide intermediate, and over the past two years, its market price was 38000～45000 yuan/ton.The pure article of trichloro pyridyl sodium alcoholate are the off-white color solid, are slightly soluble in water, and saturated strength of solution is about 0.5% in frozen water, and saturated strength of solution is about 20% in boiling water.
In general, one ton of trichloro pyridyl sodium alcoholate of the every production of trichoroacetic chloride method approximately produces 3～5 tons of alkaline hydrolysis waste water that contain trichloropyridine.Trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water composition is quite complicated; Contain materials such as 4～10% trichloro pyridyl sodium alcoholate (the trichloro pyridyl sodium alcoholate crystal that contains suspension), 8～10% sodium-chlor and other a spot of prussiate, chlorobenzene; CODcr is dense; Between 40000～60000, the poor (BOD5 of biological degradability
5/ COD ratio is between 0.15～0.2), can not use common biochemical process to handle.For this trichloro pyridyl sodium alcoholate factory effluent that contains, the common way of manufacturer is to send into after diluting 20～40 times that biochemical system is handled or burn through concentrating to send in the incinerator behind the desalination, has done following bad part like this:
(1) there are a considerable amount of trichloro pyridyl sodium alcoholates not have and just lost, reduced the yield of trichloro pyridyl sodium alcoholate, increased the production cost of trichloro pyridyl sodium alcoholate virtually through reclaiming; (2) the COD value and the salinity of waste water are too high, have increased the intractability of waste water.
Summary of the invention
For solving the problem of above existence; Produce the characteristics of trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water to the trichoroacetic chloride method; The invention provides the method that reclaims trichloro pyridyl sodium alcoholate in a kind of trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water, its technical scheme of taking is: this technical scheme mainly comprises process steps such as filtration, evaporation, dechlorination sodium, drying.It is characterized in that these method concrete steps are following:
A. filter: after trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water removes thick dirt through grid filtration, after supercooler 1 cooling, get into again and continue to be cooled to 0～10 ℃ in the water cooler 2, filter then, obtain the trichloro pyridyl sodium alcoholate crystallisate;
B. evaporate: the filtrating that filters out among the step a gets into neutralization tank and cools off in the water cooler 1 through the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water in the grid entering water cooler 1 for the neutrality back gets into through its pH value of acid-base neutralisation device adjusting, gets into successively then in vaporizer 1, the vaporizer 2 and is concentrated 6～12 times;
C. remove sodium-chlor: to being filtered by the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water after concentrating, obtain the sodium-chlor crystallisate, filtrating is mixed back entering sink drainage and is carried out biochemical treatment with the phlegma that from multiple-effect evaporator, comes out;
D. dry: as to concentrate in together the trichloro pyridyl sodium alcoholate crystal that obtains among the step a and reach dry in drying machine after the some amount, obtain content greater than 85% trichloro pyridyl sodium alcoholate powder.
The present invention has following characteristics:
A. the inventive method trichloro pyridyl sodium alcoholate recovery is higher, can the production yield of trichloro pyridyl sodium alcoholate increased more than 3%, effectively reduces the production cost of trichloro pyridyl sodium alcoholate, has higher rate of return on investment;
B. the waste water salinity after handling through the present invention can reduce more than 60%, and COD can reduce more than 85%, BOD5
5/ COD ratio can increase to more than 0.3, the big enhancing of wastewater biological degradation property, and available common biochemical process is handled the back qualified discharge;
C. can be used as Industrial Salt after the sodium-chlor of present method by-product is made with extra care uses.
Description of drawings
Fig. 1 is a technological process block-diagram of the present invention.
Combine accompanying drawing and embodiment that the present invention is described further at present.
Embodiment
Below in conjunction with embodiment the present invention is made further detailed description, but should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1:
The trichloro pyridyl sodium alcoholate alkaline hydrolysis wastewater flow rate that present embodiment need recycle is 2m
3/ h, its water quality situation is seen table 1.
Table 1 trichloro pyridyl sodium alcoholate and Chlorpyrifos 94 factory effluent water quality situation
| CODcr(mg/L) | Pyridine alcohol sodium content | Chlorobenzene content | PH | B/C | NaCl content | Cu+ content |
| 60000 | 8.25％ | 4.67％ | 10 | 0.17 | 8.7％ | 0.3％ |
The technological process block-diagram of present embodiment is seen Fig. 1, and its technology concrete steps are following:
A. filter: 2m
3The trichloro pyridyl sodium alcoholate alkaline hydrolysis wastewater temperature of/h is 20 ℃; Go to get into successively behind the thick dirt through grid filtration and filter with tripod pendulum type batch centrifugal after being cooled to 5 ℃ in spiral-plate exchanger, the brine cooler, obtain trichloro pyridyl sodium alcoholate crystallisate 240Kg/h (comprising the trichloro pyridyl sodium alcoholate crystallisate that suspends in the waste water);
B. evaporate: the filtrating that filters out among the step a gets into neutralization tank and cools off in the spiral-plate exchanger through the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water in the grid entering spiral-plate exchanger for the neutrality back gets into through its pH value of acid-base neutralisation device adjusting, gets into successively then in multiple-effect evaporator, the scraped film evaporator and is concentrated 10 times;
C. remove sodium-chlor: to being filtered with the suction filtration groove by the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water after concentrating among the step b, obtain sodium-chlor crystallisate 112Kg/h, filtrating is mixed back entering sink drainage and is carried out biochemical treatment with the phlegma that from multiple-effect evaporator, comes out;
D. dry: as to concentrate in together the trichloro pyridyl sodium alcoholate crystal that obtains among the step a and reach dry in drying machine behind the 1000Kg, obtain 706Kg content greater than 85% trichloro pyridyl sodium alcoholate powder.
Through this case method, the recovery of trichloro pyridyl sodium alcoholate reaches 87.3% in the trichloro pyridyl sodium alcoholate waste water, and the sodium-chlor decreasing ratio reaches 64.4%, and waste water COD reduces by 89.4%, BOD5
5/ COD ratio reaches 0.32, and the wastewater biological degradation property significantly strengthens, and available general biochemical method is handled.
Embodiment 2:
Present embodiment need handle the water yield and the water quality situation identical with embodiment 1.The technological process block-diagram of present embodiment is seen Fig. 1, and its technology concrete steps are following:
A. filter: 2m
3The trichloro pyridyl sodium alcoholate alkaline hydrolysis wastewater temperature of/h is 20 ℃; Go to get into successively behind the thick dirt through grid filtration and filter with tripod pendulum type batch centrifugal after being cooled to 0 ℃ in spiral-plate exchanger, the brine cooler, obtain trichloro pyridyl sodium alcoholate crystallisate 259Kg/h (comprising the trichloro pyridyl sodium alcoholate crystallisate that suspends in the waste water);
B. evaporate: the filtrating that filters out among the step a gets into neutralization tank and cools off in the spiral-plate exchanger through the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water in the grid entering spiral-plate exchanger for the neutrality back gets into through its pH value of acid-base neutralisation device adjusting, gets into successively then in multiple-effect evaporator, the scraped film evaporator and is concentrated 12 times;
C. remove sodium-chlor: to being filtered with the suction filtration groove by the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water after concentrating among the step b, obtain sodium-chlor crystallisate 122Kg/h, filtrating is mixed back entering sink drainage and is carried out biochemical treatment with the phlegma that from multiple-effect evaporator, comes out;
D. dry: as to concentrate in together the trichloro pyridyl sodium alcoholate crystal that obtains among the step a and reach dry in drying machine behind the 1000Kg, obtain 706Kg content greater than 85% trichloro pyridyl sodium alcoholate powder.
Through this case method, the recovery of trichloro pyridyl sodium alcoholate reaches 90.5% in the trichloro pyridyl sodium alcoholate waste water, and the sodium-chlor decreasing ratio reaches 76.4%, and waste water COD reduces by 70%, BOD5
5/ COD ratio reaches 0.35, and the wastewater biological degradation property significantly strengthens, and available general biochemical method is handled.
Claims (4)
1. a method that from trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water, reclaims trichloro pyridyl sodium alcoholate belongs to chemical separating and water-treatment technology field, comprises process steps such as filtration, evaporation, dechlorination sodium, drying, it is characterized in that these method concrete steps are following:
A. filter: after trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water removes thick dirt through grid filtration, after supercooler 1 cooling, get into again and continue to be cooled to 0～10 ℃ in the water cooler 2, filter then, obtain the trichloro pyridyl sodium alcoholate crystallisate;
B. evaporate: the filtrating that filters out among the step a gets into neutralization tank and cools off in the water cooler 1 through the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water in the grid entering water cooler 1 for the neutrality back gets into through its pH value of acid-base neutralisation device adjusting, gets into successively then in vaporizer 1, the vaporizer 2 and is concentrated 6～12 times;
C. remove sodium-chlor: to being filtered by the trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water after concentrating, obtain the sodium-chlor crystallisate, filtrating is mixed back entering sink drainage and is carried out biochemical treatment with the phlegma that from multiple-effect evaporator, comes out;
D. dry: as to concentrate in together the trichloro pyridyl sodium alcoholate crystal that obtains among the step a and reach dry in drying machine after the some amount, obtain content greater than 85% trichloro pyridyl sodium alcoholate powder.
2. a kind of method that from trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water, reclaims trichloro pyridyl sodium alcoholate according to claim 1; It is characterized in that water cooler 1 or water cooler 2 among a can be a kind of of dividing wall type water cooler, water drip cooler, jacketed type water cooler and coil pipe type water cooler, heat-eliminating medium can be a kind of in chilled brine, water coolant, the liquefied ammonia etc.
3. a kind of method that from trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water, reclaims trichloro pyridyl sodium alcoholate according to claim 1 is characterized in that vaporizer 1 or vaporizer 2 among the b can be a kind of in single-effect evaporator, multiple-effect falling film vaporizer, multiple-effect climbing-film evaporator, multiple-effect pump feed evaporator, multiple-effect external circulation evaporator, scraped film evaporator, the rotary evaporator etc.
4. a kind of method that from trichloro pyridyl sodium alcoholate alkaline hydrolysis waste water, reclaims trichloro pyridyl sodium alcoholate according to claim 1 is characterized in that straining installation among a or the b can be a kind of in whizzer, suction filtration groove, the pressure filter etc.
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| CN 201210148343 CN102765841B (en) | 2012-05-15 | 2012-05-15 | Method for recovering 3,5,6-Trichloropyridin-2-ol sodium from 3,5,6-Trichloropyridin-2-ol sodium alkaline hydrolysis wastewater |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570176A (en) * | 2013-11-01 | 2014-02-12 | 安徽金禾实业股份有限公司 | Method and device for processing waste water of chlorination workshop section in production of pyridinium |
| CN103922531A (en) * | 2014-04-28 | 2014-07-16 | 江苏九九久科技股份有限公司 | Method for processing 3,5,6-trichloropyridine-2-sodium alcohol wastewater |
| CN104829054A (en) * | 2015-04-29 | 2015-08-12 | 重庆华歌生物化学有限公司 | Method for processing wastewater generated in trichloropyridin-ol sodium production |
| CN105174627A (en) * | 2015-09-21 | 2015-12-23 | 重庆华歌生物化学有限公司 | Method for treating 3,5,6-trichloropyridine-2-sodium alkoxide production waste water |
| CN115321707A (en) * | 2022-08-04 | 2022-11-11 | 内蒙古犇星化学有限公司 | Method for treating alkaline hydrolysis wastewater of mother liquor of sodium trichloropyridinol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103570176A (en) * | 2013-11-01 | 2014-02-12 | 安徽金禾实业股份有限公司 | Method and device for processing waste water of chlorination workshop section in production of pyridinium |
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| CN105174627A (en) * | 2015-09-21 | 2015-12-23 | 重庆华歌生物化学有限公司 | Method for treating 3,5,6-trichloropyridine-2-sodium alkoxide production waste water |
| CN115321707A (en) * | 2022-08-04 | 2022-11-11 | 内蒙古犇星化学有限公司 | Method for treating alkaline hydrolysis wastewater of mother liquor of sodium trichloropyridinol |
| CN115321707B (en) * | 2022-08-04 | 2023-11-21 | 内蒙古犇星化学有限公司 | Mother liquor alkaline hydrolysis wastewater treatment method of sodium trichloropyridine alkoxide |
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