CN104876394A - Deep treatment method for wastewater containing 3,5,6-trichloropyridine-2-sodium alcoholate - Google Patents
Deep treatment method for wastewater containing 3,5,6-trichloropyridine-2-sodium alcoholate Download PDFInfo
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- CN104876394A CN104876394A CN201510242826.3A CN201510242826A CN104876394A CN 104876394 A CN104876394 A CN 104876394A CN 201510242826 A CN201510242826 A CN 201510242826A CN 104876394 A CN104876394 A CN 104876394A
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- trichloropyridine
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Abstract
The invention relates to the field of sewage treatment in environmental protection, and particularly relates to a deep treatment method for wastewater containing 3,5,6-trichloropyridine-2-sodium alcoholate. The method comprises the following specific operation steps: regulating wastewater containing 3,5,6-trichloropyridine-2-sodium alcoholate to be acidic; enabling the acidic wastewater to sequentially flow into a sedimentation kettle, a precipitation tank and a filter and enabling the filtered wastewater to flow into a macroporous resin adsorption device; adding a desorbing agent and clear water into the resin to perform desorption regeneration and recycling the resin; adsorbing 3,5,6-trichloropyridine-2-sodium alcoholate of which the content is less than 0.5mg/L in effluent water; distilling desorption liquid and recycling the desorption agent for repeated utilization; distilling 3,5,6-trichloropyridine-2-sodium alcoholate of which the content is 1-5% in a base solution; and returning to the precipitation tank. The method is low in process cost, environmentally friendly and energy-saving, and has a good sewage treatment effect.
Description
Technical field
The present invention relates to a kind of advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, belong to sewage treatment area.
Background technology
3,5,6-trichloropyridine-2-sodium alkoxide is the raw material producing organic phosphorous insecticide Chlorpyrifos 94, chlorpyrifos_methyl, and be slightly soluble in water, in frozen water, saturation concentration about 0.5%, is soluble in the organic solvent such as methyl alcohol, ethanol, and the conventional purity of industry is more than 85%.3,5,6-trichloropyridine-2-sodium alkoxide is easily hydrolyzed to trichloropyridine alcohol in acid condition, trichloropyridine alcohol is water insoluble, easily with conventional immiscible organic solvent, and white or cream powder, organism has solublization to it, and its tiny natural subsidence speed generated is slow.
There is emulsifying agent and a small amount of Chlorpyrifos 94 crude oil and other organism, normally microemulsified state in Chlorpyrifos 94 factory effluent, have 3,5,6-a large amount of trichloropyridine-2-sodium alkoxide suspended substances simultaneously, make 3,5,6-trichloropyridine-2-sodium alkoxide amounts in waste water to reach 3% ~ 5%.Conventional method reclaims major part 3 by the technique of filtration-concentrated-filtration or acidifying-precipitation-filtration, 5,6-trichloropyridine-2-sodium alkoxide or trichloropyridine alcohol, in waste water 0.05% ~ 0.5% 3,5,6-trichloropyridine-2-sodium alkoxide or trichloropyridine alcohol by chemical oxidation or dilution tens times after enter biochemical system, which increase cost for wastewater treatment, also result in the waste of 3,5,6-trichloropyridine-2-sodium alkoxide.
Macroporous resin stable in properties, has huge specific surface area, and by physisorption adsorb organic compound selectively, reusable, can not cause secondary pollution, energy consumption is low.The industrial impurity removal and purification technique being mainly used in natural organic matter extract at present, applies mainly to concentrate on and removes COD, colourity etc. in waste water treatment process.It is the successful case that macroporous resin is applied to material recycle in waste water that the enrichment of macroporous resin to glyphosate waste water glyphosate concentrates.But macroporous resin has no report to the selective adsorption of 3,5,6-trichloropyridine-2-sodium alkoxide.
The technical problem solved, the recovery of 3,5,6-trichloro pyridyl sodium alcoholates and removal in waste water, the dephosphorization of organism P wastewater, the recycling of Phosphorus From Wastewater.Exclusive technical characteristic: form concentrated solution after organism P wastewater resin absorption equipment carries out fractionation by adsorption, containing large amount of organic in concentrated solution, hardly containing inorganic salt, is conducive to the recycling of microcosmic salt.
Summary of the invention
Main purpose of the present invention screens suitable macroporous adsorbent resin, complete 3,5, the selective adsorption that 6-trichloropyridine-2-alcohol intermediate send, optimization process technique, by a kind of method of less energy-consumption, low cost, the degree of depth reclaims in waste water 3,5,6-trichloropyridine-2-sodium alkoxide, reaches the effect of administering waste water simultaneously.
The present invention is based on the following research fact: containing can be rapidly converted into after 3,5,6-trichloropyridine-2-sodium alkoxide waste water acid adding solubleness lower 3,5,6-trichloropyridine-2-alcohol, 3,5,6-trichloropyridine-2-alcohol, can be precipitated in conjunction with settling tank further by Multistage settling still; But still have tiny 3,5,6-trichloropyridine-2-alcohol suspended substances in a large number in waste water.
The technical solution used in the present invention is as follows:
A kind of advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, comprises acidifying, precipitation process, it is characterized in that, comprise the following steps:
(1) in the waste water containing 3,5,6-trichloropyridine-2-sodium alkoxide, adding sulphur acid for adjusting pH is 1-2;
(2) acid waste water enters strainer after six grades of sedimentation stills, settling tank;
(3) waste water after filtering enters macroporous resin adsorption device, and absorption water outlet enters biochemical treatment system;
(4) add in resin after desorbing agent and clear water carry out desorption and regeneration and reuse;
(5) desorption liquid is after distillation, reclaims desorbing agent, and distillation end liquid returns settling tank;
Described macroporous adsorbent resin is amido modified styryl structures resin.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, described strainer is kieselguhr filter.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, is characterized in that, the filtering medium used in described strainer is calcined diatomite, the mixing of one or both in flux calcination diatomite.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, is characterized in that: described macroporous resin median size is 3 ~ 5nm.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, described resin absorption water intake velocity is the resin volume of 0.8 ~ 1.5 times per hour.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, is characterized in that, described resin absorption is 2 post series connection absorption mode.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, described resin absorption single treatment wastewater flow rate is 8 ~ 12 times of resin volumes.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, described desorbing agent is the mixing of the one or both in methyl alcohol, ethanol, and described desorbing agent consumption is the resin volume of 1 ~ 2 times.
The described advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that: described rinse dosage is 4 times of resin volumes, flow velocity is 0.5 ~ 0.8 times of resin volume.
Positive progressive effect of the present invention is:
1) with kieselguhr filter in conjunction with suitable diatomite proportioning, can adsorb the suspended particle in waste water, oily matter and emulsifying agent, water outlet is limpid.2) optimize suitable resin absorption-separating process, 3,5, the 6-trichloropyridine-2-alcohol effects removed in waste water are fine, and in water outlet, content is at below 0.5mg/L.3,5,6-trichloropyridine-2-sodium alkoxide almost reclaims completely.3) desorbing agent is lower boiling organic alcohols, easy recycling, and improve atom utilization, the desorbing agent of recovery can be reused, cost-saving.
Embodiment
For a better understanding of the present invention, further illustrate the present invention below in conjunction with embodiment, but be not limitation of the present invention.
Embodiment 1:
3,5,6-trichloropyridine-2-sodium alkoxide produces alkaline hydrolysis waste water, reddish black turbid system, alkalescence.
It is 1 ~ 2 that waste water waste water adds sulphur acid for adjusting pH, trichloro pyridyl sodium alcoholate is changed into trichloropyridine alcohol.After acidifying, waste water pumps into six grades of series connection sedimentation stills and three grades of settling tanks successively.Add 2L coarse particles hydrotropy calcined diatomite and 1L fine particle calcined diatomite in strainer, carry out repeatedly film to film clarification of water; It is limpid to water outlet that waste water after precipitation enters kieselguhr filter circulation absorption.Absorption water outlet pumps into is equipped with 1m
3the adsorption system of macroporous resin, two post series connection absorption, water intake velocity is 0.8m per hour
3; Water inlet is stopped after running 10h.Add 2m successively
3methyl alcohol and 4m
3tap water carries out resin desorption regeneration.Collect 2m successively
3methyl alcohol and 0.3m
3rinse water is desorption liquid, applies mechanically during cleaning next time of residue rinse water.Desorption liquid reclaims after methyl alcohol through rectifying tower and obtains liquid at the bottom of pulpous state, returns settling tank.
Trichloropyridine alcohol (sodium) content in water after the process of table 1. Yuan Shuijige workshop section
Embodiment 2:
Chlorpyrifos 94 Workshop Production waste water, oyster white suspension system, alkalescence.
It is 1 ~ 2 that waste water adds sulphur acid for adjusting pH, trichloro pyridyl sodium alcoholate is changed into trichloropyridine alcohol.After acidifying, waste water pumps into six grades of series connection sedimentation stills and three grades of settling tanks successively.Add 2L fine particle calcined diatomite in strainer, film is to film clarification of water repeatedly; It is limpid to water outlet that waste water after precipitation enters kieselguhr filter circulation absorption.Absorption water outlet pumps into is equipped with 1m
3the adsorption system of macroporous resin, two post series connection absorption, water intake velocity is 1.5m per hour
3; Water inlet is stopped after running 7h.Add 2m successively
3methyl alcohol and 4m
3tap water carries out resin desorption regeneration.Collect 2m successively
3methyl alcohol and 0.5m
3rinse water is desorption liquid, applies mechanically during cleaning next time of residue rinse water.Desorption liquid reclaims after methyl alcohol through rectifying tower and obtains liquid at the bottom of pulpous state, returns settling tank.
Trichloropyridine alcohol (sodium) content in water after the process of table 2. Yuan Shuijige workshop section
Claims (9)
1. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide, comprises acidifying, precipitation process, it is characterized in that, comprise the following steps:
(1) in the waste water containing 3,5,6-trichloropyridine-2-sodium alkoxide, adding sulphur acid for adjusting pH is 1-2;
(2) acid waste water enters strainer after six grades of sedimentation stills, settling tank;
(3) waste water after filtering enters macroporous resin adsorption device, and absorption water outlet enters biochemical treatment system;
(4) add in resin after desorbing agent and clear water carry out desorption and regeneration and reuse;
(5) desorption liquid is after distillation, reclaims desorbing agent, and distillation end liquid returns settling tank;
Described macroporous adsorbent resin is amido modified styryl structures resin.
2. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that, described strainer is kieselguhr filter.
3. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 2, is characterized in that, the filtering medium used in described strainer is calcined diatomite, the mixing of one or both in flux calcination diatomite.
4. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, is characterized in that: described macroporous resin median size is 3 ~ 5nm.
5. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that, described resin absorption water intake velocity is the resin volume of 0.8 ~ 1.5 times per hour.
6. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, is characterized in that, described resin absorption is 2 post series connection absorption mode.
7. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that, described resin absorption single treatment wastewater flow rate is 8 ~ 12 times of resin volumes.
8. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that, described desorbing agent is the mixing of the one or both in methyl alcohol, ethanol, and described desorbing agent consumption is the resin volume of 1 ~ 2 times.
9. the advanced waste treatment method containing 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that: described rinse dosage is 4 times of resin volumes, flow velocity is 0.5 ~ 0.8 times of resin volume.
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CN105217888A (en) * | 2015-10-16 | 2016-01-06 | 河北美邦工程科技股份有限公司 | A kind of method processing pyridine derivate waste water |
CN105481137A (en) * | 2015-12-04 | 2016-04-13 | 安徽国星生物化学有限公司 | Recycling treatment process for wastewater from chlorpyrifos production |
CN113087255A (en) * | 2019-12-23 | 2021-07-09 | 南京延长反应技术研究院有限公司 | Pyridine wastewater treatment system and method |
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Cited By (4)
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CN105217888A (en) * | 2015-10-16 | 2016-01-06 | 河北美邦工程科技股份有限公司 | A kind of method processing pyridine derivate waste water |
CN105481137A (en) * | 2015-12-04 | 2016-04-13 | 安徽国星生物化学有限公司 | Recycling treatment process for wastewater from chlorpyrifos production |
CN113087255A (en) * | 2019-12-23 | 2021-07-09 | 南京延长反应技术研究院有限公司 | Pyridine wastewater treatment system and method |
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Application publication date: 20150902 |