CN106986358A - A kind of purifying technique of pyraclostrobin by-product sodium sulphate - Google Patents

A kind of purifying technique of pyraclostrobin by-product sodium sulphate Download PDF

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Publication number
CN106986358A
CN106986358A CN201710241622.7A CN201710241622A CN106986358A CN 106986358 A CN106986358 A CN 106986358A CN 201710241622 A CN201710241622 A CN 201710241622A CN 106986358 A CN106986358 A CN 106986358A
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CN
China
Prior art keywords
waste water
mvr
pyraclostrobin
sodium sulphate
purifying technique
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710241622.7A
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Chinese (zh)
Inventor
黄金祥
吴建平
刘长庆
戴玉婷
黄显超
杨亚明
张军
徐小兵
朱张
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Guangxin Agrochemcial Co Ltd
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Anhui Guangxin Agrochemcial Co Ltd
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Priority to CN201710241622.7A priority Critical patent/CN106986358A/en
Publication of CN106986358A publication Critical patent/CN106986358A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/16Purification
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention discloses a kind of purifying technique of pyraclostrobin by-product sodium sulphate, the process specifically includes following steps:The waste water sulfur acid sodium synthetically produced to chlorophenyl hydrazine, the waste water of sulfur acid sodium is put into MVR evaporators, stir 12 hours, byproduct sulfite is purified by MVR systems, produce the processing of waste water feeding sewage treatment plant, the present invention can be reclaimed the useful products in pyraclostrobin waste water, improve the value of waste water, reduce destruction of the waste water to water quality, save the cost of processing waste water, the purifying technique design of pyraclostrobin by-product sodium sulphate is optimized, the requirement of the purifying technique design of pyraclostrobin by-product sodium sulphate is met.

Description

A kind of purifying technique of pyraclostrobin by-product sodium sulphate
Technical field
The present invention relates to waste water recycling device technical field, and in particular to a kind of purification of pyraclostrobin by-product sodium sulphate Technique.
Background technology
Methoxy acrylic disinfectant is a class low toxicity, efficient, wide spectrum, interior absorption bactericide, is world pesticide circle The novel agrochemical bactericide of great development potentiality and the market vitality.Pyraclostrobin is the best methoxy acrylic acid of current activity Esters bactericide, it is the earliest developmental research of BASF Aktiengesellschaft, and is released in 2002 in European market.Pyrazoles ether bacterium Ester have the shortcomings that efficiently, low toxicity, environmentally friendly, applicable crops it is extensive.A few years since being listed from pyraclostrobin, The market of the kind is risen violently rapidly, and sales volume rises rapidly, has been classified as the second in all microbial inoculum kind markets, has been only second to phonetic bacterium Ester.
Pyraclostrobin is the methoxy acrylic bactericide for having pyrrazole structure concurrently, and 1993 public by German BASF Department finds, registers and lists within 2001, has been used at present in 100 various crops.2009, its sales volume reached that 7.35 hundred million is beautiful Member, is only second to Fluoxastrobin, as world's second largest bactericide.Pyraclostrobin wide spectrum, efficient, toxicity are low, to non-target organism Safety, it is friendly to user and environment safety, it is that good market prospect in strobilurin series bactericidal agents, patent will mistakes The staple product of phase.
The conventional method of mix reagent crystallization is, when solvent degree is fine in certain solvent for organic matter, first to use being somebody's turn to do for minimum Solvent is dissolved by heating, and is reheated the slightly worse another solvent of solubility, is reduced the solubility of the organic matter, then cooling analysis Go out crystal.Either product is dissolved with the solvent of minimal amount of favorable solubility at reflux, then from condenser pipe The relatively low solvent of dissolubility is added, to solution Hun Chi, then the drop that flows back is clear, and cooling is separated out.But this method can crystallize product Not exclusively, solvent recovery is not thorough, so as to influence the yield of product, increases post processing cost.
Waste water after the synthesis of original pyraclostrobin is that to be directly transported to sewage treatment plant of company without workshop processing straight Processing is connect, toxic composition and recyclable composition are contained in inside;Through the research of repetitious pilot plant test and big pilot production, Finally a feasible handling process route is explored, for solving problems with:
Giving up after the pyraclostrobin synthesis that sewage treatment plant of company is directly handled directly is transported to 1. being handled without workshop More harmful substance is contained in water, inside, and substantial amounts of noxious material is produced in water, water quality is had a strong impact on;
Giving up after the pyraclostrobin synthesis that sewage treatment plant of company is directly handled directly is transported to 2. being handled without workshop More deleterious acidic thing is contained in water, inside, is capable of the production equipment of sewage treatment plant of burn into destruction company, is unfavorable for production And processing;
Giving up after the pyraclostrobin synthesis that sewage treatment plant of company is directly handled directly is transported to 3. being handled without workshop The sodium sulphate for being recoverable to and utilizing is contained in water, inside, the sodium sulphate of the high-purity obtained by distillation and crystallization, can be used as pair Output is sold, and saves cost for wastewater treatment, and is fed directly to sewage treatment plant's processing, it is impossible to by-product is effectively reclaimed, seriously Damage economy.
The content of the invention
To solve the above problems, the present invention proposes a kind of purifying technique of pyraclostrobin by-product sodium sulphate.
To realize the object of the invention, the technical scheme of use is:A kind of purifying technique of pyraclostrobin by-product sodium sulphate, The purifying technique of described pyraclostrobin by-product sodium sulphate is concretely comprised the following steps:
(1) evaporative crystallizations:The waste water sulfur acid sodium synthetically produced to chlorophenyl hydrazine, by the waste water of sulfur acid sodium by feed pump It is delivered in horizontal-type evaporator and is exchanged heat with heating steam, MVR crystal separators is entered after being exchanged heat with heating steam, Continuously stir 1-2 hours, the waste water evaporation entered in MVR crystal separators produces indirect steam and sodium sulphate concentrate;
(2) wastewater treatments:The indirect steam that evaporation process is produced in MVR crystal separators flows through vapour compression machine progress Both vapor compression processing, is changed into the heating steam of HTHP small size from low-temp low-pressure large volume, and heating steam steams by horizontal After hair device is exchanged heat with the waste water conveyed from feed pump and circulating pump, heating steam is released and condensed after heat, as condensation Waste water, will produce the processing of condensation waste water feeding sewage treatment plant.
It is preferred that, the evaporation mode carried out in described MVR crystal separators is a kind of flash distillation mode, the stirring side of progress Formula is the mechanical agitation mode that a kind of agitator drives, and stir speed (S.S.) is 500~1000 turns/min.
It is preferred that, described MVR crystal separators and agitator integrated design, wherein, agitator is crystallized installed in MVR In separator top end cover, the agitating paddle of agitator is 15~20cm with the height distance of MVR crystal separators bottom.
It is preferred that, the circulating pump accounts for MVR crystal separators 1/4-1/ inside MVR crystal separators containing wastewater volume Circulated during 2 volume, wherein, it is up to 1/2 that the wastewater volume, which accounts for MVR crystal separator volumes,.
It is preferred that, 2 circulations are provided with the MVR systems, 1 is crystallized by vapour compression machine, horizontal-type evaporator and MVR The steam thermal cycle of separator composition, 1 feed liquid SAPMAC method for being made up of circulating pump, horizontal-type evaporator and MVR crystal separators.
Compared with prior art, the beneficial effects of the invention are as follows:A kind of pyraclostrobin by-product sulphur involved in the present invention The purifying technique of sour sodium, the process specifically includes following steps:The waste water sulfur acid sodium synthetically produced to chlorophenyl hydrazine, The waste water of sulfur acid sodium is put into MVR evaporators, stirred 1-2 hours, byproduct sulfite, production are purified by MVR systems Raw waste water feeding sewage treatment plant processing, with advantages below:
1. the purifying technique of pyraclostrobin by-product sodium sulphate of the present invention, first waste water is carried out effective heat exchange and Evaporation, the acid low-boiling-point substance inside waste water is steamed, and carries out recycling, it is to avoid destruction of the acid low-boiling-point substance to water quality, Save cost;
2. the purifying technique of pyraclostrobin by-product sodium sulphate of the present invention, first waste water is carried out effective heat exchange and Evaporation, the acid low-boiling-point substance inside waste water steamed, and carries out recycling, it is to avoid acid low-boiling-point substance is to company's sewage disposal The burn into destruction of plant, has ensured personal safety and the property safety of sewage treatment plant;
3. the purifying technique of pyraclostrobin by-product sodium sulphate of the present invention, will synthesis, it is refined after carry out to waste water Recycling, obtain the sodium sulphate of high-purity that can be sold as byproduct, cost can be reduced by selling byproduct, be embodied Economy and practicality, optimize the purifying technique design of pyraclostrobin by-product sodium sulphate, meet pyraclostrobin pair Produce the requirement of the purifying technique design of sodium sulphate.
Brief description of the drawings
Fig. 1 is the purifying technique flow chart of pyraclostrobin by-product sodium sulphate of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
Refer to shown in Fig. 1, the technical solution adopted by the present invention is:A kind of purification work of pyraclostrobin by-product sodium sulphate Skill, the purifying technique of described pyraclostrobin by-product sodium sulphate is concretely comprised the following steps:
(1) evaporative crystallizations:The waste water sulfur acid sodium synthetically produced to chlorophenyl hydrazine, by the waste water of sulfur acid sodium by feed pump It is delivered in horizontal-type evaporator and is exchanged heat with heating steam, MVR crystal separators is entered after being exchanged heat with heating steam, Continuously stir 1-2 hours, the waste water evaporation entered in MVR crystal separators produces indirect steam and sodium sulphate concentrate;
(2) wastewater treatments:The indirect steam that evaporation process is produced in MVR crystal separators flows through vapour compression machine progress Both vapor compression processing, is changed into the heating steam of HTHP small size from low-temp low-pressure large volume, and heating steam steams by horizontal After hair device is exchanged heat with the waste water conveyed from feed pump and circulating pump, heating steam is released and condensed after heat, as condensation Waste water, will produce the processing of condensation waste water feeding sewage treatment plant.
Operation principle:In use, due to the waste water sulfur acid sodium synthetically produced to chlorophenyl hydrazine, the waste water of sulfur acid sodium is thrown Enter into MVR evaporators, waste water, which first passes through feed pump waste water is delivered to inside horizontal-type evaporator, effectively to be exchanged heat, cold fluid For waste water, hot fluid is heating steam, and heating steam is condensed after horizontal-type evaporator, produces condensed water, will produce condensation The processing of waste water feeding sewage treatment plant, the waste water by heat exchange is entered inside MVR crystal separators, in MVR crystal separators Inside is stirred 1-2 hours using agitator, the circulating pump being provided with, and is entered when containing more waste water inside MVR crystal separators MVR crystal separators are flashed the indirect steam produced and are compressed by row circulation, the vapour compression machine being provided with, and obtain high heat Heating steam, heating steam participate in heat exchange, pass through MVR systems purify byproduct sulfite, produce waste water feeding sewage disposal Factory and office manage.
Further, the evaporation mode carried out in described MVR crystal separators is a kind of flash distillation mode, the stirring of progress Mode is the mechanical agitation mode that a kind of agitator drives, and stir speed (S.S.) is 500~1000 turns/min.
Further, described MVR crystal separators and agitator integrated design, wherein, agitator is tied installed in MVR In brilliant separator top end cover, the agitating paddle of agitator is 15~20cm with the height distance of MVR crystal separators bottom.
Further, the circulating pump accounts for MVR crystal separators 1/4- inside MVR crystal separators containing wastewater volume Circulated during 1/2 volume, wherein, it is up to 1/2 that the wastewater volume, which accounts for MVR crystal separator volumes,.
Further, 2 circulations are provided with the MVR systems, 1 is tied by vapour compression machine, horizontal-type evaporator and MVR The steam thermal cycle of brilliant separator composition, 1 feed liquid being made up of circulating pump, horizontal-type evaporator and MVR crystal separators is cold to be followed Ring.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (5)

1. a kind of purifying technique of pyraclostrobin by-product sodium sulphate, it is characterised in that:Described pyraclostrobin by-product sulfuric acid The purifying technique of sodium is concretely comprised the following steps:
(1) evaporative crystallizations:The waste water sulfur acid sodium synthetically produced to chlorophenyl hydrazine, the waste water of sulfur acid sodium is conveyed by feed pump Exchanged heat in horizontal-type evaporator with heating steam, enter MVR crystal separators after being exchanged heat with heating steam, continuously Stirring 1-2 hours, the waste water evaporation entered in MVR crystal separators produces indirect steam and sodium sulphate concentrate;
(2) wastewater treatments:The indirect steam that evaporation process is produced in MVR crystal separators flows through vapour compression machine and carries out steam Compression is handled, and is changed into the heating steam of HTHP small size from low-temp low-pressure large volume, and heating steam passes through horizontal-type evaporator After being exchanged heat with the waste water from feed pump and circulating pump conveying, heating steam is released and condensed after heat, as condensation waste water, The processing of condensation waste water feeding sewage treatment plant will be produced.
2. the purifying technique of pyraclostrobin by-product sodium sulphate according to claim 1, it is characterised in that:Described MVR The evaporation mode carried out in crystal separator is a kind of flash distillation mode, and the agitating mode of progress is the machinery that a kind of agitator drives Agitating mode, stir speed (S.S.) is 500~1000 turns/min.
3. the purifying technique of pyraclostrobin by-product sodium sulphate according to claim 1, it is characterised in that:Described MVR Crystal separator and agitator integrated design, wherein, agitator is arranged in MVR crystal separator top end covers, agitator The height distance of agitating paddle and MVR crystal separators bottom be 15~20cm.
4. the purifying technique of pyraclostrobin by-product sodium sulphate according to claim 1, it is characterised in that:The circulating pump Circulated when accounting for MVR crystal separator 1/4-1/2 volumes containing wastewater volume inside MVR crystal separators, wherein, it is described It is up to 1/2 that wastewater volume, which accounts for MVR crystal separator volumes,.
5. the purifying technique of pyraclostrobin by-product sodium sulphate according to claim 1, it is characterised in that:The MVR systems 2 circulations are provided with system, 1 steam thermal cycle for being made up of vapour compression machine, horizontal-type evaporator and MVR crystal separators, 1 The individual feed liquid SAPMAC method being made up of circulating pump, horizontal-type evaporator and MVR crystal separators.
CN201710241622.7A 2017-04-13 2017-04-13 A kind of purifying technique of pyraclostrobin by-product sodium sulphate Pending CN106986358A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN108751597A (en) * 2018-06-22 2018-11-06 江苏宜裕环保科技有限公司 A kind of method of high-performance bio strain processing pyraclostrobin agricultural chemicals waste water
CN108862783A (en) * 2018-05-29 2018-11-23 安徽广信农化股份有限公司 A kind of process of salicylonitrile wastewater treatment
CN109704368A (en) * 2019-02-20 2019-05-03 宁夏恒力生物新材料有限责任公司 A kind of sodium sulphate method of purification
CN109798696A (en) * 2019-01-23 2019-05-24 江苏科技大学 A kind of recycling of industrial wastewater waste heat is the high temperature heat pump system and its control method of working medium to water

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CN109798696A (en) * 2019-01-23 2019-05-24 江苏科技大学 A kind of recycling of industrial wastewater waste heat is the high temperature heat pump system and its control method of working medium to water
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