CN107098364A - A kind of purifying technique of pyraclostrobin by-product sodium bromide - Google Patents
A kind of purifying technique of pyraclostrobin by-product sodium bromide Download PDFInfo
- Publication number
- CN107098364A CN107098364A CN201710250607.9A CN201710250607A CN107098364A CN 107098364 A CN107098364 A CN 107098364A CN 201710250607 A CN201710250607 A CN 201710250607A CN 107098364 A CN107098364 A CN 107098364A
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- CN
- China
- Prior art keywords
- sodium bromide
- mvr
- waste water
- pyraclostrobin
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/10—Bromides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/043—Details
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/06—Flash evaporation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
Abstract
The invention discloses a kind of purifying technique of pyraclostrobin by-product sodium bromide, the process specifically includes following steps：The synthetically produced waste water of adjacent nitro benzyl bromine contains sodium bromide, it will contain in sodium bromide waste water input MVR evaporators, stir 12 hours, byproduct sodium bromide is purified by MVR systems, produce the processing of waste water feeding sewage treatment plant, purification sodium bromide is used as byproduct, 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, optimize the purifying technique design of pyraclostrobin by-product sodium bromide, meet the requirement of the purifying technique design of pyraclostrobin by-product sodium bromide.
Description
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 bromide
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 has efficient, low toxicity, the extensive shortcoming of environmentally friendly, applicable crops；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 bromide.
To realize the object of the invention, the technical scheme of use is：A kind of purifying technique of pyraclostrobin by-product sodium bromide,
The purifying technique of described pyraclostrobin by-product sodium bromide is concretely comprised the following steps：
(1) evaporative crystallizations：The synthetically produced waste water of adjacent nitro benzyl bromine contains sodium bromide, by the waste water containing sodium bromide by feeding
Pump is delivered in horizontal-type evaporator to be exchanged heat with heating steam, and MVR Crystallization Separations are entered after being exchanged heat with heating steam
Device, is continuously stirred 1-2 hours, and the waste water evaporation entered in MVR crystal separators produces indirect steam and sodium bromide 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 500~2000 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, agitator with the height distance of MVR crystal separators bottom
Outer surface is enclosed with noise-reduction device.
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.
It is preferred that, the MVR crystal separators are internally provided with spiral heating coiled pipe, the design height of spiral heating coiled pipe
For the 1/2-2/3 of MVR crystal separator height, spiral heating coiled pipe internal flow has high-temperature hot fluid, according to heating-up temperature heat
Fluid media (medium) is one kind in water, silicone oil and sand.
Compared with prior art, the beneficial effects of the invention are as follows：A kind of pyraclostrobin by-product bromine involved in the present invention
Change the purifying technique of sodium, the process specifically includes following steps：The synthetically produced waste water of adjacent nitro benzyl bromine contains bromination
Sodium, will contain in sodium bromide waste water input MVR evaporators, and stir 1-2 hours, byproduct sodium bromide is purified by MVR systems, produce
The processing of waste water feeding sewage treatment plant, purification sodium bromide is as byproduct, with advantages below：
1. the purifying technique of pyraclostrobin by-product sodium bromide 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 bromide 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 bromide 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 bromide, meet pyraclostrobin pair
Produce the requirement of the purifying technique design of sodium bromide.
Brief description of the drawings
Fig. 1 is the purifying technique flow chart of pyraclostrobin by-product sodium bromide 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 bromide
Skill, the purifying technique of described pyraclostrobin by-product sodium bromide is concretely comprised the following steps：
(1) evaporative crystallizations：The synthetically produced waste water of adjacent nitro benzyl bromine contains sodium bromide, by the waste water containing sodium bromide by feeding
Pump is delivered in horizontal-type evaporator to be exchanged heat with heating steam, and MVR Crystallization Separations are entered after being exchanged heat with heating steam
Device, is continuously stirred 1-2 hours, and the waste water evaporation entered in MVR crystal separators produces indirect steam and sodium bromide 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, because the synthetically produced waste water of adjacent nitro benzyl bromine contains sodium bromide, by the waste water containing sodium bromide
Put 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 flow
Body is waste water, and hot fluid is heating steam, and heating steam is condensed after horizontal-type evaporator, produces condensed water, will produce cold
Solidifying waste water feeding sewage treatment plant processing, the waste water by heat exchange is entered inside MVR crystal separators, in MVR Crystallization Separations
Stirred 1-2 hours using agitator inside device, the circulating pump being provided with, when containing more waste water inside MVR crystal separators
Circulated, MVR crystal separators are flashed the indirect steam produced and are compressed by the vapour compression machine being provided with, and obtain hyperpyrexia
The heating steam of amount, heating steam participates in heat exchange, and byproduct sodium bromide is purified by MVR systems, produces at waste water feeding sewage
Manage factory and office's reason.
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 500~2000 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, stirring with the height distance of MVR crystal separators bottom
Device outer surface is enclosed with noise-reduction device.
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.
Further, the MVR crystal separators are internally provided with spiral heating coiled pipe, and the design of spiral heating coiled pipe is high
Spend for the 1/2-2/3 of MVR crystal separator height, spiral heating coiled pipe internal flow has high-temperature hot fluid, according to heating-up temperature
Hot fluid medium is one kind in water, silicone oil and sand.
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 (6)
1. a kind of purifying technique of pyraclostrobin by-product sodium bromide, it is characterised in that：Described pyraclostrobin by-product bromination
The purifying technique of sodium is concretely comprised the following steps：
(1) evaporative crystallizations：The synthetically produced waste water of adjacent nitro benzyl bromine contains sodium bromide, and the waste water containing sodium bromide is defeated by feed pump
Deliver in horizontal-type evaporator and to be exchanged heat with heating steam, enter MVR crystal separators with heating after steam is exchanged heat, company
Continuous stirring 1-2 hours, the waste water evaporation entered in MVR crystal separators produces indirect steam and sodium bromide 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 bromide 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 500~2000 turns/min.
3. the purifying technique of pyraclostrobin by-product sodium bromide 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, agitator outer surface is enclosed with noise-reduction dress
Put.
4. the purifying technique of pyraclostrobin by-product sodium bromide 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 bromide 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.
6. the purifying technique of pyraclostrobin by-product sodium bromide according to claim 1, it is characterised in that：The MVR knots
Brilliant separator interior is provided with spiral heating coiled pipe, and the design height of spiral heating coiled pipe is the 1/ of MVR crystal separator height
2-2/3, spiral heating coiled pipe internal flow has high-temperature hot fluid, according to heating-up temperature hot fluid medium in water, silicone oil and sand
One kind.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710250607.9A CN107098364A (en) | 2017-04-17 | 2017-04-17 | A kind of purifying technique of pyraclostrobin by-product sodium bromide |
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| CN201710250607.9A CN107098364A (en) | 2017-04-17 | 2017-04-17 | A kind of purifying technique of pyraclostrobin by-product sodium bromide |
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| CN201710250607.9A Pending CN107098364A (en) | 2017-04-17 | 2017-04-17 | A kind of purifying technique of pyraclostrobin by-product sodium bromide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112024130A (en) * | 2020-08-06 | 2020-12-04 | 陈素恩 | Phosphogypsum flotation device |
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| CN102745755A (en) * | 2011-10-25 | 2012-10-24 | 河北凯徳生物材料有限公司 | Process for recovering sodium sulfate crystal in sebacic acid production |
| CN203447809U (en) * | 2013-07-05 | 2014-02-26 | 重庆江增船舶重工有限公司 | MVR (Mechanical Vapor Recompression) evaporative crystallization system |
| CN203959862U (en) * | 2014-06-16 | 2014-11-26 | 溧阳德维透平机械有限公司 | A kind of MVR evaporation concentration equipment for high-salt wastewater treatment industry |
| CN104399266A (en) * | 2014-11-05 | 2015-03-11 | 广州市心德实业有限公司 | MVR evaporation device and partial pressure evaporation method |
| CN104986747A (en) * | 2015-06-26 | 2015-10-21 | 江苏瑞升华能源科技有限公司 | Preparation method of dihydrate disodium hydrogen phosphate |
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2017
- 2017-04-17 CN CN201710250607.9A patent/CN107098364A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102745755A (en) * | 2011-10-25 | 2012-10-24 | 河北凯徳生物材料有限公司 | Process for recovering sodium sulfate crystal in sebacic acid production |
| CN203447809U (en) * | 2013-07-05 | 2014-02-26 | 重庆江增船舶重工有限公司 | MVR (Mechanical Vapor Recompression) evaporative crystallization system |
| CN203959862U (en) * | 2014-06-16 | 2014-11-26 | 溧阳德维透平机械有限公司 | A kind of MVR evaporation concentration equipment for high-salt wastewater treatment industry |
| CN104399266A (en) * | 2014-11-05 | 2015-03-11 | 广州市心德实业有限公司 | MVR evaporation device and partial pressure evaporation method |
| CN104986747A (en) * | 2015-06-26 | 2015-10-21 | 江苏瑞升华能源科技有限公司 | Preparation method of dihydrate disodium hydrogen phosphate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112024130A (en) * | 2020-08-06 | 2020-12-04 | 陈素恩 | Phosphogypsum flotation device |
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Application publication date: 20170829 |