CN109896683A - The cycling and reutilization treatment process of time acid producing waste water - Google Patents
The cycling and reutilization treatment process of time acid producing waste water Download PDFInfo
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- CN109896683A CN109896683A CN201910232462.9A CN201910232462A CN109896683A CN 109896683 A CN109896683 A CN 109896683A CN 201910232462 A CN201910232462 A CN 201910232462A CN 109896683 A CN109896683 A CN 109896683A
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- time acid
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Abstract
The invention discloses a kind of cycling and reutilization treatment process of time acid producing waste water.The dense salt waste water generated in time acid production process through oil removal, multiple-effect evaporation, is obtained byproduct sodium chloride salt by the technique, while evaporation water is collected separately and is back in time acid production system, and for mother liquor again after recovered organic product, set is used for multiple-effect evaporation.Present invention process can greatly reduce the processing of brine waste, mitigate the pressure of biochemical treatment, 50% or more emission reduction.Using present invention process, 1 ton of time acid of every production will rationally recycle 7 tons of water of evaporation, 10 tons of emission reduction of waste water total amount, and also bring great convenience to three-protection design.
Description
Technical field
The present invention relates to a kind of cycling and reutilization treatment process of time acid producing waste water, belong to Industrial Wastewater Treatment and clear
Clean production technical field.
Background technique
Large and medium-sized pyrethrin pesticide manufacturing enterprise during synthesizing pyrethrin pesticide be typically all since the synthesis of intermediate,
The especially manufacturing enterprises such as cyhalothrin, Biphenthrin, the overwhelming majority are produced since the synthesis of intermediate time acid.Currently,
The raw materials such as 3,3-dimethyl-4-pentenoic acid methyl ester, trifluorotrichloroethane are mainly passed through addition, cyclisation, soap by industrialized time acid production process
The processes synthesis time such as change, acidification, purification acid.Due to having used a large amount of organic matter raw material in time acid production process, such as
3,3-dimethyl-4-pentenoic acid methyl ester, trifluorotrichloroethane, ethanol amine etc. and organic solvent, such as the tert-butyl alcohol, n,N-Dimethylformamide
(DMF) etc., while containing a large amount of salt, such as stannous chloride, sodium tert-butoxide, liquid alkaline, saponification in raw material and in reaction process
The salts such as catalyst, thus time acid producing waste water complicated component and wastewater flow rate it is big, produce time acid per ton by process conditions extremely
Major general generates dense 20 tons of salt waste water or so, and waste water is difficult to be efficiently used or recycled higher cost.
The treatment process of existing time acid producing waste water is discharged again after mainly passing through oil removal, dilution, biochemical treatment.China
Patent 201520971951.3 discloses a kind of time acid production system based on membrane technology, passes through ceramic membrane filter device
Catalyst is recycled, trifluorotrichloroethane is recycled by distillation device, by bipolar membrane device by the salt treatment after saponification
At lye and acid solution, lye reuse is into saponification kettle.Above-mentioned production system realizes in waste water by using a variety of devices
The separation of main component, but water after the recovery is mainly back in saponification in the form of lye.
Summary of the invention
The purpose of the present invention is to provide a kind of cycling and reutilization treatment process of time acid producing waste water, which is used
Sewage separation and the mode individually evaporated, evaporation water individually enter recovery system storage, for producing the reuse of time acid system, simultaneously
The quality and yield of time acid are not influenced.
Realize that the technical solution of the object of the invention is as follows:
The cycling and reutilization treatment process of time acid producing waste water, specifically:
Step 1, Sewage treatment: time acid producing waste water enters density wastewater intermediate pool after oil partition tank, then is pumped into multiple-effect steaming
Rise wastewater disposal basin, opens multi-effect evaporation system, is pumped into density wastewater, adjusts negative-pressure vacuum system, opens steam-heating system, make into
Output balance is then turned on salt recovery system, collects side product chlorinated sodium salt, and evaporation water is individually deposited in recycle-water reserve tank
In, time acid to be produced uses；
Step 2, the evaporation water of recycling recycles: evaporation water is added into precipitation kettle after saponification, carrying out precipitation treatment for time acid
Dilution is acidified, and filtering obtains time acid crude, time acid fine work is obtained after recrystallization.
Time acid producing waste water of the invention can be the waste water generated in water rinses, saponification stage or precipitation stage.
For time acid producing waste water of the invention after oil partition tank, it is 7.5 that obtained water outlet, which is neutralized to pH, enters back into density wastewater
Intermediate pool.
The effect grade of multi-effect evaporation system of the invention can be 2~6 effects, preferably 3~4 effects.
The cycling and reutilization treatment process of time acid producing waste water of the invention, first by the production waste water of generation pass through respectively every
After oil groove removes part organic solvent and organic product, it is pumped into density wastewater intermediate pool, then be pumped into multiple-effect evaporation source wastewater disposal basin, later
It is pumped into multi-effect evaporation system, the effect grade of the multi-effect evaporation system can be 2~6 effects, and density wastewater is successively through each effect evaporator
Steam heating is carried out, and maintains the balance of inflow and outflow, last evaporation water is collected into recycle-water reserve tank, when time acid
After saponification, carrying out precipitation treatment, the evaporation water that collection is added into precipitation kettle substitutes conventional use of tap water and is diluted, finally
It is acidified, be recrystallized to give time acid fine work.The production waste water that each stage of reaction generates in time acid production process press respectively with
Upper step is handled, and cannot mutually be mixed, and otherwise evaporating water constituent complexity can not apply, and be not easy into salt.
Compared with prior art, the invention has the following advantages that
Dense salt waste water through oil removal, multiple-effect evaporation, is obtained byproduct sodium chloride salt by the present invention, while evaporation water is collected separately and returns
For in time acid production system, for mother liquor again after recovered organic product, set to be used for multiple-effect evaporation.Present invention process can subtract significantly
The processing of few brine waste, mitigate the pressure of biochemical treatment, 50% or more emission reduction, and outlet is also less salt, in low COD
Water.Using present invention process, 1 ton of time acid of every production will rationally recycle evaporation 7 tons of water, 10 tons of emission reduction of waste water total amount,
And it also brings great convenience to three-protection design.It is total to apply evaporation water 14000 to produce 2000 tons of time acid calculating every year
Ton/year, recycle 4000 tons/year of byproduct sodium chloride salt, 40000 tons/year of emission reduction brine waste, save originally 14000 tons of water resource/
Year.
Detailed description of the invention
Fig. 1 is the flow diagram of present invention process.
Fig. 2 is the time acid fine work spectrogram produced using present invention process recovery to time acid.
Specific embodiment
The flow diagram of present invention process is as shown in Figure 1.By traditional addition Cyclization side of time acid commercial synthesis
Method synthesizes time acid, and after addition, cyclisation, saponification and elimination reaction, the dense salt waste water that the saponification stage is generated is passed through oil partition tank
After middle removal part organic solvent and the organic matter that easily precipitates, obtained water outlet is neutralized to after pH value is 7.5, is passed through in density wastewater
Between store in pond.Density wastewater is pumped into the level-one evaporator of multi-effect evaporation system, steam-heating system, level-one evaporator are opened
The steam of generation is passed through in secondary evaporimeter again, and the steam of secondary evaporimeter, which is passed through in recycle-water reserve tank, collects evaporation water.Respectively
Remaining NaCl salt is collected by salt recovery system in evaporator.It is cyclized object to be saponified with after carrying out precipitation treatment, lead into saponification kettle
Enter to evaporate water and be diluted, be acidified, filtering obtains time acid crude, obtains time acid fine work after finally recrystallizing.
It is to be passed through tap water in saponification kettle to be acidified in traditional time acid production process.It as a comparison, will be same
Saponification is criticized, is acidified respectively with tap water and evaporation water dilution in two batches, compares the time acid crude of output, the matter of fine work
Amount.The results are shown in Table 1 for pilot plant test.As known from Table 1, evaporation water and tap water are used in the acidizing process of time acid, output
Time acid crude and fine work quality it is suitable, evaporation water energy realize reuse.
The time that 1 pilot plant test separate sources water of table obtains sour thick, fine work quality
The time that separate sources water obtains in 2 industrial production of table sour thick, fine work quality
For the feasibility of verifying present invention process in the industrial production, sewage plant multiple-effect evaporation water is directly covered and is used to produce
It in time acid acidizing process, is used as dilution water, the quality of crude acid, essence acid that comparison tap water and evaporation aquatic products go out.From table 2
As can be seen that the enough sets completely of the evaporation water energy of present invention process are used in time acid acidification system, obtained product yield and product
Matter and originally water-reducible result are very nearly the same.
Claims (5)
1. the cycling and reutilization treatment process of time acid producing waste water, which is characterized in that specifically:
Step 1, Sewage treatment: time acid producing waste water enters density wastewater intermediate pool after oil partition tank, then is pumped into multiple-effect evaporation source
Wastewater disposal basin opens multi-effect evaporation system, is pumped into density wastewater, adjusts negative-pressure vacuum system, opens steam heating system, makes input and output material
Balance, is then turned on salt recovery system, collects side product chlorinated sodium salt, and evaporation water is individually deposited in recycle-water reserve tank, to
Time acid is produced to use；
Step 2, the evaporation water of recycling recycles: it is dilute that evaporation water is added into precipitation kettle after saponification, carrying out precipitation treatment for time acid
It releases, is acidified, filtering obtains time acid crude, time acid fine work is obtained after recrystallization.
2. cycling and reutilization treatment process according to claim 1, which is characterized in that the time acid producing waste water is
The waste water that water rinses, saponification stage or precipitation stage generate.
3. cycling and reutilization treatment process according to claim 1, which is characterized in that the time acid producing waste water warp
After oil partition tank, it is 7.5 that obtained water outlet, which is neutralized to pH, enters back into density wastewater intermediate pool.
4. cycling and reutilization treatment process according to claim 1, which is characterized in that the effect of the multi-effect evaporation system
Grade is 2~6 effects.
5. cycling and reutilization treatment process according to claim 1, which is characterized in that the effect of the multi-effect evaporation system
Grade is 3~4 effects.
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| CN201910232462.9A CN109896683A (en) | 2019-03-26 | 2019-03-26 | The cycling and reutilization treatment process of time acid producing waste water |
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| CN201910232462.9A CN109896683A (en) | 2019-03-26 | 2019-03-26 | The cycling and reutilization treatment process of time acid producing waste water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702389A (en) * | 2022-03-30 | 2022-07-05 | 江苏春江润田农化有限公司 | Purification device for extracting by-product alkyne ester from waste water of kungfu acid process |
Citations (5)
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| CN101863579A (en) * | 2010-06-18 | 2010-10-20 | 安徽华星化工股份有限公司 | Iminodiacetic acid saliferous wastewater processing technology |
| CN102633398A (en) * | 2011-02-12 | 2012-08-15 | 凯膜过滤技术(上海)有限公司 | Method for recovering organic effluent brine |
| CN106186537A (en) * | 2016-08-16 | 2016-12-07 | 南京格洛特环境工程股份有限公司 | A kind of evaporative crystallization new technology of high salt high concentrated organic wastewater |
| WO2017161640A1 (en) * | 2016-03-22 | 2017-09-28 | 中国环境科学研究院 | Method for treating and recycling organic wastewater and apparatus |
| CN109502870A (en) * | 2018-12-31 | 2019-03-22 | 天津滨港电镀企业管理有限公司 | A kind of plating garden derusting waste hydrochloric acid triple effect evaporation processing system and pretreating process |
-
2019
- 2019-03-26 CN CN201910232462.9A patent/CN109896683A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863579A (en) * | 2010-06-18 | 2010-10-20 | 安徽华星化工股份有限公司 | Iminodiacetic acid saliferous wastewater processing technology |
| CN102633398A (en) * | 2011-02-12 | 2012-08-15 | 凯膜过滤技术(上海)有限公司 | Method for recovering organic effluent brine |
| WO2017161640A1 (en) * | 2016-03-22 | 2017-09-28 | 中国环境科学研究院 | Method for treating and recycling organic wastewater and apparatus |
| CN106186537A (en) * | 2016-08-16 | 2016-12-07 | 南京格洛特环境工程股份有限公司 | A kind of evaporative crystallization new technology of high salt high concentrated organic wastewater |
| CN109502870A (en) * | 2018-12-31 | 2019-03-22 | 天津滨港电镀企业管理有限公司 | A kind of plating garden derusting waste hydrochloric acid triple effect evaporation processing system and pretreating process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702389A (en) * | 2022-03-30 | 2022-07-05 | 江苏春江润田农化有限公司 | Purification device for extracting by-product alkyne ester from waste water of kungfu acid process |
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Application publication date: 20190618 |