CN108892300A - A kind of processing method of carbendazim production utilization of wastewater resource - Google Patents
A kind of processing method of carbendazim production utilization of wastewater resource Download PDFInfo
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- CN108892300A CN108892300A CN201810697137.5A CN201810697137A CN108892300A CN 108892300 A CN108892300 A CN 108892300A CN 201810697137 A CN201810697137 A CN 201810697137A CN 108892300 A CN108892300 A CN 108892300A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
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- 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
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- 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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F2001/5218—Crystallization
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- 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
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Water Treatment By Sorption (AREA)
Abstract
The invention belongs to the processing technology fields of agricultural chemicals waste water resource utilization, and the present invention provides a kind of processing methods of carbendazim production utilization of wastewater resource.Include the following steps：A) resin adsorption；B) distillation and concentration；C) deamination is reacted；D) evaporative crystallization.The processing method of carbendazim production utilization of wastewater resource provided by the invention, compared with prior art, the present invention has the following advantages：1, process is succinct, easy to operate, mild condition, and organic matter can be effectively removed；2, the calcium chloride salt that recycling obtains reaches commercial grade, can be used as raw material of industry use；3, the desorbed solution generated in resin resolving can be recycled directly；4, the molecular structure that aniline category matter is hardly destroyed in this technique, the aniline type organic being recovered to can be re-used in production technology；5, this technique is nearly free from secondary pollution, sorbent used to be recycled for multiple times, and entire technical process does not generate additional waste water, and method safety is efficient.
Description
Technical field
The invention belongs to the processing technology fields of agricultural chemicals waste water resource utilization, and in particular to a kind of carbendazim production waste water
The processing method of resource utilization.
Background technique
Carbendazim is a kind of less toxic, efficient, wide spectrum, systemic fungicide, is widely used in killing for crops as pesticide
Bacterium is disease-resistant, entitled N- (2- the benzimidazolyl)-methyl carbamate of chemistry.Its produce waste water in containing o-phenylenediamine, methanol,
The pollutants such as cyanide, rhodanide and calcium chloride and ammonium chloride, belong to high COD（COD）It is high concentration, high ammonia nitrogen, with high salt
Point, organic wastewater difficult to degrade.The discharge of such waste water causes the serious pollution of environment and being largely lost for utility, at
For the bottleneck for limiting the production industry value chain.About this wastewater treatment method, the method taken has biodegrade
Method, chemical coagulation and biochemical treatment combination method, supercritical ultrasonics technology, photochemical degradating method and carbon biological treatment etc..
Chinese invention patent (CN102910775B) discloses a kind of preconditioning technique of carbendazim wastewater, technical solution master
It to include wet oxidation process removal characteristic contamination and o-phenylenediamine, rectifying deamination.The group technology handles carbendazim after waste water
Removal rate > 98%, o-phenylenediamine removal rate > 99%, COD removal rate > 70%, ammonia nitrogen removal frank > 96% give up after pretreatment
Aquaticization B/C value is improved to 0.4 or more, after send to biochemical treatment system processing, qualified discharge.The technique by wet oxidation and
Rectifying deamination combines, and improves wastewater biodegradability, but carbendazim wastewater high salt waste water, and biochemical system needs special resistance to
Salt bacterium, to biochemical system, more stringent requirements are proposed for this.The salt in waste water and water resource do not obtain reuse and recycling simultaneously.
Chinese invention patent (CN105152408A) discloses a kind of processing method of carbendazim production waste water, using acidity
Under the conditions of carbendazim production waste water is pre-processed with the diazo-reaction of nitrite, iron-carbon micro-electrolysis technology, it is laggard
Larger molecular organics are oxidized to small molecule, then under alkaline condition adsorb oxidation treatment liquid stripping by row wet oxidation reaction
Processing, then Fenton oxidation post-processing is carried out, recycling salt is evaporated finally by MVR, processing water outlet enters biochemical treatment or outer
Row.The invention can effectively remove nitrobenzene compounds and COD in waste water by series of oxidation reaction, but the technique system
Water resource reclamation rate of uniting is lower, and is mixed salt by the salt of MVR recycling, belongs to solid dangerous waste scope, processing cost is high.
It all joined chemical reagent in the above method, generate secondary pollution, processing waste water is at high cost, and wherein useful component returns
It is low to receive reuse ratio.
Summary of the invention
1, technical problem to be solved：
All joined chemical reagent in the processing method of existing carbendazim production waste water, generate secondary pollution, processing waste water at
This height, wherein useful component recycling and reusing rate is low.
2, technical solution：
In order to solve problem above, the present invention provides a kind of processing methods of carbendazim production utilization of wastewater resource, including
Following steps：
A) resin adsorption：Enter the pillar equipped with macroporous absorbent resin after carbendazim wastewater is filtered with the flow of 0.5 ~ 3BV/h
Adsorption treatment is carried out, macroporous absorbent resin is parsed again with the flow of 0.5 ~ 3 BV/h with the desorbing agent that volume is 1 ~ 5 BV
It is raw；
B) distillation and concentration：To step a）In resin treatment after solution carry out distillation and concentration, be enriched with calcium chloride salt cycles of concentration
It is 3 ~ 4 times, and removes part COD；
C) deamination is reacted：Toward step b）Suitable calcium oxide is added in middle gained evaporated mother liquor and carries out reaction deamination, is carried out ammonia and is returned
It receives, reaction temperature is 70 ~ 90 DEG C, and reaction vacuum degree is 0.01 ~ 0.09 MPa, and the time of reaction is 0.5 ~ 2 h, reaction
After carry out heat filtering；
D) evaporative crystallization：To step c）Filtrate obtained by middle heat filtering is evaporated concentration and recycles calcium chloride salt.
In step a）The method of middle filtering is vacuum filtration or filters pressing.
In step a）Used in macroporous absorbent resin model LXT-053, XDA-1, DA201-CIII therein one
Kind or a variety of combinations.
In step a）Used in desorbing agent be the one such or a variety of combination of methanol, ethyl alcohol, acetone.
In step d）Described in evaporation and concentration with multiple be 2 ~ 4 times processing.
3, beneficial effect：
The processing method of carbendazim provided by the invention production utilization of wastewater resource, compared with prior art, the present invention just like
Lower advantage：
1, process is succinct, easy to operate, mild condition, and organic matter can be effectively removed；
2, the calcium chloride salt that recycling obtains reaches commercial grade, can be used as raw material of industry use；
3, the desorbed solution generated in resin resolving can be recycled directly；
4, the molecular structure that aniline category matter is hardly destroyed in this technique, the aniline type organic being recovered to can be re-used for
In production technology；
5, this technique is nearly free from secondary pollution, sorbent used to be recycled for multiple times, and entire technical process does not produce
Raw additional waste water, method safety are efficient.
Detailed description of the invention
Fig. 1 is the processing method flow chart that carbendazim of the invention produces utilization of wastewater resource.
Specific embodiment
The present invention is described in detail below.
The present invention provides a kind of processing methods of carbendazim production utilization of wastewater resource, carry out resin adsorption first,
It removes the o-phenylenediamine in waste water and removes coloration：After carbendazim wastewater is filtered enter equipped with macroporous absorbent resin pillar into
Row adsorption treatment, the organic matters such as o-phenylenediamine in waste water are attracted on macroporous absorbent resin, with desorbing agent to macroporous absorption
The o-phenylenediamine of resin adsorption carries out parsing recycling, then carries out carrying out distillation and concentration processing to the filtrate after resin treatment, increase
Add concentration of the calcium chloride in filtrate and removes part COD, that is, distillation and concentration；Excessive oxidation is added into evaporated mother liquor
Calcium carries out reaction deamination, carries out recovery ammonia；Namely react deamination：Last evaporative crystallization：Filtrate after reaction is tied through evaporation
Crystalline substance processing, recycles calcium chloride salt.
From the aforegoing it can be seen that parsing recycling is carried out to o-phenylenediamine in resin adsorption step, in reaction deamination step
Ammonia is recycled, calcium chloride salt is recycled in the evaporative crystallization stage.
Embodiment 1：
Its waste water is derived from domestic carbendazim factory, and water quality situation is as follows：PH is 5.1, and ammonia nitrogen is 17000 mg/L, and CODCr is
44000 mg/L。
It takes the macroporous absorbent resin of 200 mL model LXT-053 to be fitted into glass adsorption column, carbendazim is taken to produce waste water,
First it is filtered, the method for filtering is vacuum filtration or filters pressing.By filtered waste water with the stream of 1 BV/h at 25 DEG C
For amount by glass adsorption column, processing wastewater volume is 800 mL（4 BV）, waste water is by being in colourless, Zhi Houyong after glass column outflow
1 BV methanol carries out parsing regeneration treatment with 0.5 BV/h.Through detecting, the COD of column liquid outCr = 16000 mg/L。
Distillation and concentration is carried out to column liquid out, cycles of concentration is 3.5 times, obtains evaporated mother liquor.Through detecting, evaporated mother liquor CODCr
=6000 mg/L, ammonia nitrogen=33400 mg/L.
200 mL of evaporated mother liquor is taken, 14 g calcium oxide are added, reaction temperature is 80 DEG C, and vacuum degree is 0.01 MPa, and ammonia returns
Receipts absorbing liquid is water, is filtered at 90 DEG C after reacting 0.5 h, filtrate ammonia nitrogen=2100 mg/L.
Filtrate is concentrated with MVR vapo(u)rization system in the last evaporative crystallization stage, isolated pale when cycles of concentration is 2 times
Calcium chloride salt.Through detecting, calcium chloride dihydrate purity reaches 80 %, reaches the I type quality requirements in GBT 26520-2011 standard.
Embodiment 2：
It takes the macroporous absorbent resin of 200 mL model XDA-1 to be fitted into glass adsorption column, takes carbendazim to produce waste water, first to it
It is filtered, the method for filtering is vacuum filtration or filters pressing.Filtered waste water is led to the flow of 0.5 BV/h at 25 DEG C
Glass adsorption column is crossed, processing wastewater volume is 800 mL（4 BV）, waste water flowed out by glass column after in colourless, later with 3 BV
Ethyl alcohol carries out parsing regeneration treatment with 1.5 BV/h.Through detecting, the COD of column liquid outCr = 14000 mg/L。
Distillation and concentration is carried out to column liquid out, cycles of concentration is 4 times, obtains evaporated mother liquor.Through detecting, evaporated mother liquor CODCr =
8200 mg/L, ammonia nitrogen=52800 mg/L.
100 mL of evaporated mother liquor is taken, 12 g calcium oxide are added, reaction temperature is 90 DEG C, and vacuum degree is 0.05 MPa, and ammonia returns
Receipts absorbing liquid is water, is filtered at 90 DEG C after reacting 1 h, filtrate ammonia nitrogen=1560 mg/L.
Filtrate is concentrated with MVR vapo(u)rization system, when cycles of concentration is 1.5 times, isolated pale calcium chloride salt.Through examining
It surveys, calcium chloride dihydrate purity reaches 79 %, reaches the I type quality requirements in GBT 26520-2011 standard.
Embodiment 3：
It takes the macroporous absorbent resin of 200 mL model DA201-CIII to be fitted into glass adsorption column, carbendazim is taken to produce waste water,
First it is filtered, the method for filtering is vacuum filtration or filters pressing.By filtered waste water with the stream of 3 BV/h at 25 DEG C
For amount by glass adsorption column, processing wastewater volume is 800 mL（4 BV）, waste water is by being in colourless, Zhi Houyong after glass column outflow
5 BV acetone carry out parsing regeneration treatment with 3 BV/h.Through detecting, the COD of column liquid outCr = 17000 mg/L。
Distillation and concentration is carried out to column liquid out, cycles of concentration is 3 times, obtains evaporated mother liquor.Through detecting, evaporated mother liquor CODCr =
5800 mg/L, ammonia nitrogen=35400 mg/L.
200 mL of evaporated mother liquor is taken, 15 g calcium oxide are added, reaction temperature is 70 DEG C, and vacuum degree is 0.09 MPa, and ammonia returns
Receipts absorbing liquid is water, is filtered at 90 DEG C after reacting 2 h, filtrate ammonia nitrogen=2200 mg/L.
Filtrate is concentrated with MVR vapo(u)rization system, when cycles of concentration is 2 times, isolated pale calcium chloride salt.Through detecting,
Calcium chloride dihydrate purity reaches 80 %, reaches the I type quality requirements in GBT 26520-2011 standard.
Although the present invention has been described by way of example and in terms of the preferred embodiments, they be not it is for the purpose of limiting the invention, it is any ripe
This those skilled in the art is practised, without departing from the spirit and scope of the invention, can make various changes or retouch from working as, therefore guarantor of the invention
Shield range should be subject to what claims hereof protection scope was defined.
Claims (6)
1. a kind of processing method of carbendazim production utilization of wastewater resource, includes the following steps：
Resin adsorption：After carbendazim wastewater is filtered enter equipped with macroporous absorbent resin pillar with the flow of 0.5 ~ 3 BV/h into
Row adsorption treatment is parsed again macroporous absorbent resin with the flow of 0.5 ~ 3 BV/h with the desorbing agent that volume is 1 ~ 5 BV
It is raw；
Distillation and concentration：To step a）In resin treatment after solution carry out distillation and concentration, enrichment calcium chloride salt cycles of concentration be 3
~ 4 times, and remove part COD；
React deamination：Toward step b）The calcium oxide that excessive 0 ~ 10 % is added in middle gained evaporated mother liquor carries out reaction deamination, carries out
Recovery ammonia, reaction temperature are 70 ~ 90 DEG C, and reaction vacuum degree is 0.01 ~ 0.09 MPa, and the time of reaction is 0.5 ~ 5 h, reaction
After carry out heat filtering；
Evaporative crystallization：To step c）Filtrate obtained by middle heat filtering is evaporated concentration and recycles calcium chloride salt.
2. the method as described in claim 1, it is characterised in that：In step a）The method of middle filtering is vacuum filtration or filters pressing.
3. the method as described in claim 1, it is characterised in that：In step a）Used in macroporous absorbent resin model
LXT-053, XDA-1, DA201-CIII one such or a variety of combination.
4. method according to claim 1 or 2, it is characterised in that：In step a）Used in desorbing agent be methanol, second
The one such or a variety of combination of alcohol, acetone.
5. method according to claim 1 or 2, it is characterised in that：In step c）Middle reaction process recovery ammonia absorbing liquid is salt
Acid, sulfuric acid, water are one such.
6. method according to claim 1 or 2, it is characterised in that：In step d）Described in evaporation and concentration with multiple be 1.5
~ 5 times of processing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995185A (en) * | 2020-08-20 | 2020-11-27 | 京博农化科技有限公司 | Treatment method of deep-color high-concentration and high-toxicity mixed pesticide industrial wastewater |
| CN114057343A (en) * | 2022-01-18 | 2022-02-18 | 河北鑫鹏新材料科技有限公司 | Nitrate wastewater treatment method and system |
| CN115180771A (en) * | 2022-07-22 | 2022-10-14 | 安徽东至广信农化有限公司 | Treatment method of wastewater from carbendazim production |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048019A (en) * | 1989-06-14 | 1990-12-26 | 国营江阴农药厂 | A kind of wastewater treatment is also reclaimed the method for O-Phenylene Diamine |
| CN104291523A (en) * | 2014-09-18 | 2015-01-21 | 波鹰(厦门)科技有限公司 | Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater |
| CN104803529A (en) * | 2014-12-05 | 2015-07-29 | 浙江龙盛集团股份有限公司 | Processing method of aniline intermediate production wastewater |
| CN106630413A (en) * | 2016-12-17 | 2017-05-10 | 上海问鼎环保科技有限公司 | Resource treatment method of carbendazol production wastewater |
| CN107500459A (en) * | 2017-07-25 | 2017-12-22 | 浙江奇彩环境科技股份有限公司 | A kind of technique for handling methyl sulfur bacterium panacen waste water |
| CN108083365A (en) * | 2017-12-28 | 2018-05-29 | 浙江新安化工集团股份有限公司 | A kind of processing method of carbendazim wastewater |
-
2018
- 2018-06-29 CN CN201810697137.5A patent/CN108892300A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048019A (en) * | 1989-06-14 | 1990-12-26 | 国营江阴农药厂 | A kind of wastewater treatment is also reclaimed the method for O-Phenylene Diamine |
| CN104291523A (en) * | 2014-09-18 | 2015-01-21 | 波鹰(厦门)科技有限公司 | Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater |
| CN104803529A (en) * | 2014-12-05 | 2015-07-29 | 浙江龙盛集团股份有限公司 | Processing method of aniline intermediate production wastewater |
| CN106630413A (en) * | 2016-12-17 | 2017-05-10 | 上海问鼎环保科技有限公司 | Resource treatment method of carbendazol production wastewater |
| CN107500459A (en) * | 2017-07-25 | 2017-12-22 | 浙江奇彩环境科技股份有限公司 | A kind of technique for handling methyl sulfur bacterium panacen waste water |
| CN108083365A (en) * | 2017-12-28 | 2018-05-29 | 浙江新安化工集团股份有限公司 | A kind of processing method of carbendazim wastewater |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995185A (en) * | 2020-08-20 | 2020-11-27 | 京博农化科技有限公司 | Treatment method of deep-color high-concentration and high-toxicity mixed pesticide industrial wastewater |
| CN114057343A (en) * | 2022-01-18 | 2022-02-18 | 河北鑫鹏新材料科技有限公司 | Nitrate wastewater treatment method and system |
| CN115180771A (en) * | 2022-07-22 | 2022-10-14 | 安徽东至广信农化有限公司 | Treatment method of wastewater from carbendazim production |
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Application publication date: 20181127 |