CN111116402A - Imidacloprid byproduct salt treatment method - Google Patents
Imidacloprid byproduct salt treatment method Download PDFInfo
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- CN111116402A CN111116402A CN201911176082.4A CN201911176082A CN111116402A CN 111116402 A CN111116402 A CN 111116402A CN 201911176082 A CN201911176082 A CN 201911176082A CN 111116402 A CN111116402 A CN 111116402A
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- Prior art keywords
- salt
- byproduct salt
- byproduct
- imidacloprid
- charged membrane
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- 150000003839 salts Chemical class 0.000 title claims abstract description 57
- 239000006227 byproduct Substances 0.000 title claims abstract description 46
- 239000005906 Imidacloprid Substances 0.000 title claims abstract description 19
- 229940056881 imidacloprid Drugs 0.000 title claims abstract description 19
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012267 brine Substances 0.000 claims abstract description 18
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000013505 freshwater Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000011780 sodium chloride Substances 0.000 claims abstract description 3
- 239000012266 salt solution Substances 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 4
- 238000005374 membrane filtration Methods 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- 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
- C01D3/04—Chlorides
-
- 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
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/16—Total nitrogen (tkN-N)
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/20—Total organic carbon [TOC]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a method for treating imidacloprid byproduct salt, which comprises the following steps: the method comprises the following steps: drying the byproduct salt generated in the imidacloprid production process under a vacuum condition, and condensing and collecting DMF (dimethyl formamide) in the byproduct salt; step two: adding water into the dried byproduct salt to prepare strong brine, heating, filtering, cooling, and filtering with a charged membrane; step three: the filtered saline water is prepared into the required concentration, or is dried to prepare the salt. According to the invention, DMF in the byproduct salt is recovered by adopting a vacuum drying and recondensing mode, so that the recovery rate is high, and the method is simple and rapid; adopt filter equipment to get rid of the macromolecular impurity in the byproduct salt, adopt the organic impurity that contains in the high-efficient byproduct salt of getting rid of charged membrane, concentrate the salt water simultaneously, obtain high concentration salt water and fresh water, high concentration salt water can be used to allocate the salt water of other concentrations or dry into salt for use. Before entering the charged membrane, the strong brine and the fresh water are filtered in advance, so that the risk of blockage of the charged membrane is reduced.
Description
Technical Field
The invention relates to the technical field of byproduct salt treatment, in particular to a method for treating imidacloprid byproduct salt.
Background
Imidacloprid is a nicotine ultra-high-efficiency pesticide, and has the characteristics of broad spectrum, high efficiency, low toxicity, low residue, difficult generation of resistance by pests, safety to people, livestock, plants and natural enemies and the like. In the production process of imidacloprid, a large amount of byproduct salt (byproduct salt containing more than 2 percent of DMF (N, N-dimethylformamide)) is generated, which belongs to dangerous solid waste, the treatment and resource utilization of the byproduct salt are national problems, at present, enterprises usually adopt temporary storage, store a certain amount of byproduct salt and send the byproduct salt to qualified units for harmless treatment, and if the byproduct salt is leaked slightly in the storage process, the environmental safety is greatly threatened.
Disclosure of Invention
The invention aims to provide a simple and rapid method for treating imidacloprid byproduct salt.
In order to achieve the purpose, the invention provides the following technical scheme: a method for treating imidacloprid byproduct salt comprises the following steps:
the method comprises the following steps: drying the byproduct salt generated in the imidacloprid production process under a vacuum condition, and condensing and collecting DMF (dimethyl formamide) in the byproduct salt;
step two: adding water into the dried byproduct salt to prepare strong brine, heating, filtering, cooling, and filtering with a charged membrane;
step three: the filtered saline water is prepared into the required concentration, or is dried to prepare the salt.
Preferably, in the first step, the drying is controlled to be in the environment of 83-156mmHg of vacuum degree, the drying temperature is controlled to be 19.45-35 ℃, and the drying time is controlled to be 3-7 hours.
Preferably, the charged membrane filtration is performed by a charged membrane filtration device, in the second step, after the concentrated salt water is heated to 65 +/-5 ℃, the larger molecular impurities in the byproduct salt solution are filtered by a filter membrane below 0.22um, and then cooled to below 30 ℃, the concentrated salt water enters a concentrated water chamber of the charged membrane filtration device after being filtered by a 5 mu m filter element, and the pure water enters a fresh water chamber of the charged membrane filtration device after being filtered by a 1 mu m filter element.
Preferably, the charged membrane in the second step is a negatively charged membrane.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, DMF in the byproduct salt is recovered by adopting a vacuum drying and recondensing mode, so that the recovery rate is high, and the method is simple and rapid;
2. the invention adopts a filtering device to remove macromolecular impurities in the byproduct salt, adopts a charged membrane to efficiently remove organic impurities contained in the byproduct salt, and simultaneously concentrates the brine to obtain high-concentration brine and fresh water, wherein the high-concentration brine can be used for preparing brine with other concentrations or drying into salt for later use. Before entering the charged membrane, the strong brine and the fresh water are filtered in advance, so that the risk of blockage of the charged membrane is reduced.
3. After the method is adopted, DMF and finished salt can be obtained by treating the imidacloprid byproduct salt, certain economic benefit is generated, and the situation that money is needed to be spent in treating the imidacloprid byproduct salt by an applicant in the past is changed.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples 1 to 3 provided by the present invention: a method for treating imidacloprid byproduct salt comprises the following steps:
the method comprises the following steps: drying by-product salt generated in the imidacloprid production process under a vacuum condition, condensing and collecting DMF in the by-product salt, controlling the drying temperature to be 19.45-35 ℃ and the drying time to be 3-7 hours under the vacuum degree of 83-156 mmHg;
step two: adding water into the dried byproduct salt to prepare concentrated brine with the concentration of 10g/L, heating to 65 +/-5 ℃, filtering out larger molecular impurities in the byproduct salt solution by using a filter membrane below 0.22um, cooling to below 30 ℃, filtering by using a filter element of 5 mu m, feeding into a concentrated water chamber of a charged membrane filtering device, and filtering pure water by using a filter element of 1 mu m, and feeding into a fresh water chamber of the charged membrane filtering device.
Step three: blending the filtered strong brine into required concentration; or evaporating at normal pressure, evaporating at-90 kPa, filtering at 70 deg.C to obtain solid salt, and filtering to obtain solid salt solution of 26%. And analyzing the TOC, total nitrogen and ammonia nitrogen contents in the brine.
Before the treatment, the characteristic factors of the by-produced salts are shown in Table 1
TABLE 1 characteristic factors of by-product salts
The parameters for drying and debugging in the first step are shown in table 2:
TABLE 2 drying and adjusting parameters of byproduct salt
The characteristic factors of the dried byproduct salt are shown in Table 3:
TABLE 3 characterization factor of dried by-product salt
As can be seen, after the drying step, the DMF content in the byproduct salt is greatly reduced, and the TOC and the total nitrogen index are greatly reduced.
The parameters of the charged membrane in the second step are shown in Table 4
TABLE 4 charged Membrane tuning parameters
The characteristic factors of the fresh water discharged from the charged membrane device are shown in table 5.
TABLE 5 characteristic factors of fresh water discharged from charged membrane device
| TOC/ppm | Total nitrogen/ppm | |
| Example 1 | 2070 | 1620 |
| Example 2 | 1617 | 1600 |
| Example 3 | 1396 | 1340 |
The characteristic factors of the concentrated brine discharged from the charged membrane device are shown in Table 6.
TABLE 6 characteristic factors of the concentrated brine discharged from the charged membrane device
| TOC/ppm | Total nitrogen/ppm | |
| Example 1 | 330 | 210 |
| Example 2 | 318 | 220 |
| Example 3 | 377 | 280 |
The characteristic factors of the 26% saline solution reconstituted by treatment with a charged membrane and then evaporation are shown in Table 7.
TABLE 7 characterization factors for the treatment with charged membrane followed by evaporation of reconstituted 26% saline solution
| TOC/ppm | Total nitrogen/ppm | |
| Example 1 | 16 | 10 |
| Example 2 | 25 | 14 |
| Example 3 | 27.5 | 26 |
As can be seen from tables 5-7, the total nitrogen and TOC contents of the membrane-filtered strong brine and fresh water, as well as the reconstituted 26% brine, were greatly reduced to achieve the desired targets.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (4)
1. A method for treating imidacloprid byproduct salt comprises the following steps:
the method comprises the following steps: drying the byproduct salt generated in the imidacloprid production process under a vacuum condition, and condensing and collecting DMF (dimethyl formamide) in the byproduct salt;
step two: adding water into the dried byproduct salt to prepare strong brine, heating, filtering, cooling, and filtering with a charged membrane;
step three: the filtered saline water is prepared into the required concentration, or is dried to prepare the salt.
2. The method for treating imidacloprid byproduct salt according to claim 1, which is characterized in that: in the first step, the drying is controlled to be in a vacuum degree of 83-156mmHg, the drying temperature is controlled to be 15-35 ℃, and the drying time is controlled to be 3-7 hours.
3. The method for treating imidacloprid byproduct salt according to claim 1, which is characterized in that: and in the second step, the concentrated brine is heated to 60-70 ℃, then the filtering membrane with the diameter of below 0.22 mu m is adopted to filter out the larger molecular impurities in the byproduct salt solution, and then the concentrated brine is cooled to below 30 ℃, enters a concentrated water chamber of the charged membrane filtering device after being filtered by a filter element with the diameter of 5 mu m, and enters a fresh water chamber of the charged membrane filtering device after being filtered by a filter element with the diameter of 1 mu m.
4. The method for treating imidacloprid byproduct salt according to claim 3, characterized in that: and in the second step, the charged membrane is a negatively charged membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911176082.4A CN111116402A (en) | 2019-11-26 | 2019-11-26 | Imidacloprid byproduct salt treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911176082.4A CN111116402A (en) | 2019-11-26 | 2019-11-26 | Imidacloprid byproduct salt treatment method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111116402A true CN111116402A (en) | 2020-05-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911176082.4A Pending CN111116402A (en) | 2019-11-26 | 2019-11-26 | Imidacloprid byproduct salt treatment method |
Country Status (1)
| Country | Link |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239744A (en) * | 2007-02-09 | 2008-08-13 | 江都市华伦化机环保设备厂 | Dye pesticide wastewater treatment device |
| CN101302072A (en) * | 2008-06-27 | 2008-11-12 | 东南大学 | Dye pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery process and apparatus |
| CN108996838A (en) * | 2018-08-22 | 2018-12-14 | 沈阳化工研究院设计工程有限公司 | A kind of deep treatment method of dimethylformamide organic wastewater |
-
2019
- 2019-11-26 CN CN201911176082.4A patent/CN111116402A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239744A (en) * | 2007-02-09 | 2008-08-13 | 江都市华伦化机环保设备厂 | Dye pesticide wastewater treatment device |
| CN101302072A (en) * | 2008-06-27 | 2008-11-12 | 东南大学 | Dye pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery process and apparatus |
| CN108996838A (en) * | 2018-08-22 | 2018-12-14 | 沈阳化工研究院设计工程有限公司 | A kind of deep treatment method of dimethylformamide organic wastewater |
Non-Patent Citations (5)
| Title |
|---|
| 乔延江等: "《中药制剂学》", 30 April 2017, 中国协和医科大学出版社 * |
| 杨志刚等: "纳滤在高盐化工废水中的应用及研究进展", 《广东化工》 * |
| 杨青等: "基于BP神经网络的吡虫啉农药废水纳滤分离模型", 《安全与环境工程》 * |
| 杨青等: "纳滤膜在治理农药废水污染中的应用研究", 《工业水处理》 * |
| 杨青等: "纳滤预处理吡虫啉农药废水的试验", 《沈阳建筑大学学报(自然科学版)》 * |
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