CN105817149B - A kind of preparation method of the lontrel permeable membrane of concentrate 3,6 - Google Patents
A kind of preparation method of the lontrel permeable membrane of concentrate 3,6 Download PDFInfo
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- CN105817149B CN105817149B CN201610358154.7A CN201610358154A CN105817149B CN 105817149 B CN105817149 B CN 105817149B CN 201610358154 A CN201610358154 A CN 201610358154A CN 105817149 B CN105817149 B CN 105817149B
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- lontrel
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- permeable membrane
- cleaned
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- 239000012528 membrane Substances 0.000 title claims abstract description 19
- 239000012141 concentrate Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- HUBANNPOLNYSAD-UHFFFAOYSA-N clopyralid Chemical compound OC(=O)C1=NC(Cl)=CC=C1Cl HUBANNPOLNYSAD-UHFFFAOYSA-N 0.000 title abstract description 7
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005349 anion exchange Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical class C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 5
- 229920000578 graft copolymer Polymers 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- FDTUVFSBEYKVAP-UHFFFAOYSA-N formic acid;pyridine Chemical compound OC=O.C1=CC=NC=C1 FDTUVFSBEYKVAP-UHFFFAOYSA-N 0.000 claims 1
- CFCMNKJCKDXHHO-UHFFFAOYSA-N 2-ethenylterephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C=C)=C1 CFCMNKJCKDXHHO-UHFFFAOYSA-N 0.000 abstract description 3
- -1 methylimidazole hexafluorophosphate Chemical compound 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000005500 Clopyralid Substances 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- MAKFMOSBBNKPMS-UHFFFAOYSA-N 2,3-dichloropyridine Chemical compound ClC1=CC=CN=C1Cl MAKFMOSBBNKPMS-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 125000003963 dichloro group Chemical group Cl* 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000003204 osmotic effect Effects 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- HQWDILUMZXPFNW-UHFFFAOYSA-N 2-cyano-2-nitroacetamide Chemical compound NC(=O)C(C#N)[N+]([O-])=O HQWDILUMZXPFNW-UHFFFAOYSA-N 0.000 description 1
- RINGWLLNBNVTMO-UHFFFAOYSA-N 3,6-dichloropyridine Chemical compound ClC1=C[C]=C(Cl)N=C1 RINGWLLNBNVTMO-UHFFFAOYSA-N 0.000 description 1
- DIIMYURFOKYFTB-UHFFFAOYSA-N C(=O)O.ClC1=NC=CC=C1 Chemical compound C(=O)O.ClC1=NC=CC=C1 DIIMYURFOKYFTB-UHFFFAOYSA-N 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/78—Graft polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
- C07D213/803—Processes of preparation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
Denomination of invention：A kind of preparation method summary of the lontrel permeable membrane of concentrate 3,6：The present invention relates to a kind of concentrate 3, the preparation method of 6 lontrel permeable membranes, homogeneous-phase anion exchange film is immersed into 4 stibazoles, the methylimidazole hexafluorophosphate of 1 pi-allyl 3, in vinyl terephthalic acid (TPA) mixed solution, irradiated graft modification is made.
Description
Technical field
The present invention relates to a kind of preparation method of film, especially a kind of concentrate 3, the preparation of 6- lontrel permeable membranes
Method.
Background technology
The dichloropyridine acid solution post-processing approach obtained at present to electrochemical reducing is that acid adding makes dichloro in the solution
Pyridine acid crystal separates out, then the method separation and Extraction clopyralid and sodium chloride salt by filtering, being evaporated in vacuo.Vacuum is steamed
The shortcomings that hair is that energy expenditure is high, operating cost is higher.So people need to seek it is a kind of efficient and economical environmentally friendly new
Isolation technics, by probing into for a long time, diffusive dialysis method membrane separation technique turns into researchers' focus of attention.
CN102351788A is related to a kind of method of Hydrolysis kinetics clopyralid, using film concentrating and separating technology to electricity consumption
Dichloropyridine acid solution made from chemical synthesis carries out concentration, is pre-processed by micro-filtration and ultrafiltration, then using multistage
Embrane method concentration technology purifies to obtain clopyralid fine work.The clopyralid that the present invention obtains has purity high, quality better
Feature, up to more than 97%, the present invention can lower energy consumption, reduce waste water and give up HPLC contents by being undergone technological transformation to traditional handicraft
The discharge of gas, treated waste water can direct reuse or qualified discharge, to environmental protection advantageously, while improve dichloro
The yield of pyridine acid.
The A of CN 104447529 are related to the method for extraction and purification of 3,6- lontrel.The invention solves technology ask
Topic is that the yield of existing method is low, complex operation, and cost is high, is not suitable for industrialized production.The present invention solves above-mentioned technical problem
Scheme be by the difference of 3,6- lontrel and impurities exhibit under different temperatures and pH value condition, product is entered
Row isolates and purifies.The present invention is easy to operate, and device is simple, it is not necessary to increase other expensive separation agents and material, cost is low,
It is adapted to industrialized production.
3,6- lontrel concentrate technology of the prior art can only be concentrated to 97%（wt%）Left and right, still there is 2% or so
Impurity can not again enter remove.
The content of the invention
Present invention aims at solve above-mentioned technical problem present in prior art, there is provided a kind of concentrate 3,6- dichloros
The preparation method of pyridine carboxylic acid permeable membrane.It is characterized in that preparation process includes：
By weight, by 100 parts of homogeneous-phase anion exchange films, surface is cleaned with 5-10 part methanol, is dried, dry film leaching is buried
In 1000-2000 part 4- stibazoles, 0.1-0.5 part 1- pi-allyl -3- methylimidazole hexafluorophosphates, 1-5 part ethene
In base terephthalic acid (TPA) mixed solution, N2Protection, is 10-50kGy or so, exposure time 10- with 60Co gamma-rays exposure doses
60 minutes, graft copolymer membrane is taken out, the surface of film is cleaned with 1000-2000 part tetrahydrofurans, dried, that is, obtain can be used for 3,6- bis-
The permeable membrane of chloropyridine formic acid concentrate.
Described homogeneous-phase anion exchange film is commercially available prod, as Langfang City Ya De generation environmental protection equipment Co., Ltd produces
Product；Described vinyl terephthalic acid (TPA) is commercially available prod, the product produced such as Zhengzhou Alpha Chemical Co., Ltd.；Institute
1- pi-allyl -3- methylimidazoles the hexafluorophosphates stated are commercially available prod, such as Chinese Academy of Sciences's Lanzhou Chemical Physics Research Institute
Product.
Described 4- stibazoles, methanol, tetrahydrofuran are commercially available prod.
The present invention is by adopting the above-described technical solution, have the advantages that：
Homogeneous-phase anion exchange film passes through 4- stibazoles, 1- pi-allyl -3- methylimidazole hexafluorophosphates, ethene
The graft modification of base terephthalic acid (TPA), the permeance property of 3,6- lontrel is improved, 3,6- dichloropyridine first
Acid concentration can obtain the 3,6- lontrel of mass percent concentration 99%.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
In 2000L reactors, by 100Kg homogeneous-phase anion exchange films, surface is cleaned with 8Kg methanol, is dried, dry film leaching
1500Kg4- stibazoles are embedded in, 0.3Kg1- pi-allyl -3- methylimidazole hexafluorophosphates, 3Kg vinyl is to benzene two
In formic acid mixed solution, N2Protection, it is 30kGy or so with 60Co gamma-rays exposure doses, exposure time 40 minutes, by graft copolymer membrane
Take out, the surface of film is cleaned with 1500Kg tetrahydrofurans, dry, that is, obtain oozing available for 3,6- lontrel concentrates
Permeable membrane.Production code member B-1.
Embodiment 2
In 2000L reactors, by 100Kg homogeneous-phase anion exchange films, surface is cleaned with 5Kg methanol, is dried, dry film leaching
1000Kg4- stibazoles are embedded in, 0.1Kg1- pi-allyl -3- methylimidazole hexafluorophosphates, 1Kg vinyl is to benzene two
In formic acid mixed solution, N2Protection, it is 10kGy or so with 60Co gamma-rays exposure doses, exposure time 10 minutes, by graft copolymer membrane
Take out, the surface of film is cleaned with 1000Kg tetrahydrofurans, dry, that is, obtain oozing available for 3,6- lontrel concentrates
Permeable membrane.Production code member B-2.
Embodiment 3
In 3000L reactors, by 100Kg homogeneous-phase anion exchange films, surface is cleaned with 10Kg methanol, is dried, dry film
Leaching is embedded in 2000Kg4- stibazoles, and 0.5Kg1- pi-allyl -3- methylimidazole hexafluorophosphates, 5Kg vinyl is to benzene
In dioctyl phthalate mixed solution, N2Protection, is 50kGy or so with 60Co gamma-rays exposure doses, exposure time 60 minutes, will be grafted
Film is taken out, and the surface of film is cleaned with 2000Kg tetrahydrofurans, is dried, that is, is obtained available for 3,6- lontrel concentrates
Permeable membrane.Production code member B-3.
The triallyl fulminuric acid of comparative example 1 is added without, the other the same as in Example 1, production code member B-4.
1- pi-allyl -3- methylimidazole the hexafluorophosphates of comparative example 2 are added without, the other the same as in Example 1, production code member B-
5。
Comparative example 3
Vinyl terephthalic acid (TPA) is added without, the other the same as in Example 1, production code member B-6.
Comparative example 4
Using untreated 100Kg homogeneous-phase anion exchange films as permeable membrane, production code member B-7.
Embodiment 4
The 3,6- lontrel that mass percent concentration is 90 is put into the solvent with temperature control and electromagnetic agitation
For 2L stainless steel osmotic cell, the m1. embodiments 1-3 of material liquid about 400 and permeable membrane made from comparative example 1-4 totally 3 layers
It is uniform in osmotic cell, it is placed in after fully being soaked in feed liquid in pond, pressure is maintained at 30Pa on the downside of outermost tunic, through thing liquid
Nitrogen condensation is collected.Material liquid is analyzed using acid-base titration and the composition of permeate, 3, the 6- lontrel after concentration are dense
Degree see the table below：
It see the table below：
| Production code member | 3,6- lontrel concentration wt% |
| B-1 | 99 |
| B-2 | 99 |
| B-3 | 99 |
| B-4 | 97 |
| B-5 | 96 |
| B-6 | 97 |
| B-7 | 93 |
The specific embodiment of the present invention is these are only, but the technical characteristic of the present invention is not limited thereto.It is any with this hair
Based on bright, to solve essentially identical technical problem, essentially identical technique effect is realized, made simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (1)
1. a kind of concentrate 3, the preparation method of 6- lontrel permeable membranes, it is characterised in that comprise the following steps：
By weight, by 100 parts of homogeneous-phase anion exchange films, surface is cleaned with 5-10 part methanol, is dried, dry film leaching is embedded in
1000-2000 part 4- stibazoles, 0.1-0.5 part 1- pi-allyl -3- methylimidazole hexafluorophosphates, 1-5 part vinyl
In terephthalic acid (TPA) mixed solution, N2Protection, is 10-50kGy with 60Co gamma-rays exposure doses, and exposure time 10-60 divides
Clock, graft copolymer membrane is taken out, the surface of film is cleaned with 1000-2000 part tetrahydrofurans, dried, that is, obtain can be used for 3,6- dichloro pyrroles
The permeable membrane of pyridine formic acid concentrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610358154.7A CN105817149B (en) | 2016-05-26 | 2016-05-26 | A kind of preparation method of the lontrel permeable membrane of concentrate 3,6 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610358154.7A CN105817149B (en) | 2016-05-26 | 2016-05-26 | A kind of preparation method of the lontrel permeable membrane of concentrate 3,6 |
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| Publication Number | Publication Date |
|---|---|
| CN105817149A CN105817149A (en) | 2016-08-03 |
| CN105817149B true CN105817149B (en) | 2018-03-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113912533B (en) * | 2021-11-23 | 2023-06-20 | 西安凯立新材料股份有限公司 | Method for preparing 3, 6-dichloropicolinic acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4334074A (en) * | 1981-02-02 | 1982-06-08 | The Dow Chemical Company | Method of recovering 3,6-dichloropicolinic acid from basic aqueous solutions of salts thereof |
| CN102351788A (en) * | 2011-08-11 | 2012-02-15 | 横店集团东阳英洛华绿色电化学有限公司 | Method for extracting and refining clopyralid |
| CN104447529A (en) * | 2014-11-25 | 2015-03-25 | 利尔化学股份有限公司 | Method for extracting and purifying 3,6-matrigon |
| CN104815568A (en) * | 2015-04-20 | 2015-08-05 | 中国海洋大学 | Preparation method of anion exchange membrane with monovalent selective separation function |
-
2016
- 2016-05-26 CN CN201610358154.7A patent/CN105817149B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4334074A (en) * | 1981-02-02 | 1982-06-08 | The Dow Chemical Company | Method of recovering 3,6-dichloropicolinic acid from basic aqueous solutions of salts thereof |
| CN102351788A (en) * | 2011-08-11 | 2012-02-15 | 横店集团东阳英洛华绿色电化学有限公司 | Method for extracting and refining clopyralid |
| CN104447529A (en) * | 2014-11-25 | 2015-03-25 | 利尔化学股份有限公司 | Method for extracting and purifying 3,6-matrigon |
| CN104815568A (en) * | 2015-04-20 | 2015-08-05 | 中国海洋大学 | Preparation method of anion exchange membrane with monovalent selective separation function |
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| Publication number | Publication date |
|---|---|
| CN105817149A (en) | 2016-08-03 |
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