CN106279269A - A kind of method preparing glufosinate-ammonium potassium salt - Google Patents
A kind of method preparing glufosinate-ammonium potassium salt Download PDFInfo
- Publication number
- CN106279269A CN106279269A CN201610621138.2A CN201610621138A CN106279269A CN 106279269 A CN106279269 A CN 106279269A CN 201610621138 A CN201610621138 A CN 201610621138A CN 106279269 A CN106279269 A CN 106279269A
- Authority
- CN
- China
- Prior art keywords
- glufosinate
- ammonium
- potassium salt
- potassium
- drying
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/30—Phosphinic acids R2P(=O)(OH); Thiophosphinic acids, i.e. R2P(=X)(XH) (X = S, Se)
- C07F9/301—Acyclic saturated acids which can have further substituents on alkyl
Abstract
The invention provides the preparation method of a kind of glufosinate-ammonium potassium salt, including: the aqueous solution of potassium hydroxide or potassium carbonate is slowly added to glufosinate-ammonium or glufosinate-ammonium hydrochlorate, stirring reaction 0 12h at 0 90 DEG C, reaction terminates that rear reactant liquor is purified, be concentrated to give content and is the glufosinate-ammonium potassium salt soln of 30%～70%, glufosinate-ammonium potassium salt soln is dried to obtain glufosinate-ammonium potassium salt crude product, this crude product is carried out vacuum drying and obtains glufosinate-ammonium potassium salt solid.Preparation glufosinate-ammonium potassium salt method environmental protection, technique that the present invention provides are simple, it is adaptable to industrialized production, tool is of great significance.
Description
Technical field
The present invention relates to the synthetic method of a kind of glufosinate-ammonium potassium salt, belong to organic chemical synthesis field.
Background technology
Glufosinate-ammonium, the logical glufosinate-ammonium ammonium salt (glufosinate-ammonium being mentioned below is all referring to glufosinate-ammonium ammonium salt) that refers to, genus broad-spectrum touch-out type
Herbicide, systemic action is strong, and kill root from glyphosate different, and glufosinate-ammonium first kills leaf, can be plant by plant transpiration effect
Xylem conducts, between its quick-acting between N,N'-dimethyl-.gamma..gamma.'-dipyridylium and glyphosate.Glufosinate-ammonium has efficiently, low toxicity, low-residual, safety
Feature, more and more higher recently as glyphosate resistance, glufosinate-ammonium is the most increasingly paid attention to.
At present, the product main component of commercial type is glufosinate-ammonium, and the goods relating to glufosinate-ammonium potassium salt are the fewest, close equally
Also little in the patent of glufosinate-ammonium potassium salt preparation method, this is because be that glufosinate-ammonium potassium salt easily absorbs water, its molten in water
Xie Du is far longer than glufosinate-ammonium ammonium salt (glufosinate-ammonium dissolubility in water is 1370g/L) more than 2000g/L, so phosphine oxamate potassium
Salt is exposed in air and the moisture absorption will soon become starchiness, and this has higher requirement, if adopting also to the preparation of glufosinate-ammonium
Prepare glufosinate-ammonium potassium salt by existing preparation method, then necessarily require to operate under anhydrous and dry environment, and existing
Synthetic method step various, process is complicated, and therefore during preparation glufosinate-ammonium potassium salt, loss is inevitable big, the receipts of final product
Rate also can reduce accordingly.By contrast, glufosinate-ammonium potassium salt reacts in aqueous phase, is a kind of ideal method, not only yield
Height, and green non-pollution, but its difficult point is that glufosinate-ammonium easily produces side reaction in aqueous phase, is unfavorable for target product grass
The generation of ammonium phosphine potassium salt, needs reaction condition is optimized design；Same because the dissolubility of glufosinate-ammonium potassium salt is very big, use
The conventional lock out operation such as alcohol analyses, saltout obtain the poor effect of glufosinate-ammonium potassium salt solid.
For problem above, it is provided that a kind of reaction in aqueous phase, technique is simple, it is adaptable to industrialized production, environmental protection
The preparation method of glufosinate-ammonium potassium salt have great importance.
Summary of the invention
In view of this, the invention provides a kind of glufosinate-ammonium potassium salt preparation method being applicable to industrialized great production, the party
Method comprises the following steps:
The aqueous solution of potassium hydroxide or potassium carbonate is slowly added to glufosinate-ammonium or glufosinate-ammonium hydrochlorate, at 0-90 DEG C
Lower stirring reaction 0-12h, the glufosinate-ammonium potassium salt that reaction terminates that rear reactant liquor is purified, be concentrated to give content and be 30%～70% is molten
Liquid, is dried to obtain glufosinate-ammonium potassium salt crude product by glufosinate-ammonium potassium salt soln, this crude product is carried out vacuum drying and obtains glufosinate-ammonium potassium salt
Solid.
The mol ratio of described glufosinate-ammonium or glyphosate salt hydrochlorate and potassium hydroxide or potassium carbonate is 1: (0.1-5).
Preferably, glufosinate-ammonium and potassium hydroxide mol ratio are 1: (1-1.2), glufosinate-ammonium and potassium carbonate mol ratio 1:
(0.5～0.6)；Glufosinate-ammonium hydrochlorate and potassium hydroxide mol ratio 1: (2～2.4), glufosinate-ammonium and potassium carbonate mol ratio 1: (1
～1.2).
Preferably, reaction temperature is 60～80 DEG C.
Preferably, the response time is 1～3h.
Particularly, reactant liquor after the completion of reaction, need to be purified by the present invention, and way of purification can be conventional mistake
Filter, also can further include film and processes, and being processed by film will be the complete potassium hydroxide of unreacted or potassium carbonate removing in reactant liquor,
The by-product that reaction produces can also be removed simultaneously.
Particularly, reactant liquor after purification needs to carry out heating and concentrates, the concentration of the glufosinate-ammonium potassium salt soln finally given
Should control at 30%-70%.Reason is, the relatively low glufosinate-ammonium potassium salt soln of concentration need during follow-up being dried time
Between longer, long high temperature drying can cause Disassembling Products, affects the purity of product, equally, the glufosinate-ammonium potassium that concentration is higher
Saline solution mobility is poor, does not the most utilize follow-up being dried.
The drying means of heretofore described glyphosate potassium saline solution is for being spray-dried or thin film evaporation.Wherein spray dried
Dry include air current spray nozzle formula atomization drying, pressure nozzle atomization drying, rotation type atomization be dried in one, preferably pressure
Formula nozzle atomization is dried, and it is advantageous that the atomization of drive nozzle formula can produce little grainy material, reduces fine powder and fly upward, improves dry
The powder response rate, and nozzle is simple to manufacture, easy to process.
Particularly, the temperature of spray drying of the present invention is 100-250 DEG C, and described spray drying temperature is preferably
130-170℃.The temperature being spray-dried need to control within the specific limits, and temperature is the lowest, and the speed being dried is relatively slow, and the time is long, effect
The poorest；Temperature is the highest, can cause Disassembling Products, affect product quality.Equally, the time of spray drying also should be in suitable scope
In, Drying Time of Vertical Spray Dryer of the present invention is 1～15s, preferably 5-15s.
Process of vacuum drying of the present invention for set vacuum drying temperature, with vacuum pump suction-0.06～-
0.1MPa, evacuation always in drying course, promote the moisture baked out in glufosinate-ammonium potassium salt crude product can discharge rapidly, not at baking oven
Inside accumulating, humidity is excessive and causes glufosinate-ammonium potassium salt water absorbent surface caking, dissolve.
Described vacuum drying temperature is 20-150 DEG C, and described vacuum drying temperature is preferably 80-90 DEG C.The present invention is true
Empty baking temperature need to control within the specific limits, and the crude product of glufosinate-ammonium potassium salt is dried to the most aqueous by vacuum drying by the present invention
Glufosinate-ammonium potassium salt solid, therefore, be dried time relatively long, if be dried temperature on the low side; be dried insufficient, if be dried
Temperature drift, long high temperature drying can arrive and cause Disassembling Products, finally affect product quality.
The beneficial effects of the present invention is:
1, total overall reaction technique of the present invention all completes in aqueous phase, and product yield is high, synthesizes low cost.
2, production process of the present invention does not use organic solvent, environmentally friendly.
3, the present invention is without solid waste, the useless generation of liquid, and be spray-dried or produce during thin film evaporation is also steam, can
Substantially produce without the three wastes to say, be greatly saved environmental protection cost.
4, present invention process flow process is simple, omnidistance without High Temperature High Pressure, low for equipment requirements, and small investment is easy to operate, it is simple to
Industrialized great production.
5, product of the present invention is to health fanout free region, environmentally safe.
Detailed description of the invention
Below by embodiment, present aspect done concrete description, it is necessary to it is pointed out here that be that following example are served only for
The present invention is further described, it is impossible to be interpreted as limiting the scope of the invention, the person skilled in the art in this field
Nonessential improvement and adjustment can be made according to the present invention.
Embodiment 1
First weigh 90% potassium hydroxide 35g, water 400g, then by soluble in water for potassium hydroxide standby；Weigh 97% grass ammonium
Phosphonic acids 100g adds in 500ml four-hole boiling flask, then the potassium hydroxide solution prepared slowly is poured stirring in four-hole boiling flask anti-into
Should, it is warmed up to 70 DEG C of insulation reaction 1h, is filtered to remove the insoluble solid impurities brought in raw material.Filtrate first carries out reducing pressure dense
Contracting, steams moisture 241g, and now in concentrated solution, glufosinate-ammonium potassium salts content is 40%, and concentrated solution uses the mode being spray-dried to carry out
Processed, spray drying temperature is set as 150 DEG C, is spray-dried time of staying 5s；The spray-dried glufosinate-ammonium potassium obtained
Possibly together with more moisture in salt crude product, this crude product is put in vacuum drying oven and dries further, set vacuum drying temperature
90 DEG C, by vacuum pump suction-0.08～-0.1MPa, evacuation always in drying course, promote in glufosinate-ammonium potassium salt crude product
The moisture baked out can be discharged rapidly, does not accumulates in baking oven, and obtaining content after drying 4h is 94% glufosinate-ammonium potassium salt product.
Embodiment 2
First weigh 90% potassium hydroxide 35g, water 400g, then by soluble in water for potassium hydroxide standby；Weigh 97% grass ammonium
Phosphonic acids 100g adds in 500ml four-hole boiling flask, then the potassium hydroxide solution prepared slowly is poured stirring in four-hole boiling flask anti-into
Should, it is warmed up to 70 DEG C of insulation reaction 1h, is filtered to remove the insoluble solid impurities brought in raw material.Filtrate first carries out reducing pressure dense
Contracting, steams moisture 300g, and now in concentrated solution, glufosinate-ammonium potassium salts content is 50%, and concentrated solution uses the mode of thin film evaporation to carry out
Processed, possibly together with more moisture in the glufosinate-ammonium potassium salt crude product obtained, puts into vacuum by this crude product after thin film evaporation
Drying baker is dried further, sets vacuum drying temperature 90 DEG C, by vacuum pump suction-0.08～-0.1MPa, dried
Evacuation always in journey, promotes the moisture baked out in glufosinate-ammonium potassium salt crude product to discharge rapidly, does not accumulates in baking oven, dries 4h
After to obtain content be 94% glufosinate-ammonium potassium salt product.
Embodiment 3
First weigh 90% potassium hydroxide 57g, water 400g, then by soluble in water for potassium hydroxide standby；Weigh 95% grass ammonium
Phosphonium salt hydrochlorate 100g adds in 500ml four-hole boiling flask, is then slowly poured in four-hole boiling flask by the potassium hydroxide solution prepared and stirs
Mix reaction, be warmed up to 70 DEG C of insulation reaction 1h, be filtered to remove the insoluble solid impurities brought in raw material.Filtrate is processed by film
Device, separates potassium chloride with glufosinate-ammonium potassium salt soln, removes the glufosinate-ammonium potassium salt soln after potassium chloride and first carries out concentrating under reduced pressure,
Removing portion of water makes glufosinate-ammonium potassium salts content in concentrated solution be about 50%, and concentrated solution uses the mode of spray drying to take off again
Water processes, and spray drying temperature is set as 150 DEG C, is spray-dried time of staying 5s；The spray-dried glufosinate-ammonium potassium salt obtained
Possibly together with more moisture in crude product, this crude product is put in vacuum drying oven and dries further, set vacuum drying temperature 90
DEG C, by vacuum pump suction-0.08～-0.1MPa, evacuation always in drying course, promote glufosinate-ammonium potassium salt crude product dries
The moisture gone out can be discharged rapidly, does not accumulates in baking oven, and obtaining content after drying 4h is 92% glufosinate-ammonium potassium salt product.
Embodiment 4
First weigh 90% potassium hydroxide 57g, water 400g, then by soluble in water for potassium hydroxide standby；Weigh 95% grass ammonium
Phosphonium salt hydrochlorate 100g adds in 500ml four-hole boiling flask, is then slowly poured in four-hole boiling flask by the potassium hydroxide solution prepared and stirs
Mix reaction, be warmed up to 70 DEG C of insulation reaction 1h, be filtered to remove the insoluble solid impurities brought in raw material.Filtrate is processed by film
Device, separates potassium chloride with glufosinate-ammonium potassium salt soln, removes the glufosinate-ammonium potassium salt soln after potassium chloride and first carries out concentrating under reduced pressure,
Removing portion of water makes glufosinate-ammonium potassium salts content in concentrated solution be about 70%, and concentrated solution uses the mode of thin film evaporation to take off again
Water processes, and possibly together with more moisture in the glufosinate-ammonium potassium salt crude product obtained, this crude product is put into vacuum and does after thin film evaporation
Dry case is dried further, sets vacuum drying temperature 90 DEG C, with vacuum pump suction-0.08～-0.1MPa, drying course
In evacuation always, promote the moisture baked out in glufosinate-ammonium potassium salt crude product to discharge rapidly, do not accumulate in baking oven, after drying 4h
Obtaining content is 92% glufosinate-ammonium potassium salt product.
Comparative example 5
First weigh 96% potassium carbonate 46g, water 400g, then by soluble in water for potassium carbonate standby；Weigh 97% glufosinate-ammonium
100g adds in 500ml four-hole boiling flask, then the solution of potassium carbonate prepared slowly is poured into stirring reaction in four-hole boiling flask, heats up
To 80 DEG C of insulation reaction 1h, it is filtered to remove the insoluble solid impurities brought in raw material.Filtrate first carries out concentrating under reduced pressure, steams water
Dividing 226g, now in concentrated solution, glufosinate-ammonium potassium salts content is 40%, and concentrated solution uses the mode being spray-dried to carry out processed,
Spray drying temperature is set as 150 DEG C, is spray-dried time of staying 5s；In the spray-dried glufosinate-ammonium potassium salt crude product obtained also
Containing more moisture, this crude product is put in vacuum drying oven and dries further, set vacuum drying temperature 90 DEG C, use vacuum
Pumping vacuum-0.08～-0.1MPa, evacuation always in drying course, promote the moisture baked out in glufosinate-ammonium potassium salt crude product
Can discharge rapidly, not accumulate in baking oven, obtaining content after drying 4h is 96% glufosinate-ammonium potassium salt product.
Comparative example 6
First weigh 96% potassium carbonate 43g, water 400g, then by soluble in water for potassium carbonate standby；Weigh 97% glufosinate-ammonium
100g adds in 500ml four-hole boiling flask, then the solution of potassium carbonate prepared slowly is poured into stirring reaction in four-hole boiling flask, heats up
To 80 DEG C of insulation reaction 1h, it is filtered to remove the insoluble solid impurities brought in raw material.Filtrate first carries out concentrating under reduced pressure, steams water
Dividing 286, now in concentrated solution, glufosinate-ammonium potassium salts content is 50%, and concentrated solution uses the mode of thin film evaporation to carry out processed,
Possibly together with more moisture in the glufosinate-ammonium potassium salt crude product obtained after thin film evaporation, put in vacuum drying oven by this crude product
One step is dried, and sets vacuum drying temperature 90 DEG C, by vacuum pump suction-0.08～-0.1MPa, takes out in drying course always
Vacuum, promotes the moisture baked out in glufosinate-ammonium potassium salt crude product to discharge rapidly, does not accumulates in baking oven, obtains content after drying 4h
It it is 96% glufosinate-ammonium potassium salt product.
Embodiment 7
First weigh 96% potassium carbonate potassium 75g, water 400g, then by soluble in water for potassium carbonate standby；Weigh 95% glufosinate-ammonium
Hydrochlorate 100g adds in 500ml four-hole boiling flask, then the solution of potassium carbonate prepared slowly is poured stirring in four-hole boiling flask anti-into
Should, it is warmed up to 80 DEG C of insulation reaction 1h, is filtered to remove the insoluble solid impurities brought in raw material.Filtrate processes dress by film
Put, potassium chloride is separated with glufosinate-ammonium potassium salt soln, remove the glufosinate-ammonium potassium salt soln after potassium chloride and first carry out concentrating under reduced pressure, remove
Going portion of water to make glufosinate-ammonium potassium salts content in concentrated solution be about 40%, concentrated solution uses the mode of spray drying to be dehydrated again
Processing, spray drying temperature is set as 150 DEG C, is spray-dried time of staying 5s；The spray-dried glufosinate-ammonium potassium salt obtained is thick
Possibly together with more moisture in product, this crude product is put in vacuum drying oven and dries further, set vacuum drying temperature 90 DEG C,
By vacuum pump suction-0.08～-0.1MPa, evacuation always in drying course, promote glufosinate-ammonium potassium salt crude product bakes out
Moisture can discharge rapidly, do not accumulate in baking oven, dry that to obtain content after 4h be 92% glufosinate-ammonium potassium salt product.
Embodiment 8
First weigh 96% potassium carbonate 69g, water 400g, then by soluble in water for potassium carbonate standby；Weigh 95% glufosinate-ammonium salt
Hydrochlorate 100g adds in 500ml four-hole boiling flask, and then the solution of potassium carbonate prepared slowly is poured into stirring reaction in four-hole boiling flask,
It is warmed up to 80 DEG C of insulation reaction 1h, is filtered to remove the insoluble solid impurities brought in raw material.Filtrate passes through membrane treatment appts, will
Potassium chloride separates with glufosinate-ammonium potassium salt soln, removes the glufosinate-ammonium potassium salt soln after potassium chloride and first carries out concentrating under reduced pressure, removing unit
Dividing moisture to make glufosinate-ammonium potassium salts content in concentrated solution be about 60%, concentrated solution uses the mode of thin film evaporation to carry out at dehydration again
Reason, possibly together with more moisture in the glufosinate-ammonium potassium salt crude product obtained, puts into vacuum drying oven by this crude product after thin film evaporation
In dry further, set vacuum drying temperature 90 DEG C, by vacuum pump suction-0.08～-0.1MPa, in drying course one
Straight evacuation, promotes the moisture baked out in glufosinate-ammonium potassium salt crude product to discharge rapidly, does not accumulates in baking oven, obtains after drying 4h
Content is 92% glufosinate-ammonium potassium salt product.
Claims (10)
1. the method preparing glufosinate-ammonium potassium salt, it is characterised in that including: by slow for the aqueous solution of potassium hydroxide or potassium carbonate
Adding to glufosinate-ammonium or glufosinate-ammonium hydrochlorate, stirring reaction 0-12h at 0-90 DEG C, reaction terminates rear reactant liquor through pure
Change, be concentrated to give the glufosinate-ammonium potassium salt soln that content is 30%～70%, glufosinate-ammonium potassium salt soln is dried to obtain glufosinate-ammonium potassium
Salt crude product, carries out vacuum drying and obtains glufosinate-ammonium potassium salt solid this crude product；Described glufosinate-ammonium or glyphosate salt hydrochlorate with
The mol ratio of potassium hydroxide or potassium carbonate is 1: (0.1-5).
2. the method for claim 1, it is characterised in that described glufosinate-ammonium and potassium hydroxide mol ratio are 1: (1-
1.2), glufosinate-ammonium and potassium carbonate mol ratio 1: (0.5～0.6)；Glufosinate-ammonium hydrochlorate and potassium hydroxide mol ratio 1: (2～
2.4), glufosinate-ammonium and potassium carbonate mol ratio 1: (1～1.2).
3. the method for claim 1, it is characterised in that the drying means of described glyphosate potassium saline solution is spray dried
Dry or thin film evaporation.
4. synthetic method as claimed in claim 3, it is characterised in that described spray drying includes that the atomization of air current spray nozzle formula is dry
Dry, pressure nozzle atomization drying, rotation type atomization be dried in one.
5. the synthetic method as described in claim 3 or 4, it is characterised in that the temperature of described spray drying is 100-250
℃。
6. synthetic method as claimed in claim 5, it is characterised in that described spray drying temperature is preferably 130-170 DEG C.
7. the synthetic method as described in right 3 or 4, it is characterised in that described Drying Time of Vertical Spray Dryer is 1～15s.
8. synthetic method as claimed in claim 1, it is characterised in that described vacuum drying vacuum be-0.06～-
0.1MPa。
9. the synthetic method as described in claim 1 or 8, it is characterised in that described vacuum drying temperature is 20-150 DEG C.
10. synthetic method as claimed in claim 9, it is characterised in that described vacuum drying temperature is preferably 80-90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610621138.2A CN106279269A (en) | 2016-07-28 | 2016-07-28 | A kind of method preparing glufosinate-ammonium potassium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610621138.2A CN106279269A (en) | 2016-07-28 | 2016-07-28 | A kind of method preparing glufosinate-ammonium potassium salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106279269A true CN106279269A (en) | 2017-01-04 |
Family
ID=57663905
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610621138.2A Pending CN106279269A (en) | 2016-07-28 | 2016-07-28 | A kind of method preparing glufosinate-ammonium potassium salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106279269A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113666960A (en) * | 2021-10-22 | 2021-11-19 | 江苏七洲绿色科技研究院有限公司 | Method for recovering glufosinate-ammonium from glufosinate-ammonium crystallization mother liquor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186622A (en) * | 2006-11-17 | 2008-05-28 | 浙江新安化工集团股份有限公司 | Method for preparing solid glyphosate potassium salt |
| CN104262391A (en) * | 2014-07-08 | 2015-01-07 | 重庆紫光化工股份有限公司 | Environmentally-friendly clean production method of high-purity glufosinate-ammonium |
| CN105481894A (en) * | 2015-11-27 | 2016-04-13 | 浙江新安化工集团股份有限公司 | New method or preparing glufosinate ammonium salt |
-
2016
- 2016-07-28 CN CN201610621138.2A patent/CN106279269A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186622A (en) * | 2006-11-17 | 2008-05-28 | 浙江新安化工集团股份有限公司 | Method for preparing solid glyphosate potassium salt |
| CN104262391A (en) * | 2014-07-08 | 2015-01-07 | 重庆紫光化工股份有限公司 | Environmentally-friendly clean production method of high-purity glufosinate-ammonium |
| CN105481894A (en) * | 2015-11-27 | 2016-04-13 | 浙江新安化工集团股份有限公司 | New method or preparing glufosinate ammonium salt |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113666960A (en) * | 2021-10-22 | 2021-11-19 | 江苏七洲绿色科技研究院有限公司 | Method for recovering glufosinate-ammonium from glufosinate-ammonium crystallization mother liquor |
| CN113666960B (en) * | 2021-10-22 | 2022-02-18 | 江苏七洲绿色科技研究院有限公司 | Method for recovering glufosinate-ammonium from glufosinate-ammonium crystallization mother liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104262393B (en) | Energy-saving clean production method and device of glyphosate | |
| CN107253912B (en) | Synthetic method of cyhalofop-butyl | |
| CN105384714A (en) | Decolorization and purification technology for sodium dehydroacetate | |
| CN106632093A (en) | Preparation method of 2-bromine-5,6-diphenyl pyrazine | |
| CN103554179A (en) | Method for producing N-(phosphonomethyl)iminodiacetic acid and recycling mother solution by hydrogen chloride desalinization | |
| CN103896855A (en) | Method for synthesizing 4-(1-bromoethyl) -5-fluoro-6-chloropyrimidine | |
| CN106279269A (en) | A kind of method preparing glufosinate-ammonium potassium salt | |
| CN104621178B (en) | A kind of glyphosate pesticide active compound and preparation method thereof | |
| CN105646580A (en) | Method for producing pentahydrate s-ornidazole disodium phosphate | |
| CN104119243A (en) | Iminodiacetic acid energy saving cleaning production method | |
| CN107721849A (en) | A kind of method for preparing amide of mint intermediate peppermint acid | |
| CN110283104A (en) | A kind of preparation method of arginine Perindopril | |
| CN107602341A (en) | A kind of method from epoxy height boiling extraction trichloropropane | |
| CN104926692A (en) | Preparation process for bromoxynil octanoate | |
| CN104402881B (en) | A kind of synthetic method of 3-aldehyde radical-6-bromine imidazo [1,2-a] pyridine-8-ethyl formate | |
| CN107400123A (en) | A kind of production method of Diacloden | |
| CN102964225A (en) | Preparation method of 2, 3-dichloroanisole | |
| CN101575306B (en) | Method for preparing sivelestat sodium | |
| CN105175249B (en) | A kind of method for preparing 2,4 D dimethylamine salt solids | |
| CN105017049A (en) | Preparation process of dihydrophenyl glycine potassium salt | |
| CN106866739B (en) | The preparation method of one kind (R) -1- (6- amino -9H- purine -9- bases) 2- phenyl esters | |
| CN109293578A (en) | A kind of preparation method of the chloro- 5- nitro-pyrimidine of 2,4- bis- | |
| CN110437279B (en) | Preparation method of ammonium glyphosate technical | |
| CN109761786A (en) | A kind of preparation method of dicamba | |
| CN107162069A (en) | The recovery process of ruthenium trichloride catalyst in a kind of trimethyl pyruvic acid synthesis procedure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170104 |