CN106188137A - A kind of method preparing high content glyphosate dimethylamine salt - Google Patents
A kind of method preparing high content glyphosate dimethylamine salt Download PDFInfo
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- CN106188137A CN106188137A CN201510294108.0A CN201510294108A CN106188137A CN 106188137 A CN106188137 A CN 106188137A CN 201510294108 A CN201510294108 A CN 201510294108A CN 106188137 A CN106188137 A CN 106188137A
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- glyphosate
- dimethylamine
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Abstract
Glyphosate is not readily dissolved in water, therefore, typically requires before the use and is configured to glyphosate salt, and glyphosate dimethylamine salt is one of product that in current glyphosate salt, effect is best.In prior art, glyphosate and dimethylamine gas is added in alcoholic solution, crystallize after reaction, filter and i.e. obtain glyphosate dimethylamine salt, but because dimethylamine gas is inflammable and explosive, so ratio is relatively hazardous when technique produces, for the deficiencies in the prior art, the invention discloses a kind of method preparing glyphosate different diformazan salt, react including glyphosate and dimethylamine agueous solution being joined in conventional reactor, after question response is complete, reactant liquor is concentrated, adds alcohol and a small amount of crystal seed, stirred crystallization, after being down to room temperature, filter or centrifugal, be dried.Owing to adding alcoholic solution after having reacted, crystallization can be promoted, solve the problem crystallizing difficulty in prior art；The product purity obtained is high, steady quality；Owing to not using dimethylamine gas, production process is the most safe and reliable.
Description
Technical field
The present invention relates to chemical field, specifically, relate to a kind of herbicidal activity composition N-phosphonomethyl glycine (glyphosate)
The preparation method of dimethylamine salt.
Background technology
Glyphosate also known as: glyphosate, agriculture reach (Roundup), careless dry phosphine, the sweet acid of phosphine, are that a kind of non-selective, noresidue is gone out
Nature herbiciding agent, highly effective to prennical root weeds, it is widely used in rubber, Mulberry, tea, orchard and sugarcane field.But due to grass
Sweet phosphine dissolubility in water is the lowest, actually used in, it is common that glyphosate formulation is become glyphosate salt be re-dissolved in water preparation
Become liquid herbicide, and glyphosate dimethylamine salt is one of kind that in glyphosate salt, effect is best.
China Patent No. 200910154988.6 discloses a kind of addition glyphosate in alcoholic solution, then is passed through dimethylamine gas, instead
Glyphosate dimethylamine salt should be generated, and dimethylamine gas is inflammable, explosive, poisonous gas, commercial process exist bigger
Potential safety hazard, and the reaction of glyphosate and dimethylamine gas is heterogeneous, it is necessary to could react by organic solvent, due to
Glyphosate and glyphosate dimethylamine salt are all not dissolved in above-mentioned organic solvent, therefore, are particularly easy to cause reaction not exclusively, thus
Affect glyphosate dimethylamine salt product quality.
This patent document is also pointed out a technical barrier, it is simply that when using 40% dimethylamine agueous solution as reactant, crystallization
Difficulty, becomes salt rate low, and yield is low.
Summary of the invention
For problem above, the present invention provides a kind of method preparing glyphosate dimethylamine salt, and the method need not by alcoholic solution
Can react abundant, and solve and prior art uses dimethylamine agueous solution prepare glyphosate dimethylamine salt crystallization difficulty, yield
Low technical problem.
The technical scheme is that
A kind of method preparing high content glyphosate dimethylamine salt, joins popular response including by glyphosate and dimethylamine agueous solution
Device reacts, after question response is complete, reactant liquor is concentrated, adds alcohol and a small amount of crystal seed, stirred crystallization, be down to room temperature
After, filter or centrifugal, be dried.
As preferably, glyphosate is 0.8～1.3 with the mol ratio of dimethylamine.
As preferably, described dimethylamine agueous solution concentration is 10～80%.
As preferably, described thickening temperature controls at 20～140 DEG C.
As preferably, described drying mode is that pneumatic conveying drying, vacuum drying, bipyramid are dried or pallet oven drying.
As preferably, described alcohol is methanol, ethanol or isopropanol.
As preferably, described crystal seed is glyphosate dimethylamine salt solid powder.
The repeatable utilization of mother solution as preferably, after filtering or being centrifugal.
As preferably, after repeatedly utilizing, mother solution need to carry out single treatment, i.e. normal pressure or decompression distillating carbinol, after methanol is evaporated off
Mother solution can directly feed intake and prepares the former medicine of glyphosate dimethylamine salt or directly join glyphosate dimethylamine salt water preparation.
As preferably, described reaction temperature controls at 10～100 DEG C, and the described response time controls at 10 minutes～180 minutes.
As preferably, described crystallization temperature control 60 DEG C and within, described crystallization time controlled at 0.5～10 hour.
As preferably, described baking temperature controls, at 20～120 DEG C, to control described drying time at 0.1～10 hour.
Beneficial effects of the present invention:
Need not add alcoholic solution in the stage of reaction, and add alcoholic solution after completion of the reaction, crystallization can be promoted, solve existing
When technology using 40% dimethylamine agueous solution as reactant, the problem of the crystallization difficulty occurred；Because glyphosate solution and diformazan
Amine aqueous solution is homogeneous, and reaction can be made more abundant, and the product purity obtained is high, steady quality；Owing to not using to two
Methylamine gas, production process is the most safe and reliable.
Detailed description of the invention:
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1:
Add glyphosate 300g, 33% dimethylamine agueous solution 254g in a kettle., stirring be allowed to molten clear after, be heated to 20 DEG C anti-
Answer 180 minutes, be allowed to become completely salt, concentrating under reduced pressure, after without distillate, stop heating, put into 500ml methanol solution with
A small amount of glyphosate dimethylamine salt solid powder, stirring, it is cooled to room temperature, after crystallizing 5 hours, centrifugal, dry 1 at 120 DEG C little
Time, obtaining white powdery solid glyphosate dimethylamine salt 326.1g, yield 85.0%, content 99.0%, the mother solution after being centrifuged is permissible
Recycling, accumulation can apply mechanically more than 5 batches.Wherein, time with after, mother solution need to carry out single treatment, i.e. utilize normal pressure or
Methanol is collected in decompression distillation, mother solution methanol after is evaporated off and can directly feed intake synthesizing glyphosate dimethylamine salt raw pesticide or be directly made into grass
Sweet phosphine dimethylamine salt water preparation.
Embodiment 2:
Add glyphosate 300g, 33% dimethylamine agueous solution 254g in a kettle., stirring be allowed to molten clear after, be heated to 30 DEG C anti-
After answering 120 minutes, it is allowed to become completely salt, concentrating under reduced pressure, after without distillate, stops heating, put into 500ml methanol solution
With a small amount of glyphosate dimethylamine salt solid powder, stirring, it is cooled to room temperature, after crystallizing 10 hours, filters, dry at 100 DEG C
3 hours, obtain white powdery solid glyphosate dimethylamine salt 326.1g, yield 85.0%, content 99.0%, the mother solution after filtration
Can reuse, accumulation can apply mechanically more than 5 batches.Wherein, after time, mother solution need to carry out single treatment, often i.e. utilizes
Pressure or decompression distillating carbinol, be evaporated off the mother solution after methanol and can directly feed intake synthesizing glyphosate dimethylamine salt raw pesticide or be directly made into grass
Sweet phosphine dimethylamine salt water preparation.
Embodiment 3:
Add glyphosate 300g, 33% dimethylamine agueous solution 254g in a kettle., stirring be allowed to molten clear after, be heated to 60 DEG C anti-
Answer 80 minutes, be allowed to become completely salt, concentrating under reduced pressure, after without distillate, stop heating, put into 500ml methanol solution with few
Amount glyphosate dimethylamine salt solid powder, stirring, it is cooled to room temperature, after crystallizing 0.5 hour, filters, dry 6 at 50 DEG C little
Time, obtaining white powdery solid glyphosate dimethylamine salt 326.1g, yield 85.0%, content 99.0%, the mother solution after filtration is permissible
Recycling, accumulation can apply mechanically more than 5 batches.Wherein, time with after, mother solution need to carry out single treatment, i.e. utilize normal pressure or
Methanol is collected in decompression distillation, mother solution methanol after is evaporated off and can directly feed intake synthesizing glyphosate dimethylamine salt raw pesticide or be directly made into grass
Sweet phosphine dimethylamine salt water preparation.
Embodiment 4:
Add glyphosate 300g, 33% dimethylamine agueous solution 254g in a kettle., stirring be allowed to molten clear after, be heated to 100 DEG C
React 10 minutes, be allowed to become completely salt, concentrating under reduced pressure, after without distillate, stop heating, put into 500ml methanol solution with
A small amount of glyphosate dimethylamine salt solid powder, stirring, it is cooled to room temperature, crystal separates out, and after filtration, is dried, obtains white powder
Shape solid glyphosate dimethylamine salt 326.1g, yield 85.0%, content 99.0%, the mother solution after filtration can reuse, accumulation
More than 5 batches can be applied mechanically.Wherein, after time, mother solution need to carry out single treatment, i.e. normal pressure or decompression distillation and collect methanol,
Mother solution methanol after is evaporated off can directly feed intake synthesizing glyphosate dimethylamine salt raw pesticide or be directly made into glyphosate dimethylamine salt water preparation.
Embodiment 5:
Add glyphosate 300g, 33% dimethylamine agueous solution 254g in a kettle., stirring be allowed to molten clear after, be heated to 50 DEG C
React 110 minutes, be allowed to become completely salt, concentrating under reduced pressure, after without distillate, stop heating, batch mother solution reclaimed in addition
With a small amount of glyphosate dimethylamine salt solid powder, stir and be cooled to room temperature, treating that crystal separates out, centrifugal, dry, obtain white powder
Shape solid glyphosate dimethylamine salt 358.4g, yield 93.4%, content 99.0%.
Embodiment 6:
Add glyphosate 300g, 33% dimethylamine agueous solution 254g in a kettle., stirring be allowed to molten clear after, be heated to 20 DEG C anti-
Answer 180 minutes, be allowed to become completely salt, concentrating under reduced pressure, after without distillate, stop heating, put into 500ml ethanol solution with
A small amount of glyphosate dimethylamine salt solid powder, stirring, it is cooled to room temperature, after crystallizing 5 hours, centrifugal, dry 1 at 120 DEG C little
Time, obtaining white powdery solid glyphosate dimethylamine salt 326.1g, yield 85.0%, content 99.0%, the waste liquid after being centrifuged is permissible
Recycling, accumulation can apply mechanically more than 5 batches.Wherein, time with after, mother solution need to carry out single treatment, i.e. utilize normal pressure or
Ethanol is collected in decompression distillation, mother solution ethanol after is evaporated off and can directly feed intake synthesizing glyphosate dimethylamine salt raw pesticide or be directly made into grass
Sweet phosphine dimethylamine salt water preparation.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and without departing substantially from
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from which
From the point of view of Dian, all should regard embodiment as exemplary, and be nonrestrictive, protection scope of the present invention is by claim
Limit, it is intended that all changes fallen in the implication of equivalency and scope of claim are included in the present invention.No
Should be considered as limiting involved claim by any reference in claim.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only comprises
One independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should will say
Bright book is as an entirety, and the technical scheme in each embodiment can also be through appropriately combined, and forming those skilled in the art can manage
Other embodiments solved.
Claims (10)
1. the method preparing high content glyphosate dimethylamine salt, step is as follows:
-add glyphosate and dimethylamine agueous solution,
After-question response is complete, reactant liquor is concentrated,
-add alcohol and a small amount of crystal seed, stirred crystallization,
-be down to room temperature after, filter or centrifugal, be dried.
2. the method for claim 1, it is characterised in that: described glyphosate is 0.8～1.3 with the mol ratio of dimethylamine.
3. the method for claim 1, it is characterised in that: described dimethylamine agueous solution concentration is 10～80%.
4. the method for claim 1, it is characterised in that: described thickening temperature is 20～140 DEG C.
5. the method for claim 1, it is characterised in that: described drying mode is pneumatic conveying drying, vacuum drying, and bipyramid is done
Dry or pallet oven drying.
6. the method for claim 1, it is characterised in that: described alcohol is methanol, ethanol or isopropanol.
7. the method for claim 1, it is characterised in that: described filtration or centrifugal after mother solution can reuse.
8. the method as described in claim 1-7 any claim, it is characterised in that: described reaction temperature is 10～100 DEG C, instead
It is 10～180 minutes between Ying Shi.
9. the method as described in claim 1-7 any claim, it is characterised in that: described crystallization temperature be 60 DEG C and within,
Described crystallization time is 0.5～10 hour.
10. the method as described in claim 1-7 any claim, it is characterised in that: described baking temperature is 20～120 DEG C,
Described drying time is 0.1～10 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3799758A (en) * | 1971-08-09 | 1974-03-26 | Monsanto Co | N-phosphonomethyl-glycine phytotoxicant compositions |
| CN1445234A (en) * | 2002-09-05 | 2003-10-01 | 浙江新安化工集团股份有限公司 | Gas-liquid-solid three phase reactions and solvent exraction for preparing ammonia glyphosate acid |
| CN101723973A (en) * | 2009-12-09 | 2010-06-09 | 浙江新安化工集团股份有限公司 | Method for preparing glyphosate dimethylamine salt solid |
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2015
- 2015-06-01 CN CN201510294108.0A patent/CN106188137B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3799758A (en) * | 1971-08-09 | 1974-03-26 | Monsanto Co | N-phosphonomethyl-glycine phytotoxicant compositions |
| CN1445234A (en) * | 2002-09-05 | 2003-10-01 | 浙江新安化工集团股份有限公司 | Gas-liquid-solid three phase reactions and solvent exraction for preparing ammonia glyphosate acid |
| CN101723973A (en) * | 2009-12-09 | 2010-06-09 | 浙江新安化工集团股份有限公司 | Method for preparing glyphosate dimethylamine salt solid |
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