CN104860989A - Preparation method of glyphosate sodium and glyphosate sodium preparation - Google Patents
Preparation method of glyphosate sodium and glyphosate sodium preparation Download PDFInfo
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- CN104860989A CN104860989A CN201510289393.7A CN201510289393A CN104860989A CN 104860989 A CN104860989 A CN 104860989A CN 201510289393 A CN201510289393 A CN 201510289393A CN 104860989 A CN104860989 A CN 104860989A
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Abstract
The invention provides a preparation method of glyphosate sodium and a glyphosate sodium preparation. The method comprises the following steps: alkaline materials containing sodium ion and solid glyphosate acid are put into a kneading machine to be reacted, the reaction temperature is 5 to 70 DEG C, the rotate speed of the kneading machine is 10 to 50 rpm, and the reaction time is 10 to 300 min. The invention further provides a glyphosate sodium preparation. The glyphosate sodium preparation comprises the following components in percentage by weight: 20 to 95 percent of the glyphosate sodium prepared through the method, 0 to 25 percent of a surface active agent, and 0 to 75 percent of other fills. The preparation method and the glyphosate sodium preparation have the advantages that the method is simple to operate, the reaction condition is mild, drying heat load is reduced, generated nitrosamine is reduced, antioxidants do not need to be added during the reaction process, the involvement of organic solvent is avoided at the same time, a third type of material does not need to be introduced, the pollution is low, and the cost is low.
Description
Technical field
The invention belongs to technical field of pesticide, be specifically related to a kind of preparation method and sodium glyphosate preparation of sodium glyphosate.
Background technology
Glyphosate is inner sucting conduction type wide spectrum steriland herbicide, sterling is non-volatile white solid, proportion is 0.5, greatly about about 230 DEG C fusings also adjoint decomposition, the solubleness under normal temperature in water only has 1.2 grams, in actual applications, normally glyphosphonic acid is mixed with water miscible salt, the more glyphosate salt formulations of current use is glyphosate isopropyl amine salt, glyphosate potassium, ammonium glyphosate and sodium glyphosate, and wherein, most widely used is ammonium glyphosate.
At present, glyphosate formulation, still based on aqua, because aqua comprises a large amount of water, is made troubles to the aspects such as packaging, transport and storage, is caused cost to increase simultaneously, along with the development in market, more and more urgent to the demand of high content glyphosate solid preparation.
Chinese patent application 96196134.1 discloses a kind of ammoniacal liquor and glyphosate reacts the method preparing ammonium glyphosate, wherein a large amount of moisture content need be removed by the form of drying warm air drying, energy consumption is high and moisture content removal efficiency is not high, because long hot air dries causes the oxidation of glyphosphonic acid, the nitrosamine needing to control content can be generated, reaction process also needs to add antioxidant S-WAT, adds production cost.
Chinese patent application 02141788.1 discloses one and first adds glyphosate and water, and then pass into the reaction of ammonia, ammonium glyphosate salt brine solution is generated after reacting completely, then utilizing organic solvent that ammonium glyphosate is extracted acquisition glyphosate ammonium salt solid, the method speed of response is fast, simple to operate, but interpolation organic solvent adds cost.
Chinese patent application 200610154745.9 discloses a kind of method preparing solid glyphosate potassium salt, this reaction needs to add a large amount of water in generating process, the solid wet product obtained forms glyphosate potassium salt technical product by drying, the method has a large amount of mother liquors to generate, and not easily crystallization, energy consumption is large, and cost is high.
Sodium glyphosate has following advantage compared with other soluble salts such as ammonium glyphosate: a certain amount of sodium element can improve that plant absorbs water, fertilizer sucting ability, the transpiration of plant can be reduced to a certain extent, promote plant cell growth, the stomatal movement of adjusting vane, improves the photosynthesis of plant.
Summary of the invention
Not enough for prior art, the invention provides a kind of preparation method and sodium glyphosate preparation of sodium glyphosate, the method is easy and simple to handle, and reaction conditions is gentle, decreases oven dry thermal load, decrease the generation of nitrosamine, do not need in reaction process to add antioxidant, avoid the intervention of organic solvent simultaneously, do not need to introduce the third material, pollute few, cost is low.
In order to realize foregoing invention object, the invention provides following technical scheme:
A preparation method for sodium glyphosate, comprise and reacting in the alkaline matter containing sodium ion and solid glyphosate acid input kneader, temperature of reaction is 5-70 DEG C, and kneader rotating speed is 10-50 rev/min, and the reaction times is 10-300min.
Be preferably, this reaction system is without the need to adding water, and do not have extra mother liquor to produce, oven dry power consumption is low.
Be preferably, described temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, and the described reaction times is 300min.
Preferably, this reaction system also needs to add water, and described solid glyphosate acid is 1:0.01-0.09 with the weight ratio of water, and the method amount of water is few, and do not have extra mother liquor to produce, oven dry power consumption is low.
Be preferably, described temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, and the reaction times is 120min.
Be preferably, the described alkaline matter containing sodium ion be selected from sodium hydroxide, sodium carbonate and sodium bicarbonate any one or multiple.
Be preferably, the described alkali containing sodium cation is sodium hydroxide, and sodium hydroxide stable chemical nature is cheap.
The invention still further relates to the preparation of the sodium glyphosate prepared by aforesaid method, the technique means taked is:
A preparation for the sodium glyphosate adopting aforesaid method to prepare, by weight percentage, composed of the following components: sodium glyphosate is 20-95%, tensio-active agent is 0-25%, other fillers 0-75%.
Be preferably, described tensio-active agent is selected from alkyl glycoside class tensio-active agent or tallow amine surfactants.
Preferably, other described fillers are selected from one or more in sodium sulfate, ammonium sulfate, ammonium chloride, urea.
The beneficial effect of the preparation method of a kind of sodium glyphosate of the present invention is: the method is easy and simple to handle, reaction conditions is gentle, decrease oven dry thermal load, decrease the generation of nitrosamine, do not need in reaction process to add antioxidant, avoid the intervention of organic solvent simultaneously, do not need to introduce the third material, pollute few, cost is low, this sodium glyphosate preparation contains a certain amount of sodium element, plant water suction can be improved, fertilizer sucting ability, the transpiration of plant can be reduced to a certain extent, promote plant cell growth, the stomatal movement of adjusting vane, improve the photosynthesis of plant.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below; obviously; described embodiment is only the present invention's part embodiment; instead of whole embodiments; based on the embodiment in the present invention; those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1: sodium glyphosate
Glyphosphonic acid dry powder 200.0g is added in kneader, powdered sodium hydroxide 55.0g, ceaselessly stir kneading, temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, exothermic heat of reaction, material moisture increases simultaneously, and the material of semi-solid is directly dried after reaching 300min by the reaction times, obtain white solid, obtain the former medicine 232.7g of sodium glyphosate after crushed.Content is 93.8% by analysis.
Embodiment 2: sodium glyphosate
Glyphosphonic acid dry powder 200.0g is added in kneader, powdery sodium bicarbonate 115.0g, ceaselessly stir kneading, temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, exothermic heat of reaction also ceaselessly releases carbon dioxide, material moisture increases simultaneously, and the material of semi-solid is directly dried after reaching 300min by the reaction times, obtain white solid, obtain the former medicine 230.5g of sodium glyphosate after crushed.Content is 93.5% by analysis.
Embodiment 3: sodium glyphosate
Glyphosphonic acid dry powder 200.0g is added in kneader, powdered sodium carbonate 72.3g, ceaselessly stir kneading, temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, exothermic heat of reaction also ceaselessly releases carbon dioxide, material moisture increases simultaneously, and the material of semi-solid is directly dried after reaching 300min by the reaction times, obtain white solid, obtain the former medicine 231.5g of sodium glyphosate after crushed.Content is 93.2% by analysis.
Embodiment 4: sodium glyphosate
Glyphosphonic acid dry powder 200.0g is added in kneader, powdered sodium hydroxide 55.0g, add 2.0g water after mixing and ceaselessly stir kneading, temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, exothermic heat of reaction, material moisture increases simultaneously, and the material of semi-solid is directly dried after reaching 300min by the reaction times, obtain white solid, obtain the former medicine 233.0g of sodium glyphosate after crushed.Content is 94.0% by analysis.
Embodiment 5: sodium glyphosate
Glyphosphonic acid dry powder 200.0g is added in kneader, powdered sodium hydroxide 55.0g, add 10.0g water after mixing and ceaselessly stir kneading, temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, exothermic heat of reaction, material moisture increases simultaneously, and the material of semi-solid is directly dried after reaching 240min by the reaction times, obtain white solid, obtain the former medicine 233.2g of sodium glyphosate after crushed.Content is 94.1% by analysis.
Embodiment 6: sodium glyphosate
Glyphosphonic acid dry powder 200.0g is added in kneader, powdered sodium hydroxide 55.0g, add 18.0g water after mixing and ceaselessly stir kneading, temperature of reaction is 32 DEG C, and kneader rotating speed is 30 revs/min, exothermic heat of reaction, material moisture increases simultaneously, and the material of semi-solid is directly dried after reaching 120min by the reaction times, obtain white solid, obtain the former medicine 233.5g of sodium glyphosate after crushed.Content is 94.3% by analysis.
Embodiment 7: sodium glyphosate granula
Take sodium glyphosate dry product 20g, ammonium sulfate 55g mixes, then adds 25g tallow amine Soxylat A 25-7 ceaselessly stirring, then add 20g water stir after granulation dry, obtain sodium glyphosate soluble granula.
Embodiment 8: sodium glyphosate pulvis
Take sodium glyphosate dry product 95g, ammonium sulfate 2g and tallow amine Soxylat A 25-7 3g mixes, and obtains sodium glyphosate pulvis.
Embodiment 9: sodium glyphosate tablet
Take sodium glyphosate dry product 50g, ammonium sulfate 55g mixes, then adds 5g tallow amine Soxylat A 25-7 ceaselessly stirring, then add 20g water stir after compressing tablet dry, obtain sodium glyphosate tablet.
Claims (9)
1. the preparation method of a sodium glyphosate, it is characterized in that: comprise and reacting in the alkaline matter containing sodium ion and solid glyphosate acid input kneader, temperature of reaction is 5-70 DEG C, and kneader rotating speed is 10-50 rev/min, and the reaction times is 10-300min.
2. the preparation method of sodium glyphosate as claimed in claim 1, is characterized in that: this reaction system is without the need to adding water.
3. the preparation method of sodium glyphosate as claimed in claim 2, it is characterized in that: described temperature of reaction is 32 DEG C, kneader rotating speed is 30 revs/min, and the described reaction times is 300min.
4. the preparation method of sodium glyphosate as claimed in claim 1, is characterized in that: this reaction system also needs to add water, and described solid glyphosate acid is 1:0.01-0.09 with the weight ratio of water.
5. the preparation method of sodium glyphosate as claimed in claim 4, it is characterized in that: described temperature of reaction is 32 DEG C, kneader rotating speed is 30 revs/min, and the reaction times is 120min.
6. the preparation method of the sodium glyphosate as described in as arbitrary in claim 1 to 5, is characterized in that: the described alkaline matter containing sodium ion be selected from sodium hydroxide, sodium carbonate and sodium bicarbonate any one or multiple.
7. a preparation for the sodium glyphosate adopting method as claimed in claim 6 to prepare, it is characterized in that: by weight percentage, composed of the following components: sodium glyphosate is 20-95%, tensio-active agent is 0-25%, and other fillers are 0-75%.
8. the preparation of sodium glyphosate as claimed in claim 7, is characterized in that: described tensio-active agent is selected from alkyl glycoside class tensio-active agent or tallow amine surfactants.
9. sodium glyphosate preparation as claimed in claim 7, is characterized in that: other described fillers be selected from sodium sulfate, ammonium sulfate, ammonium chloride, urea one or more.
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| CN201510289393.7A CN104860989A (en) | 2015-06-01 | 2015-06-01 | Preparation method of glyphosate sodium and glyphosate sodium preparation |
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| CN201510289393.7A CN104860989A (en) | 2015-06-01 | 2015-06-01 | Preparation method of glyphosate sodium and glyphosate sodium preparation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106259324A (en) * | 2016-07-14 | 2017-01-04 | 山东润博生物科技有限公司 | A kind of glyphosate dimethylamine salt water-soluble granule and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5070197A (en) * | 1986-03-20 | 1991-12-03 | Uniroyal Chemical Company, Inc. | Dry reactive processing |
| CN1684586A (en) * | 2002-08-31 | 2005-10-19 | 孟山都技术公司 | Sodium glyphosate compositions and process for their preparation |
| CN101524085A (en) * | 2009-04-21 | 2009-09-09 | 山东潍坊润丰化工有限公司 | Preparation method of glyhosate ammonium water-soluble granules |
-
2015
- 2015-06-01 CN CN201510289393.7A patent/CN104860989A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5070197A (en) * | 1986-03-20 | 1991-12-03 | Uniroyal Chemical Company, Inc. | Dry reactive processing |
| CN1684586A (en) * | 2002-08-31 | 2005-10-19 | 孟山都技术公司 | Sodium glyphosate compositions and process for their preparation |
| CN101524085A (en) * | 2009-04-21 | 2009-09-09 | 山东潍坊润丰化工有限公司 | Preparation method of glyhosate ammonium water-soluble granules |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106259324A (en) * | 2016-07-14 | 2017-01-04 | 山东润博生物科技有限公司 | A kind of glyphosate dimethylamine salt water-soluble granule and preparation method thereof |
| CN106259324B (en) * | 2016-07-14 | 2020-03-17 | 山东润博生物科技有限公司 | Glyphosate dimethylamine salt water-soluble granule and preparation method thereof |
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Application publication date: 20150826 |