CN101875671A - Synthesis method of glyphosate - Google Patents
Synthesis method of glyphosate Download PDFInfo
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- CN101875671A CN101875671A CN2009100501837A CN200910050183A CN101875671A CN 101875671 A CN101875671 A CN 101875671A CN 2009100501837 A CN2009100501837 A CN 2009100501837A CN 200910050183 A CN200910050183 A CN 200910050183A CN 101875671 A CN101875671 A CN 101875671A
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Abstract
The invention relates to a synthesis method of glyphosate, which comprises the following steps: (1) respectively pouring paraformaldehyde, methanol and triethylamine into a reaction kettle, controlling the temperature of the reaction kettle to be 30-50 DEG C, and reacting for 0.5-2h under stirring; (2) adding glycine into the reaction kettle, controlling the temperature of the reaction kettle to be 30-50 DEG C, and reacting for 0.5-2h under stirring; (3) adding dimethyl phosphite into the reaction kettle, controlling the temperature of the reaction kettle to be 55-65 DEG C, and reacting for 0.5-1.5h under stirring; (4) controlling the temperature of the reaction kettle to be 40-50 DEG C, adding hydrochloric acid into the reaction kettle, increasing the temperature of the reaction kettle to be 110-135 DEG C, and preserving the temperature and precipitating for 1-2h; and (5) after heat preservation and precipitating, cooling, crystallizing, carrying out suction filtration, and then, drying to obtain glyphosate raw powder. By increasing the temperature of condensation reaction, the invention shortens the synthesis time of the glyphosate and improves the yield of the glyphosate; and the obtained glyphosate raw powder has larger particles.
Description
Technical field
The present invention relates to a kind of synthetic method, especially relate to a kind of synthetic method of glyphosate.
Background technology
Glyphosate is as a kind of broad-spectrum herbicide, because its special herbicidal effect has become Pesticidal products most widely used in the world, that output is maximum.In recent years, along with the development of transgenosis glyphosate resistant crops, the glyphosate consumption increases year by year.At present, the synthetic production of glyphosate mainly by two lines, is respectively: IDA route and glycine route.External glyphosate production producer walks the IDA route to produce glyphosate; Domestic glyphosate production producer then adopts mostly by the glycine of the spontaneous development of China and produces route.The production technique of glycine route mainly comprises: depolymerization, addition, condensation, hydrolysis and crystallization, because adding some uncontrollable factors, the various and complicacy of its building-up reactions make the yield of glyphosate can not get bigger lifting, and the production cycle is longer.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of raising setting-up point for the defective that overcomes above-mentioned prior art existence, shortens the reaction times, improves the synthetic method of the glyphosate of yield.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of synthetic method of glyphosate is characterized in that, this method shortens soaking time by improving the glyphosate setting-up point, increases the yield of glyphosate, specifically may further comprise the steps:
(1) Paraformaldehyde 96, methyl alcohol and triethylamine are dropped into reactor respectively, control still temperature is 30-50 ℃, and stirring reaction 0.5-2h obtains depolymerization liquid;
(2) glycine is added in the reactor, opening chuck recirculated water control still temperature is 30-50 ℃, stirring reaction 0.5-2h;
(3) dimethylphosphite is added in the reactor, control still temperature is 55-65 ℃, stirring reaction 0.5-1.5h;
(4) control still temperature is 40-50 ℃, and hydrochloric acid is added reactor, again with the still temperature rise to 110-135 ℃, be incubated precipitation 1-2h;
(5) after the insulation precipitation finishes, behind decrease temperature crystalline, suction filtration after drying, obtain the former powder of glyphosate.
The weight ratio of Paraformaldehyde 96, methyl alcohol and triethylamine is (0.88-0.98) in the described step (1): (5.9-6.5): (1.4-1.45).
The add-on of glycine and the weight ratio of Paraformaldehyde 96 are (1.1-1.2) in the described step (2): (0.88-0.98).
The add-on of dimethylphosphite and the weight ratio of Paraformaldehyde 96 are (1.9-1.95) in the described step (3): (0.88-0.98).
The add-on of hydrochloric acid and the weight ratio of Paraformaldehyde 96 are (5.5-5.85) in the described step (4): (0.88-0.98).
The concentration expressed in percentage by weight of hydrochloric acid is 30-35% in the described step (4).
Compared with prior art, the present invention shortens soaking time by improving the glyphosate setting-up point, increases the yield of glyphosate, has the following advantages:
(1) by improving setting-up point, shortened the generated time of glyphosate;
(2) yield of glyphosate increases to some extent;
The particle of the former powder of glyphosate that (3) obtains increases to some extent, is easy to packing and transportation.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
Shorten soaking time and increase the yield of glyphosate by the temperature that improves the glyphosate condensation reaction, it is characterized in that the raising of temperature has aggravated reaction, impel to react completely.
(1) Paraformaldehyde 96 88kg, methyl alcohol 590kg and triethylamine 140kg are dropped into reactor respectively, open whipping appts and control the still temperature at 30 ℃, insulation 0.5h carries out depolymerization reaction;
(2) after depolymerization reaction finishes, keep stirring, glycine 110kg is added in the reactor, opening chuck recirculated water control still temperature is 30 ℃, and insulation 2h carries out addition reaction;
(3) after addition reaction finishes, dimethylphosphite 190kg is added in the reactor, keep stirring and being warming up to 55 ℃, insulation 0.5h carries out condensation reaction;
(4) after the condensation reaction end, control still temperature is 40 ℃, keeps stirring hydrochloric acid 550kg is added in the reactor, after the hydrochloric acid adding finishes temperature is risen to 110 ℃, insulation precipitation 1h;
(5) after the insulation precipitation finishes, behind decrease temperature crystalline, suction filtration after drying, obtain the former powder of glyphosate.
Embodiment 2
Shorten soaking time and increase the yield of glyphosate by the temperature that improves the glyphosate condensation reaction, it is characterized in that the raising of temperature has aggravated reaction, impel to react completely.
(1) Paraformaldehyde 96 95kg, methyl alcohol 620kg and triethylamine 142kg are dropped into reactor respectively, open whipping appts and control the still temperature at 40 ℃, insulation 1h carries out depolymerization reaction;
(2) after depolymerization reaction finishes, keep stirring, glycine 115kg is added in the reactor, opening chuck recirculated water control still temperature is 40 ℃, and insulation 1h carries out addition reaction;
(3) after addition reaction finishes, dimethylphosphite 193kg is added in the reactor, keep stirring and being warming up to 60 ℃, insulation 1h carries out condensation reaction;
(4) after the condensation reaction end, control still temperature is 45 ℃, keeps stirring hydrochloric acid 580kg is added in the reactor, after the hydrochloric acid adding finishes temperature is risen to 125 ℃, insulation precipitation 1.5h;
(5) after the insulation precipitation finishes, behind decrease temperature crystalline, suction filtration after drying, obtain the former powder of glyphosate.
Embodiment 3
Shorten soaking time and increase the yield of glyphosate by the temperature that improves the glyphosate condensation reaction, it is characterized in that the raising of temperature has aggravated reaction, impel to react completely.
(1) Paraformaldehyde 96 98kg, methyl alcohol 650kg and triethylamine 145kg are dropped into reactor respectively, open whipping appts and control the still temperature at 50 ℃, insulation 2h carries out depolymerization reaction;
(2) after depolymerization reaction finishes, keep stirring, glycine 120kg is added in the reactor, opening chuck recirculated water control still temperature is 50 ℃, and insulation 2h carries out addition reaction;
(3) after addition reaction finishes, dimethylphosphite 195kg is added in the reactor, keep stirring and being warming up to 65 ℃, insulation 1.5h carries out condensation reaction;
(4) after the condensation reaction end, control still temperature is 50 ℃, keeps stirring hydrochloric acid 585kg is added in the reactor, after the hydrochloric acid adding finishes temperature is risen to 135 ℃, insulation precipitation 2h;
(5) after the insulation precipitation finishes, behind decrease temperature crystalline, suction filtration after drying, obtain the former powder of glyphosate.
Claims (6)
1. the synthetic method of a glyphosate is characterized in that, this method shortens soaking time by improving the glyphosate setting-up point, increases the yield of glyphosate, specifically may further comprise the steps:
(1) Paraformaldehyde 96, methyl alcohol and triethylamine are dropped into reactor respectively, control still temperature is 30-50 ℃, and stirring reaction 0.5-2h obtains depolymerization liquid;
(2) glycine is added in the reactor, opening chuck recirculated water control still temperature is 30-50 ℃, stirring reaction 0.5-2h;
(3) dimethylphosphite is added in the reactor, control still temperature is 55-65 ℃, stirring reaction 0.5-1.5h;
(4) control still temperature is 40-50 ℃, and hydrochloric acid is added reactor, again with the still temperature rise to 110-135 ℃, be incubated precipitation 1-2h;
(5) after the insulation precipitation finishes, behind decrease temperature crystalline, suction filtration after drying, obtain the former powder of glyphosate.
2. the synthetic method of a kind of glyphosate according to claim 1 is characterized in that, the weight ratio of Paraformaldehyde 96, methyl alcohol and triethylamine is (0.88-0.98) in the described step (1): (5.9-6.5): (1.4-1.45).
3. the synthetic method of a kind of glyphosate according to claim 1 is characterized in that, the add-on of glycine and the weight ratio of Paraformaldehyde 96 are (1.1-1.2) in the described step (2): (0.88-0.98).
4. the synthetic method of a kind of glyphosate according to claim 1 is characterized in that, the add-on of dimethylphosphite and the weight ratio of Paraformaldehyde 96 are (1.9-1.95) in the described step (3): (0.88-0.98).
5. the synthetic method of a kind of glyphosate according to claim 1 is characterized in that, the add-on of hydrochloric acid and the weight ratio of Paraformaldehyde 96 are (5.5-5.85) in the described step (4): (0.88-0.98).
6. the synthetic method of a kind of glyphosate according to claim 1 is characterized in that, the concentration expressed in percentage by weight of hydrochloric acid is 30-35% in the described step (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100501837A CN101875671A (en) | 2009-04-28 | 2009-04-28 | Synthesis method of glyphosate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100501837A CN101875671A (en) | 2009-04-28 | 2009-04-28 | Synthesis method of glyphosate |
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| CN101875671A true CN101875671A (en) | 2010-11-03 |
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| CN2009100501837A Pending CN101875671A (en) | 2009-04-28 | 2009-04-28 | Synthesis method of glyphosate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775441A (en) * | 2012-07-30 | 2012-11-14 | 浙江金帆达生化股份有限公司 | Continuous production method of glyphosate synthetic liquid |
| CN103254036A (en) * | 2013-05-22 | 2013-08-21 | 吉林众鑫化工集团有限公司 | Method for gaseous-phase catalysis-free continuous synthesizing of 3-methyl-3-butenyl-1-alcohol |
| CN105254665A (en) * | 2015-11-13 | 2016-01-20 | 安徽省益农化工有限公司 | Preparation technology of glyphosate |
| CN107325126A (en) * | 2017-07-13 | 2017-11-07 | 安徽东至广信农化有限公司 | A kind of acidizing process of glyphosate production technique |
| CN107522738A (en) * | 2017-07-13 | 2017-12-29 | 安徽东至广信农化有限公司 | A kind of synthesis technique of glyphosate |
| CN114031637A (en) * | 2021-11-05 | 2022-02-11 | 安徽东至广信农化有限公司 | Continuous hydrolysis method of glyphosate |
-
2009
- 2009-04-28 CN CN2009100501837A patent/CN101875671A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775441A (en) * | 2012-07-30 | 2012-11-14 | 浙江金帆达生化股份有限公司 | Continuous production method of glyphosate synthetic liquid |
| CN102775441B (en) * | 2012-07-30 | 2015-07-22 | 浙江金帆达生化股份有限公司 | Continuous production method of glyphosate synthetic liquid |
| CN103254036A (en) * | 2013-05-22 | 2013-08-21 | 吉林众鑫化工集团有限公司 | Method for gaseous-phase catalysis-free continuous synthesizing of 3-methyl-3-butenyl-1-alcohol |
| CN105254665A (en) * | 2015-11-13 | 2016-01-20 | 安徽省益农化工有限公司 | Preparation technology of glyphosate |
| CN107325126A (en) * | 2017-07-13 | 2017-11-07 | 安徽东至广信农化有限公司 | A kind of acidizing process of glyphosate production technique |
| CN107522738A (en) * | 2017-07-13 | 2017-12-29 | 安徽东至广信农化有限公司 | A kind of synthesis technique of glyphosate |
| CN114031637A (en) * | 2021-11-05 | 2022-02-11 | 安徽东至广信农化有限公司 | Continuous hydrolysis method of glyphosate |
| CN114031637B (en) * | 2021-11-05 | 2024-06-11 | 安徽东至广信农化有限公司 | Method for continuously hydrolyzing glyphosate |
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Application publication date: 20101103 |