CN102503978A - Process of adding acids prior to hydrolysis in glyphosate production - Google Patents

Process of adding acids prior to hydrolysis in glyphosate production Download PDF

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CN102503978A
CN102503978A CN2011103201155A CN201110320115A CN102503978A CN 102503978 A CN102503978 A CN 102503978A CN 2011103201155 A CN2011103201155 A CN 2011103201155A CN 201110320115 A CN201110320115 A CN 201110320115A CN 102503978 A CN102503978 A CN 102503978A
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hydrolysis
glyphosate
acid adding
water cooler
adding process
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CN2011103201155A
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CN102503978B (en
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姜永红
王利平
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Fuhua Tongda Chemical Co ltd
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SICHUAN LESHAN FUHUA TONGDA PESTICIDE TECHNOLOGY Co Ltd
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Abstract

The invention provides a process of adding acids prior to hydrolysis in glyphosate production. According to the invention, firstly hydrochloric acid is mixed with the condensation reaction liquid before hydrolysis to carry away most heat, and then hydrolysis is carried out. The process effectively reduces adverse effects of reaction heat, increases the yield of glyphosate and makes post-treatment easy.

Description

Acid adding process in a kind of glyphosate production before the hydrolysis
Technical field
The present invention relates to a kind of production technique of Glyphosate 62 IPA Salt, more particularly, the present invention relates to the acid adding process of hydrolysis in a kind of glyphosate production.
Background technology
Glyphosate 62 IPA Salt (glyphosate), formal name used at school N-((phosphonomethyl)) glycocoll, N-((phosphonomethyl)) Padil is a kind of organophosphorus herbicide.The herbicidal properties of Glyphosate 62 IPA Salt is to be found by U.S. D.D. Baird etc. in 1971, by Monsanto Company's Development and Production, has become the important kind of world's weedicide to the eighties in last century.Glyphosate 62 IPA Salt is the chronic wide spectrum steriland herbicide of inner sucting conduction type; The main interior enol acetonyl shikimin phosphate synthase of object that suppresses; Thereby suppress the conversion of shikimin, make proteinic synthetic being interfered cause plant dead to phenylalanine(Phe), cruel propylhomoserin and tryptophane.Glyphosate 62 IPA Salt is transmitted to each position of plant after absorbing through cauline leaf, can prevent and kill off the plant of sections more than 40 such as unifacial leaf and dicotyledonous, annual and perennial, draft and shrub.Combine with metals ions such as iron, aluminium very soon after Glyphosate 62 IPA Salt buries and lose activity, seed and the soil microorganisms that hides in the soil had no adverse effects.
The industrialized preparing process of Glyphosate 62 IPA Salt mainly contains two kinds at present: IDA method and glycine method.The glycine method key step is synthetic, hydrolysis, crystallization and solid-liquid separation.Be specially methyl alcohol, Paraformaldehyde 96 and triethylamine and carry out depolymerization reaction; Add glycocoll after reaction is accomplished and carry out addition reaction; Add dimethyl sulfite after the reaction again and carry out condensation reaction and obtain the synthetic liquid of condensation reaction, obtain Glyphosate 62 IPA Salt and acid mother liquor through hydrolysis, crystallization and solid-liquid separation at last, acid mother liquor adds the liquid caustic soda neutralization; After reclaiming triethylamine, remaining is alkaline mother liquor.Contain a small amount of Glyphosate 62 IPA Salt in the alkali liquor, about 1-2% has higher recovery value.
Will carry out the acid adding process step before the condensated liquid hydrolysis, traditional to add acid be in still, to add earlier to go up the step condensation reaction solution and add hydrochloric acid again, or add hydrochloric acid earlier and add and go on foot condensation reaction solution.Which kind of mode all can be because of increasing the generation of controlling difficulty and side reaction with concentrated heat release in hydrochloric acid and the triethylamine.
Summary of the invention
The present invention is intended to solve the problem of acid adding process concentrated heat release increasing control difficulty and side reaction in the prior art, and the acid adding process before the hydrolysis in a kind of glyphosate production is provided, and can effectively reduce the generation of reaction heat and side reaction.
In order to realize the foregoing invention purpose, concrete technical scheme of the present invention is following:
Acid adding process in a kind of glyphosate production before the hydrolysis is characterized in that: comprise following process step:
A, with synthetic liquid of condensation reaction and mol ratio calculating separately the flow of hydrochloric acid according to glycocoll and hydrogenchloride, mix in the input mixer respectively by two pipelines;
B, the neutralizer that after mixing, obtains get into water cooler immediately, in reaction, take the reaction heat exchange out of reaction system, guarantee that water cooler material liquid outlet temperature is equal to or less than the hydrolysis process temperature;
C, mix the neutralizer obtain and laggardly go into hydrolytic reaction pot and be hydrolyzed and make Glyphosate 62 IPA Salt through cooling off.
The glycocoll in the steps A of the present invention and the mol ratio of hydrogenchloride are 1:2.8~3.5.
Mixing tank in the steps A of the present invention is the mixing tank of ripple packing mode.
The filler of the mixing tank of above-mentioned ripple packing mode is pottery or acrylic plastering.
The sheating material of the mixing tank of above-mentioned ripple packing mode is graphite or acrylic plastering.
Water cooler among the step B of the present invention can be piece cellular type graphite cooler or piece cellular type glass cools device.
Water cooler of the present invention is to adopt chilled brine circulation cooling.
Water cooler material liquid outlet among the step B of the present invention is provided with TP, according to outlet feed temperature control neutralizer flow.
Hydrolysis process temperature among the step B of the present invention is 45 ℃.
The useful technique effect that the present invention brings:
1, through earlier condensation reaction solution and hydrochloric acid being reacted, cooling gets in the refrigerative pipeline again, produces neutralization reaction, has removed reaction heat in time, makes reaction become gentle, and side reaction reduces;
2, side reaction is inhibited, and under the identical situation of other technology of Glyphosate 62 IPA Salt synthetic, the yield of Glyphosate 62 IPA Salt has improved 1.2% (respectively doing three times MV), simultaneously aftertreatment is become easily, and the washing water yield reduces by 250 kilograms, has reduced production cost greatly.
3, effectively shift reaction is hot for the mixing tank of the graphite material of ripple packing mode and piece cellular type graphite cooler or piece cellular type glass cools device, reduces the severe of reaction, has improved the security of producing.
Description of drawings
Fig. 1 of Figure of description is a process flow diagram of the present invention.
Fig. 2 of Figure of description is the structural representation of the preceding feeding device of hydrolysis in the glyphosate production of the present invention's employing.
Reference numeral: 1 is that condensation reaction still, 2 is that hydrochloric acid scale tank, 3 is that flow director, 4 is that mixing tank, 5 is that water cooler, 6 is that TP, 7 is that hydrolytic reaction pot, 8 is that chilled brine import, 9 is that chilled brine exports.
Embodiment
Embodiment 1
Acid adding process in a kind of glyphosate production before the hydrolysis is characterized in that: comprise following process step:
A, with synthetic liquid of condensation reaction and mol ratio calculating separately the flow of hydrochloric acid according to glycocoll and hydrogenchloride, mix in the input mixer respectively by two pipelines;
B, the neutralizer that after mixing, obtains get into water cooler immediately, in reaction, take the reaction heat exchange out of reaction system, guarantee that water cooler material liquid outlet temperature is 30 ℃;
C, mix the neutralizer obtain and laggardly go into hydrolytic reaction pot and be hydrolyzed and make Glyphosate 62 IPA Salt through cooling off.
The glycocoll in the steps A of the present invention and the mol ratio of hydrogenchloride are 1:2.8.
Mixing tank in the steps A of the present invention is the mixing tank of ripple packing mode.
The filler of above-mentioned mixing tank is pottery or acrylic plastering.
The sheating material of above-mentioned mixing tank is graphite or acrylic plastering.
Water cooler among the step B of the present invention can be piece cellular type graphite cooler or piece cellular type glass cools device.
Water cooler of the present invention is to adopt chilled brine circulation cooling, and the temperature of chilled brine is-15 ℃.
Water cooler material liquid outlet among the step B of the present invention is provided with TP, according to outlet feed temperature control neutralizer flow.
Embodiment 2
Acid adding process in a kind of glyphosate production before the hydrolysis is characterized in that: comprise following process step:
A, with synthetic liquid of condensation reaction and mol ratio calculating separately the flow of hydrochloric acid according to glycocoll and hydrogenchloride, mix in the input mixer respectively by two pipelines;
B, the neutralizer that after mixing, obtains get into water cooler immediately, in reaction, take the reaction heat exchange out of reaction system, guarantee that water cooler material liquid outlet temperature is 45 ℃;
C, mix the neutralizer obtain and laggardly go into hydrolytic reaction pot and be hydrolyzed and make Glyphosate 62 IPA Salt through cooling off.
The glycocoll in the steps A of the present invention and the mol ratio of hydrogenchloride are 1:3.5.
Mixing tank in the steps A of the present invention is the mixing tank of ripple packing mode.
The filler of above-mentioned mixing tank is pottery or acrylic plastering.
The sheating material of above-mentioned mixing tank is graphite or acrylic plastering.
Water cooler among the step B of the present invention can be piece cellular type graphite cooler or piece cellular type glass cools device.
Water cooler of the present invention is to adopt chilled brine circulation cooling, and the temperature of chilled brine is-35 ℃.
Water cooler material liquid outlet among the step B of the present invention is provided with TP, according to outlet feed temperature control neutralizer flow.
Embodiment 3
Acid adding process in a kind of glyphosate production before the hydrolysis is characterized in that: comprise following process step:
A, with synthetic liquid of condensation reaction and mol ratio calculating separately the flow of hydrochloric acid according to glycocoll and hydrogenchloride, mix in the input mixer respectively by two pipelines;
B, the neutralizer that after mixing, obtains get into water cooler immediately, in reaction, take the reaction heat exchange out of reaction system, guarantee that water cooler material liquid outlet temperature is 35 ℃;
C, mix the neutralizer obtain and laggardly go into hydrolytic reaction pot and be hydrolyzed and make Glyphosate 62 IPA Salt through cooling off.
The glycocoll in the steps A of the present invention and the mol ratio of hydrogenchloride are 1:3.15.
Mixing tank in the steps A of the present invention is the mixing tank of ripple packing mode.
The filler of above-mentioned mixing tank is pottery or acrylic plastering.
The sheating material of above-mentioned mixing tank is graphite or acrylic plastering.
Water cooler among the step B of the present invention can be piece cellular type graphite cooler or piece cellular type glass cools device.
Water cooler of the present invention is to adopt chilled brine circulation cooling, and the temperature of chilled brine is-15 ℃.
Water cooler material liquid outlet among the step B of the present invention is provided with TP, according to outlet feed temperature control neutralizer flow.
Embodiment 4
Acid adding process in a kind of glyphosate production before the hydrolysis is characterized in that: comprise following process step:
A, with synthetic liquid of condensation reaction and mol ratio calculating separately the flow of hydrochloric acid according to glycocoll and hydrogenchloride, mix in the input mixer respectively by two pipelines;
B, the neutralizer that after mixing, obtains get into water cooler immediately, in reaction, take the reaction heat exchange out of reaction system, guarantee that water cooler material liquid outlet temperature is 40 ℃;
C, mix the neutralizer obtain and laggardly go into hydrolytic reaction pot and be hydrolyzed and make Glyphosate 62 IPA Salt through cooling off.
The glycocoll in the steps A of the present invention and the mol ratio of hydrogenchloride are 1:3.45.
Mixing tank in the steps A of the present invention is the mixing tank of ripple packing mode.
The filler of above-mentioned mixing tank is pottery or acrylic plastering.
The sheating material of above-mentioned mixing tank is graphite or acrylic plastering.
Water cooler among the step B of the present invention can be piece cellular type graphite cooler or piece cellular type piece cellular type glass cools device.
Water cooler of the present invention is to adopt chilled brine circulation cooling, and the temperature of chilled brine is-35 ℃.
Water cooler material liquid outlet among the step B of the present invention is provided with TP, according to outlet feed temperature control neutralizer flow.
Embodiment 5
In conjunction with Fig. 2: the feeding device in a kind of glyphosate production before the hydrolysis; Comprise condensation reaction still 1, hydrolytic reaction pot 7 and hydrochloric acid scale tank 2; It is characterized in that: through an end of the same mixing tank 4 of pipe connection, described pipeline is provided with flow director 3 respectively for condensation reaction still 1 and hydrochloric acid scale tank 2; The other end of described mixing tank 4 is connected with water cooler 5, and described water cooler 5 is connected with hydrolytic reaction pot 7 again.
Described mixing tank 4 is the mixing tank of ripple packing mode.
The filler of described mixing tank 4 is pottery or acrylic plastering.
The sheating material of described mixing tank 4 is graphite or acrylic plastering.
Described water cooler 5 is piece cellular type graphite cooler or piece cellular type glass cools device.
Described water cooler 5 lower ends are provided with chilled brine import 8, and the upper end is provided with chilled brine outlet 9.
Described water cooler 5 material liquid outlet places are provided with TP 6.

Claims (9)

1. the acid adding process before the hydrolysis in the glyphosate production is characterized in that: comprise following process step:
A, with synthetic liquid of condensation reaction and mol ratio calculating separately the flow of hydrochloric acid according to glycocoll and hydrogenchloride, mix in the input mixer respectively by two pipelines;
B, the neutralizer that after mixing, obtains get into water cooler immediately, in reaction, take the reaction heat exchange out of reaction system, guarantee that water cooler material liquid outlet temperature is equal to or less than the hydrolysis process temperature;
C, mix the neutralizer obtain and laggardly go into hydrolytic reaction pot and be hydrolyzed and make Glyphosate 62 IPA Salt through cooling off.
2. the acid adding process in a kind of glyphosate production according to claim 1 before the hydrolysis, it is characterized in that: the mol ratio at glycocoll described in the steps A and hydrogenchloride is 1:2.8~3.5.
3. the acid adding process in a kind of glyphosate production according to claim 1 before the hydrolysis is characterized in that: be the mixing tank of ripple packing mode at the mixing tank described in the steps A.
4. the acid adding process in a kind of glyphosate production according to claim 3 before the hydrolysis is characterized in that: the filler of the mixing tank of described ripple packing mode is pottery or acrylic plastering.
5. the acid adding process in a kind of glyphosate production according to claim 3 before the hydrolysis, it is characterized in that: the sheating material of the mixing tank of described ripple packing mode is graphite or acrylic plastering.
6. the acid adding process in a kind of glyphosate production according to claim 1 before the hydrolysis, it is characterized in that: at the water cooler described in the step B is piece cellular type graphite cooler or piece cellular type glass cools device.
7. according to the acid adding process before the hydrolysis in claim 1 or the 6 described a kind of glyphosate production, it is characterized in that: water cooler of the present invention is to adopt chilled brine circulation cooling.
8. the acid adding process in a kind of glyphosate production according to claim 1 before the hydrolysis, it is characterized in that: the water cooler material liquid outlet described in the step B is provided with TP.
9. the acid adding process in a kind of glyphosate production according to claim 1 before the hydrolysis, it is characterized in that: in the hydrolysis process temperature described in the step B is 45 ℃.
CN201110320115.5A 2011-10-20 2011-10-20 Process of adding acids prior to hydrolysis in glyphosate production Active CN102503978B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103739625A (en) * 2014-01-23 2014-04-23 四川省乐山市福华通达农药科技有限公司 Continuous hydrolysis process for preparing glyphosate by glycine method
CN103788127A (en) * 2014-01-23 2014-05-14 四川省乐山市福华通达农药科技有限公司 Continuous hydrolysis system for preparing glyphosate by glycine method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101993455A (en) * 2010-12-13 2011-03-30 四川省乐山市福华通达农药科技有限公司 Glyphosate synthesis process

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101993455A (en) * 2010-12-13 2011-03-30 四川省乐山市福华通达农药科技有限公司 Glyphosate synthesis process

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103739625A (en) * 2014-01-23 2014-04-23 四川省乐山市福华通达农药科技有限公司 Continuous hydrolysis process for preparing glyphosate by glycine method
CN103788127A (en) * 2014-01-23 2014-05-14 四川省乐山市福华通达农药科技有限公司 Continuous hydrolysis system for preparing glyphosate by glycine method
CN103739625B (en) * 2014-01-23 2017-01-11 四川省乐山市福华通达农药科技有限公司 Continuous hydrolysis process for preparing glyphosate by glycine method
CN103788127B (en) * 2014-01-23 2017-01-11 四川省乐山市福华通达农药科技有限公司 Continuous hydrolysis system for preparing glyphosate by glycine method

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Denomination of invention: Process of adding acids prior to hydrolysis in glyphosate production

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Pledgee: Chengdu Branch of China CITIC Bank Co.,Ltd.

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Denomination of invention: A process of adding acid before hydrolysis in glyphosate production

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Address after: 614803 Jinsu Town, Wutongqiao District, Leshan City, Sichuan Province

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