CN108997086A - The purifying process of glyphosate by using glycine by-product dimethoxym ethane - Google Patents
The purifying process of glyphosate by using glycine by-product dimethoxym ethane Download PDFInfo
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- CN108997086A CN108997086A CN201811009483.6A CN201811009483A CN108997086A CN 108997086 A CN108997086 A CN 108997086A CN 201811009483 A CN201811009483 A CN 201811009483A CN 108997086 A CN108997086 A CN 108997086A
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- CN
- China
- Prior art keywords
- glyphosate
- dimethoxym ethane
- product
- chloromethanes
- sodium hydroxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/12—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids
- C07C29/124—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids of halides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of purifying process of glyphosate by using glycine by-product dimethoxym ethane, then carry out dimethoxym ethane rectification working process to the sodium hydroxide solution of glyphosate solution addition more amount so that substitution reaction occurs for sodium hydroxide and chloromethanes.The concentration range of sodium hydroxide liquid alkaline is 32% ~ 40%.Technical process of the invention is simple, and most chloromethanes in system can be removed by only increasing alkali number, does not influence system and stablizes, harmless to equipment.
Description
Technical field
The present invention relates to a kind of methods of purification of glyphosate production byproduct.
Background technique
Glyphosate (N- (phosphonomethyl) glycine) is steriland herbicide after the bud of one kind efficiently, less toxic, safe, to more
The prevention and treatment of the deep root malignant weed of year life is very effective, has good bioactivity, belongs to amino acid derivativges, be to apply at present
One of most commonly used herbicide.
Glyphosate production technique mainly has glycine method and iminodiacetic acid (salt) acid system, and glycine method mainly produces at home.
Final products glyphosate is obtained by hydrolysis of ester group in glyphosate by using glycine production process, and reaction is in certain temperature, acid item
It is carried out under part, under this condition, the carbon on the methoxyl group (methanol) that the chloride ion meeting attack hydrolysis of ester group in hydrochloric acid obtains, generates chlorine
Methane.Chloromethanes low boiling point, it is volatile, but simultaneously chloromethanes in water with have certain solubility in methanol, reacting
Code insurance stays in system in the middle part of journey.It is steamed in last handling process with dimethoxym ethane, affects the purity of dimethoxym ethane, simultaneously because first
The presence of chloromethanes in acetal, after sealed package under transportational process, especially hot conditions, chloromethanes can expanded by heating, make
There is swollen bucket phenomenon in pail pack, and there are biggish security risks.
Summary of the invention
Goal of the invention: the present invention provides a kind of methods easy-to-use in production, do not change original technology controlling and process item
Part merely adds the amount of one of raw material, and most of chloromethanes in removing system does not influence system and stablizes, lossless to equipment
The purifying process of harmful glyphosate by using glycine by-product dimethoxym ethane.
Technical solution:
Liquid alkaline will be added in solution containing methanol, dimethoxym ethane and a small amount of chloromethanes, continuously into dimethoxym ethane rectifying column, collects and steam
Dimethoxym ethane analyzes the content of wherein chloromethanes, dimethoxym ethane.Raffinate again through methanol rectifying tower collect methanol after, remaining alkaline residue
In, aqueous, a small amount of methanol, alkali, salt etc..
Reaction principle:
The foundation of the reaction is above-mentioned reaction, is typical bimolecular nucleophilic subsititution.Reaction rate=k of the reaction
[CH3Cl][HO-]mol·L-1S-1, reaction rate and the concentration of substrate and nucleopilic reagent are all directly proportional, and it is dynamic to show as second order reaction
Mechanics.In the case where that cannot change reaction substrate chloromethanes concentration, the concentration for increasing alkali can also accelerate reaction rate.
Dimethoxym ethane is easy to decompose under acidic environment, and property is stablized under alkaline environment, will not decompose.
The control of reaction condition and feeding quantity:
In above scheme, the concentration range 10% ~ 40% of liquid alkaline, preferably 32% ~ 40%；It is preferred that sodium hydroxide, pico- excessive, neutralization can
It after potential acid waste liquid can continue that substitution reaction occurs.Moreover, in residual night composition be easy carry out post-processing, expense of raw materials compared with
It is low.
The additional amount and the extent of reaction of liquid alkaline have direct relation, and increasing additional amount can accelerate to react, and pH scope control is 12
More than, preferably 13-14, chloromethanes almost replaces at this time, and the temperature heated is without too high, and 45-55 DEG C,
Energy consumption is lower.
The utility model has the advantages that
It is an advantage of the present invention that original process process, which without change, only increases caustic dosage, to remove the chloromethanes in system, no
Influence system is stablized, harmless to equipment.
Compared with prior art, the chloromethanes after improvement in dimethoxym ethane can be substantially reduced, and the content of chloromethanes is by original
8% be down to 1% or less.Dimethoxym ethane content is improved by original 80% to 90% or more.
Specific embodiment
In the three-necked flask equipped with condenser, feed liquid 200g before dimethoxym ethane rectifying in production of reborning, wherein chloromethanes content
It is 0.5%, dimethoxym ethane content is 8%, methanol content 40%, aqueous 51.5%, chloride ion content 180ppm.It is added thereto
40%NaOH adjusts pH to 14, and stirring is warming up to 50 DEG C, and sampling analysis chloromethanes content is 0 after half an hour, and dimethoxym ethane content is
7.85%, methanol content 39.5%, aqueous 52.0%, chloride ion content 2985ppm.
Claims (3)
1. a kind of purifying process of glyphosate by using glycine by-product dimethoxym ethane, by-product chlorine is contained in reaction product glyphosate solution
Methane, it is characterised in that: in the last handling process of glyphosate solution have dimethoxym ethane rectification working process, dimethoxym ethane rectification working process it
Before, to the sodium hydroxide solution of glyphosate solution addition more amount, the molal quantity of sodium hydroxide is higher than rubbing for by-product chloromethanes
That number, so that substitution reaction occurs for sodium hydroxide and chloromethanes.
2. the purifying process of sour method glyphosate by-product dimethoxym ethane as described in claim 1, it is characterised in that: distillation residual liquid is again
Methanol is collected through methanol rectifying tower.
3. the purifying process of sour method glyphosate by-product dimethoxym ethane as described in claim 1, it is characterised in that: caustic lye of soda
The concentration range of alkali is 32% ~ 40%, and after liquid alkaline is added, the pH scope control of solution is in 13-14, and heating and temperature control is in 45-55
℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811009483.6A CN108997086A (en) | 2018-08-31 | 2018-08-31 | The purifying process of glyphosate by using glycine by-product dimethoxym ethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811009483.6A CN108997086A (en) | 2018-08-31 | 2018-08-31 | The purifying process of glyphosate by using glycine by-product dimethoxym ethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108997086A true CN108997086A (en) | 2018-12-14 |
Family
ID=64590625
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811009483.6A Pending CN108997086A (en) | 2018-08-31 | 2018-08-31 | The purifying process of glyphosate by using glycine by-product dimethoxym ethane |
Country Status (1)
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| CN (1) | CN108997086A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307289A (en) * | 2021-08-02 | 2021-08-27 | 清大国华环境集团股份有限公司 | Resource recycling method for hazardous waste containing brominated alkanes |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR870001466B1 (en) * | 1984-12-28 | 1987-08-12 | 몬산토 캄파니 | Process for the preparation of glyphosate and glyphosate derivatives |
| CN103736384A (en) * | 2014-01-27 | 2014-04-23 | 山东潍坊润丰化工股份有限公司 | Treatment process of glyphosate hydrolyzing tail gas |
| CN104190104A (en) * | 2014-08-27 | 2014-12-10 | 江苏凯茂石化科技有限公司 | Process equipment and method for refining dimethoxymethane in byproducts produced in production of glyphosate by glycine method |
| CN108404637A (en) * | 2018-04-20 | 2018-08-17 | 湖北泰盛化工有限公司 | A kind of alkyl esterification method glyphosate hydrolyzing tail gas reclaimer and technique |
| CN108409532A (en) * | 2018-04-20 | 2018-08-17 | 湖北泰盛化工有限公司 | A kind of alkyl esterification method production glyphosate solvent recovering system and technique based on B-grade condensation |
-
2018
- 2018-08-31 CN CN201811009483.6A patent/CN108997086A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR870001466B1 (en) * | 1984-12-28 | 1987-08-12 | 몬산토 캄파니 | Process for the preparation of glyphosate and glyphosate derivatives |
| CN103736384A (en) * | 2014-01-27 | 2014-04-23 | 山东潍坊润丰化工股份有限公司 | Treatment process of glyphosate hydrolyzing tail gas |
| CN104190104A (en) * | 2014-08-27 | 2014-12-10 | 江苏凯茂石化科技有限公司 | Process equipment and method for refining dimethoxymethane in byproducts produced in production of glyphosate by glycine method |
| CN108404637A (en) * | 2018-04-20 | 2018-08-17 | 湖北泰盛化工有限公司 | A kind of alkyl esterification method glyphosate hydrolyzing tail gas reclaimer and technique |
| CN108409532A (en) * | 2018-04-20 | 2018-08-17 | 湖北泰盛化工有限公司 | A kind of alkyl esterification method production glyphosate solvent recovering system and technique based on B-grade condensation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113307289A (en) * | 2021-08-02 | 2021-08-27 | 清大国华环境集团股份有限公司 | Resource recycling method for hazardous waste containing brominated alkanes |
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