CN104944398A - Method for recycling glyphosate mother solution - Google Patents
Method for recycling glyphosate mother solution Download PDFInfo
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- CN104944398A CN104944398A CN201510365757.5A CN201510365757A CN104944398A CN 104944398 A CN104944398 A CN 104944398A CN 201510365757 A CN201510365757 A CN 201510365757A CN 104944398 A CN104944398 A CN 104944398A
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- glyphosate mother
- mother solution
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a method for recycling glyphosate mother solution, and belongs to the technical field of chemical engineering. The method comprises the following steps: producing glyphosate and glyphosate mother solution by a glycine method or an iminodiacetic acid method; concentrating the glyphosate mother solution; carrying out an oxidization treatment on the glyphosate mother solution concentrate; cooling and crystallizing the glyphosate mother solution oxidation solution, taking out the crystallized glyphosate mother solution oxidation solution and concentrating; concentrating the permeate to obtain a sodium chloride product, and reusing the distillate; adjusting the pH value of the concentrate to 3-4, and then carrying out a photocatalytic oxidation reaction; adjusting the pH value to obtain a disodium hydrogen phosphate product or a trisodium phosphate product. According to the method disclosed by the invention, the concentration treatment is carried out before the glyphosate mother solution is oxidized, thus reducing the content of chloride ions in the glyphosate mother solution, increasing the concentration of the reactant, and increasing the efficiency of the subsequent oxidization reaction; hydrogen peroxide photocatalytic oxidation is carried out on the concentrate, the reaction is thorough, the oxidability is better, the substances difficult to oxidize by oxygen-enriched wet oxidization can be oxidized, and the reaction conditions are moderate.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to glyphosate mother solution recoverying and utilizing method.
Background technology
Glyphosate is the pesticide species that global sales is maximum and rate of growth is the fastest because of its low toxicity, efficient, low residue, broad spectrum, and along with the succeeding in developing and to promote the use of and energy shortage causes sowing and the popularization of biofuel crop of genetically modified crops of glyphosate, the production for glyphosate provides new opportunity.
Glyphosate production mainly contains two kinds of synthesis modes, and one is iminodiacetic acid (salt) acid system, namely with diethanolamine or prussic acid for starting raw material, Meng Shan Dou Deng offshore company of the U.S. generally adopts this method; Another kind is alkyl esterification method, and most domestic enterprise adopts this method.Alkyl esterification method glyphosate production main raw material is paraformaldehyde (formaldehyde), Padil, dimethylphosphite, triethylamine, methyl alcohol, hydrochloric acid, wherein the depolymerization of paraformaldehyde take triethylamine as catalyzer, through depolymerization, addition, condensation, hydrolysis reaction, then, after desolvation methyl alcohol and excessive hydrochloric acid, glyphosate crystal is separated out.
The glyphosate mother solution obtained after glyphosate crystal adds the recovery that alkali carries out catalyst of triethylamine, obtain glyphosate alkaline mother liquor, its main component is sodium-chlor, glyphosate and reaction intermediate thereof and by product, its sodium chloride content 12-16%, COD30,000-70,000mg/L, Tp15,000-30,000mg/L.Treatment process is as more complicated in patent CN 103012474A electrocatalytic oxidation metallization processes; Sodium chloride content in mother liquor just reduces by CN101402652A, does not carry out effective resource reclaim; CN103864040A carries out atmospheric oxidation, and efficiency is low, the inefficient problem of secondary oxidation, Btu utilization rate variance, because heat of reaction is greater than the activation energy needed for reaction, and generate energy Accumulation Phenomenon, and need noble metal catalyst.
Summary of the invention
For prior art Problems existing, the object of the invention is to design the technical scheme that glyphosate mother solution recoverying and utilizing method is provided.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that comprising following processing step:
1) glyphosate and glyphosate mother solution is obtained with glycine method, the production of iminodiacetic acid (salt) acid system;
2) glyphosate mother solution is concentrated, obtain glyphosate mother solution concentrated solution;
3) glyphosate mother solution concentrated solution is carried out oxide treatment, obtain glyphosate mother solution oxidation solution;
4) glyphosate mother solution oxidation solution is carried out decrease temperature crystalline and obtain phosphate product, the glyphosate mother solution oxidation solution taken out after crystallization concentrates, and obtains concentrated solution and permeate;
5) permeate obtains sodium-chlor product through concentrated, and distillate carries out reuse;
6) adjust concentrated solution pH value to 3 ~ 4, then add hydrogen peroxide and catalyzer carries out photocatalysis oxidation reaction under ultraviolet;
7) react end and add sodium hydroxide adjustment pH value to 9 ± 0.5 or 12 ± 0.5, when PH is 9, return catalytic wet oxidation liquid in the lump crystallisation by cooling or separately crystallisation by cooling obtain Sodium phosphate dibasic product, when PH is 12, the independent crystallisation by cooling of Ultraviolet Oxidation liquid obtains tertiary sodium phosphate product.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that described step 2) glyphosate mother solution is concentrated into COD is greater than 50,000mg/L, be preferably COD and be greater than 60,000mg/L, Tp is greater than 30,000mg/L, is preferably greater than 40,000mg/L.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that by glyphosate mother solution, air and oxygen mix in described step 3), and at temperature 220 ~ 260 DEG C, reaction 30 ~ 60min, obtains glyphosate mother solution oxidation solution.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that described step 4) glyphosate mother liquor oxidation solution is cooled to 0 ~ 10 DEG C and carries out crystallization.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that adopting nanofiltration membrane to concentrate in described step 4).
Described glyphosate mother solution recoverying and utilizing method, is characterized in that adopting mechanical vapor recompression technology or multiple-effect evaporation technology to concentrate in described step 5).
Described glyphosate mother solution recoverying and utilizing method, to is characterized in that in described step 6) that hydrogen peroxide consumes concentrated solution 100 ~ 150mg/L COD per ton amount by 1L hydrogen peroxide and adds.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that in described step 6), catalyzer is ferrous salt or mantoquita, and during interpolation, control concentrated solution ferrous ions and copper ion concentration are 50 ~ 200mg/L.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that reaction times 5 ~ 48h in described step 6), is preferably 20 ~ 40h; Temperature of reaction 20 ~ 70 DEG C, is preferably 30 ~ 60 DEG C; UV-light 180 ~ 260nm, is preferably 200 ~ 240nm.
Described glyphosate mother solution recoverying and utilizing method, is characterized in that the mass ratio of described glyphosate mother solution and air is 80:12 ~ 16, and regulates content of oxygen in air to be 21 ~ 50% by adding liquid oxygen.
Above-mentioned glyphosate mother solution recoverying and utilizing method, reasonable in design, carry out concentration before glyphosate mother solution oxidation, reduce the content of chlorion in glyphosate mother solution, improve the concentration of reactant, improve the efficiency of subsequent oxidation reaction; Concentrated solution carries out hydrogen peroxide photochemical catalytic oxidation, and thoroughly, oxidisability is better in reaction, and oxygen enrichment wet oxidation can be difficult to the material be oxidized, be oxidized, reaction conditions is gentle.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
1) glyphosate and glyphosate mother solution is obtained with glycine method production;
2) glyphosate mother solution is concentrated into COD 60,000mg/L, Tp 40,000mg/L, obtains glyphosate mother solution concentrated solution;
3) by the glyphosate mother solution after concentrated and pressurized air in mass ratio 80:14 mix, and be 40% by oxygen content in interpolation liquid oxygen adjustment pressurized air, at temperature 240 DEG C, react 30min, obtain glyphosate mother solution oxidation solution;
4) glyphosate mother solution oxidation solution is cooled to 5 DEG C to carry out crystallization and obtain phosphate product, takes out the glyphosate mother solution oxidation solution after crystallization and adopt nanofiltration membrane to concentrate, obtain concentrated solution and permeate;
5) permeate adopts mechanical vapor recompression technology or multiple-effect evaporation technology to carry out concentratedly obtaining sodium-chlor product, and distillate carries out reuse;
6) adjust concentrated solution pH value to 3.5, then add hydrogen peroxide and catalyzer carries out photocatalysis oxidation reaction 20h under temperature 50 C, 200nm UV-light, wherein hydrogen peroxide consumes concentrated solution 120mg/L COD per ton amount by 1L hydrogen peroxide and adds; Catalyzer is ferrous salt or mantoquita, and control concentrated solution ferrous ions and copper ion concentration are 100mg/L;
7) react end and add sodium hydroxide adjustment pH value to 9 ± 0.5 or 12 ± 0.5, when PH is 9, return catalytic wet oxidation liquid in the lump crystallisation by cooling or separately crystallisation by cooling obtain Sodium phosphate dibasic product, when PH is 12, the independent crystallisation by cooling of Ultraviolet Oxidation liquid obtains tertiary sodium phosphate product.
Embodiment 2
1) glyphosate and glyphosate mother solution is obtained with glycine method production;
2) glyphosate mother solution is concentrated into COD 50,000mg/L, Tp 30,000mg/L, obtains glyphosate mother solution concentrated solution;
3) by the glyphosate mother solution after concentrated and pressurized air in mass ratio 80:12 mix, and be 30% by oxygen content in interpolation liquid oxygen adjustment pressurized air, at temperature 220 DEG C, react 50min, obtain glyphosate mother solution oxidation solution;
4) glyphosate mother solution oxidation solution is cooled to 0 DEG C to carry out crystallization and obtain phosphate product, takes out the glyphosate mother solution oxidation solution after crystallization and adopt nanofiltration membrane to concentrate, obtain concentrated solution and permeate;
5) permeate adopts mechanical vapor recompression technology or multiple-effect evaporation technology to carry out concentratedly obtaining sodium-chlor product, and distillate carries out reuse;
6) adjust concentrated solution pH value to 3, then add hydrogen peroxide and catalyzer carries out photocatalysis oxidation reaction 5h under temperature 70 C, 180nm UV-light, wherein hydrogen peroxide consumes concentrated solution 100mg/L COD per ton amount by 1L hydrogen peroxide and adds; Catalyzer is ferrous salt or mantoquita, and control concentrated solution ferrous ions and copper ion concentration are 200mg/L;
7) react end and add sodium hydroxide adjustment pH value to 9 ± 0.5 or 12 ± 0.5, when PH is 9, return catalytic wet oxidation liquid in the lump crystallisation by cooling or separately crystallisation by cooling obtain Sodium phosphate dibasic product, when PH is 12, the independent crystallisation by cooling of Ultraviolet Oxidation liquid obtains tertiary sodium phosphate product.
Embodiment 3
1) glyphosate and glyphosate mother solution is obtained with the production of iminodiacetic acid (salt) acid system;
2) glyphosate mother solution is concentrated into COD 60,000mg/L, Tp 50,000mg/L, obtains glyphosate mother solution concentrated solution;
3) by the glyphosate mother solution after concentrated and pressurized air in mass ratio 80:16 mix, and be 50% by oxygen content in interpolation liquid oxygen adjustment pressurized air, at temperature 260 DEG C, react 30min, obtain glyphosate mother solution oxidation solution;
4) glyphosate mother solution oxidation solution is cooled to 10 DEG C to carry out crystallization and obtain phosphate product, takes out the glyphosate mother solution oxidation solution after crystallization and adopt nanofiltration membrane to concentrate, obtain concentrated solution and permeate;
5) permeate adopts mechanical vapor recompression technology or multiple-effect evaporation technology to carry out concentratedly obtaining sodium-chlor product, and distillate carries out reuse;
6) adjust concentrated solution pH value to 4, then add hydrogen peroxide and catalyzer carries out photocatalysis oxidation reaction 48h under temperature 20 DEG C, 260nm UV-light, wherein hydrogen peroxide consumes concentrated solution 100mg/L COD per ton amount by 1L hydrogen peroxide and adds; Catalyzer is ferrous salt or mantoquita, and control concentrated solution ferrous ions and copper ion concentration are 50mg/L;
7) react end and add sodium hydroxide adjustment pH value to 9 ± 0.5 or 12 ± 0.5, when PH is 9, return catalytic wet oxidation liquid in the lump crystallisation by cooling or separately crystallisation by cooling obtain Sodium phosphate dibasic product, when PH is 12, the independent crystallisation by cooling of Ultraviolet Oxidation liquid obtains tertiary sodium phosphate product.
Claims (10)
1. glyphosate mother solution recoverying and utilizing method, is characterized in that comprising following processing step:
1) glyphosate and glyphosate mother solution is obtained with glycine method, the production of iminodiacetic acid (salt) acid system;
2) glyphosate mother solution is concentrated, obtain glyphosate mother solution concentrated solution;
3) glyphosate mother solution concentrated solution is carried out oxide treatment, obtain glyphosate mother solution oxidation solution;
4) glyphosate mother solution oxidation solution is carried out decrease temperature crystalline and obtain phosphate product, the glyphosate mother solution oxidation solution taken out after crystallization concentrates, and obtains concentrated solution and permeate;
5) permeate obtains sodium-chlor product through concentrated, and distillate carries out reuse;
6) adjust concentrated solution pH value to 3 ~ 4, then add hydrogen peroxide and catalyzer carries out photocatalysis oxidation reaction under ultraviolet;
7) react end and add sodium hydroxide adjustment pH value to 9 ± 0.5 or 12 ± 0.5, when PH is 9, return catalytic wet oxidation liquid in the lump crystallisation by cooling or separately crystallisation by cooling obtain Sodium phosphate dibasic product, when PH is 12, the independent crystallisation by cooling of Ultraviolet Oxidation liquid obtains tertiary sodium phosphate product.
2. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that described step 2) glyphosate mother solution is concentrated into COD is greater than 50,000mg/L, be preferably COD and be greater than 60,000mg/L, Tp is greater than 30,000mg/L, is preferably greater than 40,000mg/L.
3. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that by glyphosate mother solution, air and oxygen mix in described step 3), and at temperature 220 ~ 260 DEG C, reaction 30 ~ 60min, obtains glyphosate mother solution oxidation solution.
4. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that described step 4) glyphosate mother liquor oxidation solution is cooled to 0 ~ 10 DEG C and carries out crystallization.
5. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that adopting nanofiltration membrane to concentrate in described step 4).
6. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that adopting mechanical vapor recompression technology or multiple-effect evaporation technology to concentrate in described step 5).
7. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, to is characterized in that in described step 6) that hydrogen peroxide consumes concentrated solution 100 ~ 150mg/L COD per ton amount by 1L hydrogen peroxide and adds.
8. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that in described step 6), catalyzer is ferrous salt or mantoquita, and during interpolation, control concentrated solution ferrous ions and copper ion concentration are 50 ~ 200mg/L.
9. glyphosate mother solution recoverying and utilizing method as claimed in claim 1, is characterized in that reaction times 5 ~ 48h in described step 6), is preferably 20 ~ 40h; Temperature of reaction 20 ~ 70 DEG C, is preferably 30 ~ 60 DEG C; UV-light 180 ~ 260nm, is preferably 200 ~ 240nm.
10. glyphosate mother solution recoverying and utilizing method as claimed in claim 3, is characterized in that the mass ratio of described glyphosate mother solution and air is 80:12 ~ 16, and regulates content of oxygen in air to be 21 ~ 50% by adding liquid oxygen.
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| CN201510365757.5A CN104944398B (en) | 2015-06-29 | 2015-06-29 | Glyphosate mother solution recoverying and utilizing method |
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| CN201510365757.5A CN104944398B (en) | 2015-06-29 | 2015-06-29 | Glyphosate mother solution recoverying and utilizing method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330688A (en) * | 2015-11-26 | 2016-02-17 | 浙江工业大学 | Method for preparing glyphosate by utilizing visible light to catalyze and oxidize phosphonomethyl iminodiacetic acid |
| CN105692960A (en) * | 2016-03-04 | 2016-06-22 | 安徽国星生物化学有限公司 | Treatment method for glyphosate mother liquor |
| CN106044731A (en) * | 2016-08-13 | 2016-10-26 | 安徽东至广信农化有限公司 | Method for preparing disodium hydrogen phosphate based on glyphosate mother solution |
| CN107162278A (en) * | 2017-07-13 | 2017-09-15 | 成都美富特膜科技有限公司 | A kind of recycling PMIDA produces the handling process of waste water |
| CN108689392A (en) * | 2018-07-09 | 2018-10-23 | 江西金龙化工有限公司 | A kind of glyphosate three wastes integrated conduct method |
| CN114933289A (en) * | 2022-06-22 | 2022-08-23 | 四川福思达生物技术开发有限责任公司 | Co-production process for glyphosate and ferric phosphate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330688A (en) * | 2015-11-26 | 2016-02-17 | 浙江工业大学 | Method for preparing glyphosate by utilizing visible light to catalyze and oxidize phosphonomethyl iminodiacetic acid |
| CN105330688B (en) * | 2015-11-26 | 2017-08-22 | 浙江工业大学 | Utilize the method for visible light catalytic oxidation preparing glyphosate from N-phosphonomethyl aminodiacetic acid |
| CN105692960A (en) * | 2016-03-04 | 2016-06-22 | 安徽国星生物化学有限公司 | Treatment method for glyphosate mother liquor |
| CN106044731A (en) * | 2016-08-13 | 2016-10-26 | 安徽东至广信农化有限公司 | Method for preparing disodium hydrogen phosphate based on glyphosate mother solution |
| CN107162278A (en) * | 2017-07-13 | 2017-09-15 | 成都美富特膜科技有限公司 | A kind of recycling PMIDA produces the handling process of waste water |
| CN108689392A (en) * | 2018-07-09 | 2018-10-23 | 江西金龙化工有限公司 | A kind of glyphosate three wastes integrated conduct method |
| CN108689392B (en) * | 2018-07-09 | 2019-10-25 | 江西金龙化工有限公司 | A kind of glyphosate three wastes integrated conduct method |
| CN114933289A (en) * | 2022-06-22 | 2022-08-23 | 四川福思达生物技术开发有限责任公司 | Co-production process for glyphosate and ferric phosphate |
| CN114933289B (en) * | 2022-06-22 | 2024-03-15 | 四川福思达生物技术开发有限责任公司 | Co-production process for glyphosate and ferric phosphate |
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Effective date of registration: 20160217 Address after: 333332 Jiangxi city of Jingdezhen province Leping City Tashan Industrial Park Applicant after: JIANGXI JINLONG CHEMICAL CO., LTD. Applicant after: Zhejiang Jinfanda Biochemical Co., Ltd. Address before: 333332 Jiangxi city of Jingdezhen province Leping City Tashan Industrial Park Applicant before: JIANGXI JINLONG CHEMICAL CO., LTD. |
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