CN101570547B - Method for processing glyphosate mother liquor - Google Patents
Method for processing glyphosate mother liquor Download PDFInfo
- Publication number
- CN101570547B CN101570547B CN2009101155259A CN200910115525A CN101570547B CN 101570547 B CN101570547 B CN 101570547B CN 2009101155259 A CN2009101155259 A CN 2009101155259A CN 200910115525 A CN200910115525 A CN 200910115525A CN 101570547 B CN101570547 B CN 101570547B
- Authority
- CN
- China
- Prior art keywords
- glyphosate
- mother liquor
- triethylamine
- solution
- ipa salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 40
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 40
- 239000012452 mother liquor Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 21
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- PDYXIVPKOMYDOK-UHFFFAOYSA-N Glyphosate-monoammonium Chemical compound [NH4+].OC(=O)CNCP(O)([O-])=O PDYXIVPKOMYDOK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 150000003839 salts Chemical class 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000010413 mother solution Substances 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- 239000011780 sodium chloride Substances 0.000 abstract 1
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 6
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 3
- 239000004471 Glycine Substances 0.000 description 2
- YWICANUUQPYHOW-UHFFFAOYSA-M sodium;2-(phosphonomethylamino)acetate Chemical compound [Na+].OP(O)(=O)CNCC([O-])=O YWICANUUQPYHOW-UHFFFAOYSA-M 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000009333 weeding Methods 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
A method for processing glyphosate mother liquor, comprising the following steps: (1) adding triethylamine as extractant to glyphosate acid mother liquor, mixing evenly, regulating the PH value of theobtained solution to 8-10 by adding alkali for standing and layering, separating the solution to obtain triethylamine salt solution on the upper layer and glyphosate concentrated mother liquor on the lower layer which has 6%-8% of glyphosate; (2) regulating the PH value of glyphosate concentrated mother liquor obtained in step (1) to about 11 by adding alkali, distilling the solution and obtaining a small quantity of triethylamine and a residual mother liquor which can be used to prepare 30% glyphosate ammonium water solution. The invention has the advantages that the operation of the invention is simple and the cost is low, the content of the obtained glyphosate mother liquor reaches 6-8% and sodium chloride in the concentrated mother liquor is few which can be used to prepare 30% glyphosate ammonium water solution.
Description
Technical field
The present invention relates to a kind of treatment process of glyphosate mother solution, relate in particular to a kind of treatment process of glyphosate by using glycine mother liquor.
Background technology
Glyphosate 62 IPA Salt is a most popular weedicide on the world market, has characteristics such as efficient, low toxicity and noresidue, and China is the maximum production base of Glyphosate 62 IPA Salt at present.Glyphosate production mainly contains two kinds of methods, and the one, the IDA method, offshore company generally adopts this method, another kind of glycine method, domestic big multiple enterprises adopts this method, and production capacity is above 300,000 tons/year.Can produce a large amount of Cl that contains during preparing glyphosate by glycin method
-Acid mother liquid, the main method of domestic most glyphosate production business processes mother liquors is: in acid mother liquor, add 30% sodium hydroxide solution, regulate pH value 10-12; Standing demix; Reclaim the upper strata catalyst of triethylamine, the residue alkali liquor is after concentrate, removing part sodium-chlor; Get the concentrated mother liquor that Glyphosate 62 IPA Salt content is about 2-3%, be used to prepare 10% sodium glyphosate aqua.Because contain a large amount of sodium-chlor in the 10% sodium glyphosate aqua, weeding ratio is low in the use, environmental pollution is serious, and usage quantity reduces year by year, and will behind 1-2, eliminate out weedicide market.
Summary of the invention
The object of the invention is to provide a kind of production cost low, the mother liquor processing method that the Glyphosate 62 IPA Salt utility value is high, and this method reaction conditions is gentle, and glyphosate mother solution pollutes little after treatment, and Glyphosate 62 IPA Salt content is high in the recovery.
The present invention is achieved in that and it is characterized in that process step is:
(1) press extraction agent triethylamine and glyphosphonic acid aqueous mother liquor weight ratio 1: 2-5 mixes, and under temperature 30-60 ℃, in mother liquor, adds triethylamine; After stirring; Add alkali and regulate PH to 8-10, standing demix separates the upper strata, back and gets triethylamine salt solution; Lower floor gets the dense mother liquor of Glyphosate 62 IPA Salt, and its Glyphosate 62 IPA Salt content is 6%-8%;
(2) add alkali behind the dense mother liquor of Glyphosate 62 IPA Salt that step (1) is obtained, transfer pH, distill out triethylamine, remain mother liquor and be used to prepare 30% ammonium glyphosate aqua to 11-12;
(3) with the triethylamine salt solution that obtains in the step (1), add alkali and transfer pH value 10-12, standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of Glyphosate 62 IPA Salt, and a small amount of triethylamine is told in lower floor's rectifying, gets into Sewage treatment systems.
Alkali of the present invention is sodium hydroxide, and its concentration is 30%-99%.
Advantage of the present invention is: 1, use this method simple to operate, cost is low; The catalyzer of using in extraction agent that uses in the process and the reaction all is a triethylamine, reclaims easy.2, the glyphosate mother solution content that obtains reaches 6-8%, and sodium-chlor is few in the dense mother liquor, can be used for preparing 30% ammonium glyphosate aqua.
Embodiment
Embodiment one
Get adding triethylamine 100g in the 400g glyphosphonic acid mother liquor, after stirring, add 98% sodium hydroxide 25g, regulate PH to 9.0, standing demix, upper strata triethylamine salt solution weight 418.5g, the heavy 106.5g of the dense mother liquor of lower floor's Glyphosate 62 IPA Salt, Glyphosate 62 IPA Salt content is 7.25%;
Triethylamine salt solution adds 30% sodium hydroxide accent pH to 12, and standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of Glyphosate 62 IPA Salt, and a small amount of triethylamine is told in lower floor's rectifying, gets into Sewage treatment systems.
The dense mother liquor of Glyphosate 62 IPA Salt adds 98% sodium hydroxide accent pH to 11, and rectifying goes out a spot of triethylamine, the heavy 108.0g of residue mother liquor, and Glyphosate 62 IPA Salt content 7.15% is used to prepare 30% ammonium glyphosate aqua.
Embodiment two
Get adding triethylamine 100g in the 400g glyphosphonic acid mother liquor, after stirring, add 30% sodium hydroxide 90g, regulate PH to 9.3, standing demix, upper strata triethylamine salt solution weight 474.5g, the heavy 115.5g of the dense mother liquor of lower floor's Glyphosate 62 IPA Salt, Glyphosate 62 IPA Salt content is 6.65%;
Upper strata triethylamine salt solution adds 30% sodium hydroxide accent pH to 12, and standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of Glyphosate 62 IPA Salt, and a small amount of triethylamine is told in lower floor's rectifying, gets into Sewage treatment systems.
The dense mother liquor of Glyphosate 62 IPA Salt adds 30% sodium hydroxide accent pH to 11, and rectifying goes out a spot of triethylamine, the heavy 126.5g of residue mother liquor, and Glyphosate 62 IPA Salt content 6.08% is used to prepare 30% ammonium glyphosate aqua.
Claims (2)
1. the treatment process of a glyphosate mother solution is characterized in that process method step is:
(1) press extraction agent triethylamine and glyphosphonic acid aqueous mother liquor weight ratio 1: 2-5 mixes, and under temperature 30-60 ℃, in mother liquor, adds triethylamine; After stirring; Add alkali and regulate pH to 8-10, standing demix separates the upper strata, back and gets triethylamine salt solution; Lower floor gets the dense mother liquor of Glyphosate 62 IPA Salt, and its Glyphosate 62 IPA Salt content is 6%-8%;
(2) add alkali behind the dense mother liquor of Glyphosate 62 IPA Salt that step (1) is obtained, transfer pH, distill out triethylamine, remain mother liquor and be used to prepare 30% ammonium glyphosate aqua to 11-12;
(3) with the triethylamine salt solution that obtains in the step (1), add adjusting PH with base value 10-12, standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of Glyphosate 62 IPA Salt, and a small amount of triethylamine is told in lower floor's rectifying, gets into Sewage treatment systems.
2. the treatment process of glyphosate mother solution according to claim 1 is characterized in that alkali is sodium hydroxide, and its concentration is 30%-99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101155259A CN101570547B (en) | 2009-06-16 | 2009-06-16 | Method for processing glyphosate mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101155259A CN101570547B (en) | 2009-06-16 | 2009-06-16 | Method for processing glyphosate mother liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101570547A CN101570547A (en) | 2009-11-04 |
| CN101570547B true CN101570547B (en) | 2012-07-04 |
Family
ID=41230042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101155259A Expired - Fee Related CN101570547B (en) | 2009-06-16 | 2009-06-16 | Method for processing glyphosate mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101570547B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079757B (en) * | 2010-12-13 | 2013-03-27 | 四川省乐山市福华通达农药科技有限公司 | Process for extracting glyphosate from acid mother liquor |
| CN103665035B (en) * | 2013-12-11 | 2016-08-17 | 鹤壁市农林制药有限公司 | A kind of processing method of glyphosate mother solution |
| CN110396048A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The comprehensive recovering process of glyphosate mother solution |
| CN110396047A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The recoverying and utilizing method of glyphosate mother solution |
| CN110393188A (en) * | 2018-04-25 | 2019-11-01 | 刘德亮 | The purification process technique of glyphosate mother solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001008480A1 (en) * | 1999-07-29 | 2001-02-08 | Monsanto Technology Llc | Process for making ammonium glyphosate powder |
| CN1648131A (en) * | 2004-12-23 | 2005-08-03 | 浙江新安化工集团股份有限公司 | Process for treating glyphosate mother liquid |
| CN101691382A (en) * | 2009-10-15 | 2010-04-07 | 山东潍坊润丰化工有限公司 | Method for recycling glyphosate from glyphosate mother liquor of IDA method |
| CN101830927A (en) * | 2009-03-09 | 2010-09-15 | 刘鑫峰 | Recycling method of glyphosate mother liquor |
-
2009
- 2009-06-16 CN CN2009101155259A patent/CN101570547B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001008480A1 (en) * | 1999-07-29 | 2001-02-08 | Monsanto Technology Llc | Process for making ammonium glyphosate powder |
| CN1648131A (en) * | 2004-12-23 | 2005-08-03 | 浙江新安化工集团股份有限公司 | Process for treating glyphosate mother liquid |
| CN101830927A (en) * | 2009-03-09 | 2010-09-15 | 刘鑫峰 | Recycling method of glyphosate mother liquor |
| CN101691382A (en) * | 2009-10-15 | 2010-04-07 | 山东潍坊润丰化工有限公司 | Method for recycling glyphosate from glyphosate mother liquor of IDA method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101570547A (en) | 2009-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101570547B (en) | Method for processing glyphosate mother liquor | |
| US11008638B2 (en) | Method for separating nickel and cobalt from a solution | |
| CN105129893A (en) | High efficiency extractant and extraction method of H-acid mother liquor | |
| CN103752158B (en) | A kind of processing method of glyphosate hydrolysis tail gas | |
| CN101830948A (en) | Method for preparing tea saponin by using tea seed degreased dreg | |
| CN104451770B (en) | Combined resource utilization method and device of brownification waste liquid and microetching waste liquid | |
| CN1830762A (en) | Method of continuously preparing potassium dihydrogen phosphate | |
| CN107502747A (en) | It is a kind of with microemulsion from vanadium wastewater extracting vanadium method | |
| CN104532022A (en) | Technological method of full load fractional extracting and separating rare earths | |
| CN101307002B (en) | Recovery method of triethylamine in glyphosate mother liquid | |
| CN103304423A (en) | Method for recovering triethylamine from glyphosate material | |
| CN103253689B (en) | The method of lithium, magnesium is extracted from salt lake brine | |
| US20120095204A1 (en) | Method to prepare d-glucosamine hydrochloride | |
| CN103951116A (en) | Method for treating casing processing wastewater and application of treatment product | |
| CN104000243B (en) | A kind of method extracting Concha Ostreae powder from Concha Ostreae cooking liquor | |
| CN104610043B (en) | A kind of method reclaiming oxalic acid from rare-earth industry waste water | |
| CN103991846B (en) | Iodomethane prepares iodine and the method for gallium of reclaiming in trimethyl gallium residual liquid | |
| CN102936052B (en) | Method for recycling carboxymethylcellulose production wastewater | |
| CN105016963A (en) | Synthetic method of 2-bromo-5-iodotoluene | |
| CN107602481A (en) | A kind of 2 methyl 4 amino 5 (formyl aminomethyl) pyrimidine hydrolysis process | |
| CN106756011A (en) | The method that saponification directly extracts calcium is exempted from a kind of synergic solvent extraction from solution | |
| CN111362821A (en) | Environment-friendly and efficient levodopa production method | |
| CN111635439A (en) | Process method for improving yield of icariin | |
| CN112391186A (en) | Method for separating phenolic compounds from coal tar | |
| CN110106357A (en) | A method of rhodium is recycled from rhodium caprylate production waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171228 Address after: 425100 Taojiang Road, Lingling District, Yongzhou, Hunan Province, No. 53 Patentee after: Yongzhou Guangfeng agrochemical Co. Ltd. Address before: 330000 Chemical Industry School of Jiangxi Province, Nanchang, east suburb of Jiangxi Province Patentee before: Wu Lunfei |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120704 Termination date: 20180616 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |