CN101570324A - Method for recovering phosphite from glyphosate mother liquor - Google Patents
Method for recovering phosphite from glyphosate mother liquor Download PDFInfo
- Publication number
- CN101570324A CN101570324A CNA2009101155263A CN200910115526A CN101570324A CN 101570324 A CN101570324 A CN 101570324A CN A2009101155263 A CNA2009101155263 A CN A2009101155263A CN 200910115526 A CN200910115526 A CN 200910115526A CN 101570324 A CN101570324 A CN 101570324A
- Authority
- CN
- China
- Prior art keywords
- phosphite
- acid
- solution
- glyphosate
- reclaims
- 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.)
- Granted
Links
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 32
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 32
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000012452 mother liquor Substances 0.000 title claims abstract description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 17
- 239000010413 mother solution Substances 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 8
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 7
- 239000005819 Potassium phosphonate Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- YXXXKCDYKKSZHL-UHFFFAOYSA-M dipotassium;dioxido(oxo)phosphanium Chemical compound [K+].[K+].[O-][P+]([O-])=O YXXXKCDYKKSZHL-UHFFFAOYSA-M 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- JDRJCBXXDRYVJC-UHFFFAOYSA-N OP(O)O.N.N.N Chemical compound OP(O)O.N.N.N JDRJCBXXDRYVJC-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 238000010413 gardening Methods 0.000 description 1
- 244000144980 herd Species 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- 238000006263 metalation reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
Abstract
A method for recovering phosphite from glyphosate mother liquor, comprising the following steps: (1) evenly mixing triethylamine as extractant and glyphosate mother liquor for standby, separating the solution to obtain triethylamine salt solution on the upper layer and a mixed solution of glyphosate and phosphite on the lower layer; (2) mixing the obtained mixed solution in step (1) and an acid and crystalizing by decreasing temperature to obtain a filter cake of phosphite. The invention has the advantage that phosphite is effectively recovered from glyphosate mother liquor, thus increasing the competitiveness of the enterprise.
Description
Technical field
The present invention relates to a kind of method that reclaims phosphite, relate in particular to a kind of method that from glyphosate mother solution, reclaims phosphite.
Background technology
As everyone knows, glyphosate is very effective to the control of perennial dark root malignant weed, farming, woods, herd, aspect such as gardening uses very extensively, the production method of glyphosate has a lot.At present, glycine method is the domestic production technique that generally adopts, and will produce a large amount of glyphosate mother solutions in its production process, and these mother liquors and contain a large amount of phosphites except containing a small amount of glyphosate.Phosphite uses very extensive in industry, when electroless plating, phosphite makes the metallic surface have anticorrosive anti-wear as reductive agent, evenly dense, firm phosphor alloy coating, be surface metalations such as plastics, pottery, prepare various industrial preservatives, can be used as oxidation inhibitor, anti-discoloring agent, dispersion agent.Therefore from glyphosate mother solution, recycle phosphite and can effectively improve enterprise competitiveness.
Summary of the invention
The object of the present invention is to provide a kind of method that from glyphosate mother solution, reclaims phosphite,, reclaim phosphite by handling glyphosate mother solution.
The present invention is achieved like this, and it is characterized in that step method is:
(1) press triethylamine and mother liquor weight ratio 1: 2-5 mixes, and adds triethylamine in mother liquor, after stirring, adds alkali and regulates PH to 8-10, and standing demix separates the upper strata, back and gets triethylamine salt solution, and lower floor gets the mixing solutions of glyphosate and phosphite;
(2) mixed solution that step (1) is obtained and acid are by weight 1: 1-5 mixes, cools to 0-20 ℃, and crystallization 1-2 hour, must filter cake and filtrate after the filtration;
(3) step (2) obtains the hydrolysis reaction that filtrate can be used for glyphosate production;
(4) filter cake that obtains of step (2) is the phosphite crude product, through washing, drying, the phosphite finished product.
Alkali of the present invention is sodium hydroxide, potassium hydroxide or ammonia.
Acid of the present invention is hydrochloric acid, sulfuric acid or hydrogen chloride gas.
The described alkali of step of the present invention (1) is mixed with the alkaline solution of 30-99% when using.
The present invention is the described acid of step (2) when being sulfuric acid, and the acid solution that is mixed with 30-98% uses.
The present invention is that the described acid of step (2) is hydrochloric acid when acid, and the acid solution that is mixed with 25-38% uses.
The present invention is the described acid of step (2) when being hydrogen chloride gas, and its hydrogen chloride content is at 40-99%.
Advantage of the present invention is: simple for process, production cost is low, can be from glyphosate mother solution the efficient recovery phosphite, improve enterprise competitiveness.
Embodiment
Embodiment one
(1) in the 400g glyphosate mother solution, add triethylamine 100g, after stirring, add 48% sodium hydroxide 50g, regulate pH to 9.0, standing demix, lower floor gets glyphosate and sodium phosphite mixing solutions 110.5g.
(2) the hydrochloric acid 300g of adding 36% in above-mentioned 110.5g mixing solutions cools to 20 ℃, and crystallization 1 hour is filtered, and gets sodium phosphite crude product 31.5g.
(3) with above-mentioned sodium phosphite crude product, washing is dry, must get sodium phosphite finished product 25.0g.
Embodiment two
(1) in the 400g glyphosate mother solution, add triethylamine 100g, after stirring, add 25% ammoniacal liquor 30g, regulate pH to 8.5, standing demix, lower floor gets glyphosate and ammonium phosphite mixing solutions 112.5g.。
(2) feed hydrogen chloride gas 40g in above-mentioned 112.5g mixing solutions, cool to 10 ℃, crystallization 1 hour is filtered, and gets sodium phosphite crude product 26.5g.
(3) with above-mentioned ammonium phosphite crude product, washing is dry, must get sodium phosphite finished product 22.5g.
Embodiment two
(1) in the 400g glyphosate mother solution, add triethylamine 100g, after stirring, add 99% potassium hydroxide 38.5g, regulate pH to 9.2, standing demix, lower floor gets glyphosate and potassium phosphite mixing solutions 106.5g.
(2) add 98% sulfuric acid 150g in above-mentioned 106.5g mixing solutions, cool to 10 ℃, crystallization 1.5 hours is filtered, and gets potassium phosphite crude product 33.5g.
(3) with above-mentioned potassium phosphite crude product, washing is dry, must get sodium phosphite finished product 30.5g.
Claims (7)
1, a kind of method that reclaims phosphite from glyphosate mother solution is characterized in that step method is:
(1) press triethylamine and mother liquor weight ratio 1: 2-5 mixes, and adds triethylamine in mother liquor, after stirring, adds alkali and regulates PH to 8-10, and standing demix separates the upper strata, back and gets triethylamine salt solution, and lower floor gets the mixing solutions of glyphosate and phosphite;
(2) mixed solution that step (1) is obtained and acid are by weight 1: 1-5 mixes, cools to 0-20 ℃, and crystallization 1-2 hour, must filter cake and filtrate after the filtration;
(3) step (2) obtains the hydrolysis reaction that filtrate can be used for glyphosate production;
(4) filter cake that obtains of step (2) is the phosphite crude product, through washing, drying, the phosphite finished product.
2, the method that reclaims phosphite from glyphosate mother solution as claimed in claim 1 is characterized in that described alkali is sodium hydroxide, potassium hydroxide or ammonia.
3, the method that reclaims phosphite from glyphosate mother solution as claimed in claim 1 is characterized in that described acid is hydrochloric acid, sulfuric acid or hydrogen chloride gas.
4, the method that reclaims phosphite from glyphosate mother solution as claimed in claim 1 is characterized in that the described alkali of step (1) is mixed with the alkaline solution of 30-99% when using.
5, the method that reclaims phosphite from glyphosate mother solution as claimed in claim 1 is characterized in that it being the described acid of step (2) when being sulfuric acid, and the acid solution that is mixed with 30-98% uses.
6, the method that reclaims phosphite from glyphosate mother solution as claimed in claim 1 is characterized in that it being the described acid of step (2) when being hydrochloric acid acid, and the acid solution that is mixed with 25-38% uses.
7, the method that reclaims phosphite from glyphosate mother solution as claimed in claim 1 is characterized in that it being the described acid of step (2) when being hydrogen chloride gas, and its hydrogen chloride content is at 40-99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910115526 CN101570324B (en) | 2009-06-16 | 2009-06-16 | Method for recovering phosphite from glyphosate mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910115526 CN101570324B (en) | 2009-06-16 | 2009-06-16 | Method for recovering phosphite from glyphosate mother liquor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101570324A true CN101570324A (en) | 2009-11-04 |
| CN101570324B CN101570324B (en) | 2013-05-08 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910115526 Expired - Fee Related CN101570324B (en) | 2009-06-16 | 2009-06-16 | Method for recovering phosphite from glyphosate mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101570324B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830928A (en) * | 2010-05-28 | 2010-09-15 | 吴伦飞 | Method for recovering glyphosate raw powder from glyphosate mother liquid |
| CN111333519A (en) * | 2020-03-11 | 2020-06-26 | 陈兴华 | Comprehensive treatment and resource recycling method for glyphosate mother liquor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6448434B1 (en) * | 1999-07-29 | 2002-09-10 | 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 |
| CN1657532A (en) * | 2005-01-31 | 2005-08-24 | 浙江新安化工集团股份有限公司 | Process for treating cglyphosate mother liquor |
| CN1824668A (en) * | 2005-02-25 | 2006-08-30 | 浙江新安化工集团股份有限公司 | Treatment method of glyphosate mother liquor |
| CN101190926A (en) * | 2006-11-29 | 2008-06-04 | 浙江新安化工集团股份有限公司 | Method for treating glyphosate mother liquid |
-
2009
- 2009-06-16 CN CN 200910115526 patent/CN101570324B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6448434B1 (en) * | 1999-07-29 | 2002-09-10 | 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 |
| CN1657532A (en) * | 2005-01-31 | 2005-08-24 | 浙江新安化工集团股份有限公司 | Process for treating cglyphosate mother liquor |
| CN1824668A (en) * | 2005-02-25 | 2006-08-30 | 浙江新安化工集团股份有限公司 | Treatment method of glyphosate mother liquor |
| CN101190926A (en) * | 2006-11-29 | 2008-06-04 | 浙江新安化工集团股份有限公司 | Method for treating glyphosate mother liquid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830928A (en) * | 2010-05-28 | 2010-09-15 | 吴伦飞 | Method for recovering glyphosate raw powder from glyphosate mother liquid |
| CN101830928B (en) * | 2010-05-28 | 2016-01-20 | 吴伦飞 | A kind of method reclaiming the former powder of glyphosate from glyphosate mother solution |
| CN111333519A (en) * | 2020-03-11 | 2020-06-26 | 陈兴华 | Comprehensive treatment and resource recycling method for glyphosate mother liquor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101570324B (en) | 2013-05-08 |
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| C06 | Publication | ||
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| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20091104 Assignee: Xuchang Dongfang Chemical Co.,Ltd. Assignor: Wu Lunfei Contract record no.: 2014410000033 Denomination of invention: Method for recovering phosphite from glyphosate mother liquor Granted publication date: 20130508 License type: Exclusive License Record date: 20140422 |
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Change date: 20150709 Contract record no.: 2014410000033 Assignee after: HENAN HDF CHEMICAL COMPANY LTD. Assignee before: Xuchang Dongfang Chemical Co.,Ltd. |
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| TR01 | Transfer of patent right |
Effective date of registration: 20171115 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 |
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| EC01 | Cancellation of recordation of patent licensing contract | ||
| EC01 | Cancellation of recordation of patent licensing contract |
Assignee: HENAN HDF CHEMICAL COMPANY LTD. Assignor: Yongzhou Guangfeng agrochemical Co. Ltd. Contract record no.: 2014410000033 Date of cancellation: 20180524 |
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| EM01 | Change of recordation of patent licensing contract | ||
| EM01 | Change of recordation of patent licensing contract |
Change date: 20180524 Contract record no.: 2014410000033 Assignor after: Yongzhou Guangfeng agrochemical Co. Ltd. Assignor before: Wu Lunfei |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20130508 Termination date: 20180616 |