CN101589724A - Utilize the method for glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations - Google Patents
Utilize the method for glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations Download PDFInfo
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- CN101589724A CN101589724A CNA2009101002145A CN200910100214A CN101589724A CN 101589724 A CN101589724 A CN 101589724A CN A2009101002145 A CNA2009101002145 A CN A2009101002145A CN 200910100214 A CN200910100214 A CN 200910100214A CN 101589724 A CN101589724 A CN 101589724A
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Abstract
The invention discloses a kind of method of utilizing glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations, it is to contain the mother liquor of glyphosate 1～4% in the dimethylphosphite method glyphosate production, enter the one-level membrane separation device and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates dense mother liquor and the light mother liquor of secondary, and dense mother liquor returns the import of one-level membrane separation device; Smart mother liquor is through after the preliminary treatment, add the former powder of glyphosate, auxiliary agent, ammonia (or isopropylamine, potassium hydroxide and potash one of them) be deployed into the glyphosate formulation of concentration 30～70%, the light mother liquor lease making of secondary multiple-effect evaporation concentrates, crystallization, centrifugation, dried recovered accessory substance NaCl, add slaked lime after the mother liquor oxidation after the separation, dephosphorization is handled, and precipitation is told calcium phosphate.The present invention utilizes the glyphosate formulation of glyphosate mother solution preparation more than 30%, reclaims the accessory substance in the mother liquor, reduces the glyphosate production wastewater treating capacity significantly.
Description
Technical field
The present invention relates to the research field of the mother liquid obtained treatment process of glyphosate production.More particularly, the present invention relates to utilize the method for glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations.Utilize the mother liquid obtained preparation high concentration of dimethylphosphite method glyphosate production glyphosate formulation, achieve the method for abundant recycling active ingredient, minimizing wastewater treatment capacity, reduction mother liquor processing cost.
Background technology
Glyphosate is a kind of high-efficiency low-toxicity low-residual, wide spectrum and inner sucting conduction type nonselective herbicide, because of its superior performance develops at present the weed killer herbicide kind of output maximum in the world.
The main synthetic method of glyphosate has chloroactic acid method, dimethylphosphite method, iminodiacetic acid (salt) acid system etc., the dimethylphosphite method is because low, the characteristics such as yield is high, product purity height of cost, becomes the main flow production technology of domestic production enterprise.But this technology can produce a large amount of mother liquors, and 1 ton of folding of every production, hundred glyphosates will produce 5 tons of glyphosate mother solutions, and wherein glyphosate content about 2.5%, sodium chloride content about 10～20%; Treatment process commonly used is: mother liquor is removed part sodium chloride through concentrating, and concentrated mother liquor contains glyphosate 3～8%, is mixed with 10% gyphosate solution.
The mother liquor method for concentration mainly contains: evaporation and concentration and membrane separation concentrated contracting (CN101058586).The concentrated mother liquor that existing method obtains all can only be mixed with the gyphosate solution of low concentration.The Ministry of Agriculture of country has issued bulletin in by the end of February, 2009 No. 1158 in, concentration to glyphosate formulation is stipulated, the least concentration of gyphosate solution is 30% (effective ingredient), must not carry out the production of 10% gyphosate solution, for this reason, domestic enterprise has only two lines to walk: promptly a large amount of mother liquors will be handled as the three wastes, perhaps carries out recycling.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing technology, a kind of method of utilizing glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations is provided.
Utilize the method for glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations to comprise the steps:
1) is equipped with glyphosate mother solution in the glyphosate production by the dimethylphosphite legal system, after micro-filtration is removed solid impurity, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) in smart mother liquor, add the former powder of glyphosate, 5～20% APG glyphosate auxiliary agent and 3～8% the ammonia or 10～30% the isopropylamine of smart mother liquor amount 25～72%, or 10～30% potassium hydroxide, or 11～33% potash is prepared into the gyphosate solution of active ingredient 30～41%;
Perhaps earlier smart mother liquid evaporation being concentrated into glyphosate mother solution content is 20～30%, adopt atomized drying again or directly adopt atomized drying to obtain ammonium glyphosate dry powder, the ammonium glyphosate, 1～5% APG glyphosate auxiliary agent that add smart mother liquor amount 0.1～80% are made active ingredient 30～80% soluble powders or granula;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor that centrifugation obtains use the oxidant oxidation, adds slaked lime and carries out dephosphorization and handle, and precipitates and tells calcium phosphate.
The light mother liquor of described secondary is concentrated through multiple-effect evaporation, salt is adopted in crystallization, centrifugation is to adopt 2～4 to imitate the light mother liquors of evaporation and concentration secondarys, and second effect to quadruple effect adopts cyclone hydraulic separators to adopt salt, recovery NaCl.Oxidant is chlorine dioxide or hydrogen peroxide.
The present invention adopts multistage membrane separation device to handle mother liquor, and glyphosate content height in the smart mother liquor and salt content is low can the compounding high concentration preparation, and the glyphosate rate of recovery is more than 90%.Adopt multiple-effect evaporation to concentrate high saliferous mother liquor, can reduce steam consumption significantly.Adopt smart mother liquor directly to dispose high concentration aqua and the concentrated light mother liquor of secondary of multiple-effect evaporation, needed the wastewater flow rate of subsequent treatment to reduce significantly.
The present invention can utilize the high-grade glyphosate formulation of glyphosate mother solution preparation 30% above active ingredient, reclaims the accessory substance in the mother liquor, reduces the glyphosate production wastewater treating capacity significantly, significantly reduces the mother liquor processing cost.
Description of drawings
Accompanying drawing is the schematic flow sheet that glyphosate mother solution prepares the high concentration glyphosate formulation.
Embodiment
Embodiment 1
1) is equipped with glyphosate alkali liquor in the glyphosate production by the dimethylphosphite legal system, after micro-filtration is removed solid impurity, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) in smart mother liquor, add the former powder of glyphosate, 5% APG glyphosate CGN-3 auxiliary agent (Yang Zhouchenization production) of smart mother liquor amount 30%, the gyphosate solution that 3.5% ammonia is prepared into active ingredient 30%;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor that centrifugation obtains, logical chlorine dioxide 1 hour adds slaked lime and carries out dephosphorization and handle, precipitation is told calcium phosphate.
Embodiment 2
1) is equipped with glyphosate alkali liquor in the glyphosate production by the dimethylphosphite legal system, after micro-filtration is removed solid impurity, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) in smart mother liquor, add the former powder of glyphosate, 20% APG glyphosate CGN-3 auxiliary agent (Yang Zhouchenization production) of smart mother liquor amount 72%, the gyphosate solution that 30% potassium hydroxide (or potash of 33%) is prepared into active ingredient 41%;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor that centrifugation obtains, logical chlorine dioxide 1 hour adds slaked lime and carries out dephosphorization and handle, precipitation is told calcium phosphate.
Embodiment 3
1) is equipped with glyphosate alkali liquor in the glyphosate production by the dimethylphosphite legal system, after micro-filtration is removed solid impurity, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5%, salinity 0.8%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) earlier smart mother liquid evaporation being concentrated into glyphosate mother solution content is 10%, adds the former powder of glyphosate, 3% APG glyphosate CGN-3 auxiliary agent (Yang Zhouchenization production) of smart mother liquor amount 30%, the gyphosate solution that 3.5% ammonia is prepared into active ingredient 30% again;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor that centrifugation obtains, logical chlorine dioxide 1 hour adds slaked lime and carries out dephosphorization and handle, precipitation is told calcium phosphate.
Embodiment 4
1) is equipped with glyphosate alkali liquor in the glyphosate production by the dimethylphosphite legal system, after micro-filtration is removed solid impurity, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) earlier smart mother liquid evaporation being concentrated into glyphosate mother solution content is 20%, adopt atomized drying again or directly adopt atomized drying to obtain ammonium glyphosate dry powder, the ammonium glyphosate, 5% APG glyphosate CGN-3 auxiliary agent (Yang Zhouchenization production), 5% ammonium sulfate that add smart mother liquor amount 0.1% are made active ingredient 30% soluble powder;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor that centrifugation obtains, logical chlorine dioxide 1 hour adds slaked lime and carries out dephosphorization and handle, precipitation is told calcium phosphate.
Embodiment 5
1) is equipped with glyphosate alkali liquor in the glyphosate production by the dimethylphosphite legal system, after solid impurity is removed in ultrafiltration, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) earlier smart mother liquid evaporation being concentrated into glyphosate mother solution content is 30%, adopt atomized drying to obtain ammonium glyphosate dry powder again, the ammonium glyphosate, 5% APG glyphosate CGN-3 auxiliary agent (Yang Zhouchenization production), 5% ammonium sulfate that add smart mother liquor amount 80% are made active ingredient 70% soluble powder or granula;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor that centrifugation obtains, logical chlorine dioxide 1 hour adds slaked lime and carries out dephosphorization and handle, precipitation is told calcium phosphate.
Method described in the invention can be carried out multiple combination, does not do the limit explanation in the present invention, also should be included in the present invention even the processing scheme of being done on basis of the present invention is different from embodiment.
Claims (3)
1. a method of utilizing glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations is characterized in that, comprises the steps:
1) is equipped with glyphosate mother solution in the glyphosate production by the dimethylphosphite legal system, after micro-filtration is removed solid impurity, enter the one-level membrane separation device continuously and isolate light mother liquor and smart mother liquor, smart mother liquor contains glyphosate 5～10%, salinity＜2.0%, light mother liquor enters the secondary membrane separation device and isolates light mother liquor of secondary and dense mother liquor, dense mother liquor returns the import of one-level membrane separation device, and the light mother liquor of secondary contains glyphosate＜0.2%;
2) potash that adds the isopropylamine of the former powder of glyphosate, 5～20% APG glyphosate auxiliary agent of smart mother liquor amount 25～72% and 3～8% ammonia or 10～30% or 10～30% potassium hydroxide or 11～33% in smart mother liquor is prepared into the gyphosate solution of active ingredient 30～41%;
Perhaps earlier smart mother liquid evaporation being concentrated into glyphosate mother solution content is 20～30%, adopt atomized drying again or directly adopt atomized drying to obtain ammonium glyphosate dry powder, the ammonium glyphosate, 2～10% APG glyphosate auxiliary agents that add smart mother liquor amount 0.1～80% are made active ingredient 30～70% soluble powders or granula;
3) the light mother liquor of secondary through multiple-effect evaporation concentrate, crystallization adopts salt, centrifugation, dried recovered accessory substance NaCl, the mother liquor after the centrifugation use the oxidant oxidation, adds slaked lime and carries out dephosphorization and handle, and precipitates and tells calcium phosphate.
2. a kind of method of utilizing glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations according to claim 1, it is characterized in that the light mother liquor of described secondary is concentrated through multiple-effect evaporation, salt is adopted in crystallization, centrifugation is to adopt 2～4 to imitate the light mother liquors of evaporation and concentration secondarys, second effect to quadruple effect adopts cyclone hydraulic separators to adopt salt, reclaim NaCl, use the centrifuge separating, washing then, drying.
3. a kind of method of utilizing glyphosate mother solution preparation 30～70% active ingredient glyphosate formulations according to claim 1 is characterized in that described oxidant is chlorine dioxide or hydrogen peroxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786735A (en) * | 2010-02-11 | 2010-07-28 | 浙江新安化工集团股份有限公司 | Film treatment method of glyphosate mother liquor |
| CN101967161A (en) * | 2010-04-22 | 2011-02-09 | 浙江新安化工集团股份有限公司 | Comprehensive treatment method for glyphosate mother liquid |
| CN101985426A (en) * | 2010-09-06 | 2011-03-16 | 山东潍坊润丰化工有限公司 | Method for treating glyphosate mother solution |
| CN102161677A (en) * | 2010-02-18 | 2011-08-24 | 浙江新安化工集团股份有限公司 | Membrane process technology for extracting glyphosate from glyphosate mother liquor |
| CN102786187A (en) * | 2012-08-17 | 2012-11-21 | 四川省乐山市福华通达农药科技有限公司 | Integrated process for recycling glyphosate mother liquor |
| CN104719333A (en) * | 2015-03-24 | 2015-06-24 | 淮南师范学院 | Method for producing 30% glyphosate solution by using glyphosate mother liquid |
| CN105230656A (en) * | 2015-11-13 | 2016-01-13 | 安徽省益农化工有限公司 | Preparation process for 30%-45% glyphosate preparation |
-
2009
- 2009-06-25 CN CNA2009101002145A patent/CN101589724A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786735A (en) * | 2010-02-11 | 2010-07-28 | 浙江新安化工集团股份有限公司 | Film treatment method of glyphosate mother liquor |
| CN102161677A (en) * | 2010-02-18 | 2011-08-24 | 浙江新安化工集团股份有限公司 | Membrane process technology for extracting glyphosate from glyphosate mother liquor |
| CN102161677B (en) * | 2010-02-18 | 2015-07-22 | 浙江新安化工集团股份有限公司 | Membrane process technology for extracting glyphosate from glyphosate mother liquor |
| CN101967161A (en) * | 2010-04-22 | 2011-02-09 | 浙江新安化工集团股份有限公司 | Comprehensive treatment method for glyphosate mother liquid |
| CN101967161B (en) * | 2010-04-22 | 2012-12-26 | 浙江新安化工集团股份有限公司 | Comprehensive treatment method for glyphosate mother liquid |
| CN101985426A (en) * | 2010-09-06 | 2011-03-16 | 山东潍坊润丰化工有限公司 | Method for treating glyphosate mother solution |
| CN101985426B (en) * | 2010-09-06 | 2013-07-03 | 山东潍坊润丰化工有限公司 | Method for treating glyphosate mother solution |
| CN102786187A (en) * | 2012-08-17 | 2012-11-21 | 四川省乐山市福华通达农药科技有限公司 | Integrated process for recycling glyphosate mother liquor |
| CN102786187B (en) * | 2012-08-17 | 2013-11-06 | 四川省乐山市福华通达农药科技有限公司 | Integrated process for recycling glyphosate mother liquor |
| CN104719333A (en) * | 2015-03-24 | 2015-06-24 | 淮南师范学院 | Method for producing 30% glyphosate solution by using glyphosate mother liquid |
| CN105230656A (en) * | 2015-11-13 | 2016-01-13 | 安徽省益农化工有限公司 | Preparation process for 30%-45% glyphosate preparation |
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Application publication date: 20091202 |