CN101172985A - Improved process for producing glyphosate acid ammonium salt - Google Patents
Improved process for producing glyphosate acid ammonium salt Download PDFInfo
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- CN101172985A CN101172985A CNA2006101430623A CN200610143062A CN101172985A CN 101172985 A CN101172985 A CN 101172985A CN A2006101430623 A CNA2006101430623 A CN A2006101430623A CN 200610143062 A CN200610143062 A CN 200610143062A CN 101172985 A CN101172985 A CN 101172985A
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- glyphosate
- solid
- ammoniacal liquor
- glyphosate acid
- acid
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Abstract
The invention discloses a high-efficiency continuous method with simple technique for producing glyphosate ammonium salt. The technique adopts solid glyphosate and ammonia as raw materials, and adopts solid glyphosate as stationary phase and ammonia as mobile phase, and then a certain quantity of filling materials or carriers are filled, a certain height of solid glyphosate is filled, and then ammonia is led to flow through solid glyphosate to react, thereby obtaining glyphosate ammonium salt.
Description
Technical field
The present invention relates to a kind of improving one's methods of ammonium glyphosate of producing
Background technology
Glyphosate has efficiently, does not have advantages such as residual in low toxicity and the soil as weedicide, has become the maximum and the fastest steriland herbicide of rate of growth of sales volume in the world at present.
Because the solubleness of glyphosate in water very low (1.2 grams/100 grams, 25 ℃) is normally made glyphosphonic acid salt soluble solids preparation, emulsion or aqua in actual applications.Characteristics such as compare with aqua with the glyphosate pulvis, it is long that glyphosate salt soluble solids preparation has validity period, and the transport and storage cost is low and easy to use.Glyphosate salt has sodium salt, sylvite and ammonium salt.The sodium salt water absorbability is strong, sylvite cost height, so ammonium glyphosate is used more extensive.
At present, there have been many patents to relate to synthetic method, mainly have been divided into two classes by ammonium glyphosate.The patent disclosure of the first kind with the gas-solid reaction method of glyphosate and anhydrous ammonia gas prepared in reaction ammonium glyphosate, relevant patent has CN1068008; IL118576; KR257283; ZA9604774; AU704518; HU9802088; NZ306043; CA2221299; EP0832086; US5633397; WO9640697 and AU5419596.With patent CN1068008 is example, and the shortcoming of this gas-solid reaction method is that the solid product that is deposited on the reactor wall can influence in time removing of reaction heat; It is improper that ammonia adds speed control, easily forms the dirt plug of ingress.In addition, the solid ammonium salt that generates at the glyphosphonic acid solid surface can hinder the reaction of solid interior glyphosphonic acid and anhydrous ammonia gas.Can strike off precipitated solid product on the wall continuously so must install in reactor, strict control ammonia adds speed and makes raw material particulate glyphosate acid granularity as far as possible little.The patented technology of second class is disclosed mainly to be to react the synthesizing glyphosate acid ammonium salt with ammonia soln and glyphosphonic acid, and relevant patent has CN1192743; CN1365254; CA2444608; EP1381278; US2002173423; WO02085122; US6734142; GR3036355T; IL118577; KP266126; ZA9604775; HU9802333; NZ307310; CA2221298; AU694877; EP0845000; US5716903; US5614468; WO9640696 and AU5662096 etc.This class patent needs timing sampling analysis moisture content in order to control the water-content in the reaction system, and strict control ammoniacal liquor adding speed and employing are warmed wind exsiccant form and removed the water that generates in the dereaction; In order to reduce the oxidation of warm air to glyphosphonic acid, also need to add the antioxidant S-WAT in the reaction process, complex process and power consumption are high.
At above deficiency, 200410069352.9 of Institute of Botany, Chinese Academy of Sciences's application discloses the method that a kind of high-efficiency and continuous, technology are simply produced ammonium glyphosate.With solid glyphosate acid and ammoniacal liquor is raw material, is stationary phase with solid glyphosate acid, is moving phase with ammoniacal liquor, and it is sour and react to make ammoniacal liquor flow through solid glyphosate, obtains ammonium glyphosate.This patented technology can solve the problems referred to above, but, carrying out along with reaction, particulate glyphosate acid is more and more thinner, tap density as stationary phase is then increasing, cause the resistance to mass transfer of ammoniacal liquor increasing, the contact surface with particulate glyphosate acid also reduces simultaneously, has influenced reaction greatly and has carried out.
Summary of the invention
The method of production ammonium glyphosate provided by the invention is to be raw material with solid glyphosate acid and ammoniacal liquor, is stationary phase with solid glyphosate acid, is moving phase with ammoniacal liquor, and it is sour and react to make ammoniacal liquor flow through solid glyphosate.Its reaction process is carried out in specified reaction tower, and adds a certain amount of filler or carrier in advance in tower, fills the solid glyphosate acid of certain altitude then, makes ammoniacal liquor flow through solid glyphosate acid and reacts, and obtains ammonium glyphosate.
Wherein, the concentration of volume percent of described ammoniacal liquor should be at 5-20%;
Wherein, ammoniacal liquor flow through solid glyphosate acid time or and should be controlled at 10 minutes-1.5 hours duration of contact of solid glyphosate acid, preferably between 20 minutes-50 minutes, and make the high ammoniacal liquor of concentration have slower flow velocity as far as possible.
Filler described in the present invention or carrier can be selected the random packing of materials such as pottery, plastics for use, as arc ring, Haier's ring etc. in Pall ring, Raschig ring, cascade ring, rectangular saddle ring, the Taylor's garland, eight or four; Also can select regular corrugation filler efficiently for use, and various acid-proof ceramics, ceramic honey comb etc.
Selectable, embodiment can followingly be carried out: a certain amount of filler of device or carrier in the reaction tower, the bottom is provided with sieve plate, the solid glyphosate acid of filling certain altitude is as stationary phase in the tower, ammoniacal liquor sprays to the sweet acid of solid grass from the reaction tower top, and flows through solid glyphosate acid, and the ammonium glyphosate salt brine solution of generation flows out from the tower bottom, go to concentrate also crystallization then and obtain the ammonium glyphosate solid phase prod, yield can reach more than 98%.
In patent 200410069352.9, because carrying out along with reaction, the concentration of ammoniacal liquor reduces in process of flowing gradually, particulate glyphosate acid is also more and more thinner simultaneously, and the tap density of stationary phase is also increasing, and ammoniacal liquor is also increasing toward dirty resistance, so cause bottom at tower, carrying out of reaction is more and more difficult, needs the sufficiently long time to satisfy the contact reacts of ammoniacal liquor and glyphosphonic acid, and reaction is carried out not thorough and can cause glyphosphonic acid to be in for a long time oxidation takes place under the high temperature.
Method of the present invention is except that the advantage that possesses Chinese patent 200410069352.9, also effectively remedied its deficiency: because of materials such as the filler that in tower, added certain altitude or carriers, can not influence reaction because of tap density increases, make reaction more abundant, reaction rate accelerates, reaction times shortens, and the ammonium glyphosate purity salt of reaction gained is higher.
Embodiment
Embodiment 1
Highly be that 1.8 rice diameters are the filler of 1.5 meters of fillings in 15 centimetres the reaction tower, inserting then highly is 1.5 meters solid glyphosate acid, adding concentration expressed in percentage by volume from top amount with 10 milliliters/second then is 5% ammoniacal liquor, when the glyphosphonic acid solid reduces to 1.2 meters, in time add glyphosphonic acid solid to 1.5 meter.This moment, ammoniacal liquor flow through the time of solid glyphosate acid or be 20 minutes the duration of contact of ammoniacal liquor and solid glyphosate acid, and the temperature in the reaction tower can maintain 30～50 ℃, and condensing crystal then obtains purity and be 98.8% ammonium glyphosate solid phase prod.
Embodiment 2
It highly is being 1.8 meters, diameter is the filler of 1.5 meters of fillings in 15 centimetres the reaction tower, inserting then highly is 1.5 meters solid glyphosate acid, adding concentration from top amount with 10 milliliters/second then is 20% ammoniacal liquor, when the glyphosphonic acid solid reduces to 1.2 meters, in time add glyphosphonic acid solid to 1.5 meter.This moment, ammoniacal liquor flow through the time of solid glyphosate acid or be 40 minutes the duration of contact of ammoniacal liquor and solid glyphosate acid, and the temperature in the reaction tower 1 can maintain 50～65 ℃, and condensing crystal then obtains purity and be 98.8% ammonium glyphosate solid phase prod.
Claims (7)
1. produce improving one's methods of ammonium glyphosate for one kind, comprise that with solid glyphosate acid and ammoniacal liquor be raw material, solid glyphosate acid is stationary phase, ammoniacal liquor is moving phase, making ammoniacal liquor flow through solid glyphosate acid in tower reacts, obtain ammonium glyphosate, it is characterized in that: place certain filler or carrier in the tower, filling solid glyphosate acid then.
2. the method for claim 1, the concentration expressed in percentage by volume that it is characterized in that described ammoniacal liquor is 5-20%.
3. the method for claim 1 is characterized in that the product ammonium glyphosate that obtains can also obtain high purity, highly active ammonium glyphosate solid phase prod through dehydration and crystallisation step.
4. method as claimed in claim 1 or 2 is characterized in that described ammoniacal liquor flows through the time of solid glyphosate acid or be 10 minutes-1.5 hours the duration of contact of ammoniacal liquor and solid glyphosate acid.
5. 4 method as claimed in claim is characterized in that be 40 minutes-70 minutes described duration of contact.
6. the method for claim 1 is characterized in that described filler or carrier can be random packings, or structured packing.
7. method as claimed in claim 6 is characterized in that described random packing is arc ring in Pall ring, Raschig ring, cascade ring, rectangular saddle ring, the Taylor's garland, eight or four, Haier's ring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101430623A CN101172985B (en) | 2006-10-31 | 2006-10-31 | Improved process for producing glyphosate acid ammonium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101430623A CN101172985B (en) | 2006-10-31 | 2006-10-31 | Improved process for producing glyphosate acid ammonium salt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101172985A true CN101172985A (en) | 2008-05-07 |
| CN101172985B CN101172985B (en) | 2011-04-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2006101430623A Expired - Fee Related CN101172985B (en) | 2006-10-31 | 2006-10-31 | Improved process for producing glyphosate acid ammonium salt |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948482A (en) * | 2010-09-01 | 2011-01-19 | 南通利华农化有限公司 | Process for producing glyphosate ammonium dry powder |
| CN110437279A (en) * | 2019-08-27 | 2019-11-12 | 鹤壁市鹤农生物科技有限公司 | A kind of preparation method of ammonium glyphosate technical product |
| CN110452264A (en) * | 2019-08-21 | 2019-11-15 | 永农生物科学有限公司 | A kind of preparation method of high optical selective essence glufosinate-ammonium ammonium salt |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244587C (en) * | 2002-09-05 | 2006-03-08 | 浙江新安化工集团股份有限公司 | Gas-liquid-solid three phase reactions and solvent exraction for preparing ammonia glyphosate acid |
| CN1328283C (en) * | 2004-07-19 | 2007-07-25 | 中国科学院植物研究所 | Method of producing ammonium glyphosate |
-
2006
- 2006-10-31 CN CN2006101430623A patent/CN101172985B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948482A (en) * | 2010-09-01 | 2011-01-19 | 南通利华农化有限公司 | Process for producing glyphosate ammonium dry powder |
| CN110452264A (en) * | 2019-08-21 | 2019-11-15 | 永农生物科学有限公司 | A kind of preparation method of high optical selective essence glufosinate-ammonium ammonium salt |
| CN110437279A (en) * | 2019-08-27 | 2019-11-12 | 鹤壁市鹤农生物科技有限公司 | A kind of preparation method of ammonium glyphosate technical product |
| CN110437279B (en) * | 2019-08-27 | 2022-02-08 | 鹤壁市鹤农生物科技有限公司 | Preparation method of ammonium glyphosate technical |
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| Publication number | Publication date |
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| CN101172985B (en) | 2011-04-20 |
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