CN101692809B - Preparation method of glyphosate ammonium salt granules - Google Patents
Preparation method of glyphosate ammonium salt granules Download PDFInfo
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- CN101692809B CN101692809B CN 200910167853 CN200910167853A CN101692809B CN 101692809 B CN101692809 B CN 101692809B CN 200910167853 CN200910167853 CN 200910167853 CN 200910167853 A CN200910167853 A CN 200910167853A CN 101692809 B CN101692809 B CN 101692809B
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Abstract
The invention provides a preparation method of solid glyphosate ammonium salt granules. The preparation method comprises the step of enabling glyphosate wet powder and ammonia to react in a gas-solid phase reaction device to directly prepare glyphosate ammonium salt granules. The gas-solid phase reaction device comprises a boiling reactor with a filter screen, a spraying gun , a heater and a fan for providing power, and the spraying gun , the heater and the fan are arranged in the reactor; a condenser is arranged on a path formed by the reactor, the heater and the fan; and a circulating path is formed between the reactor and the heater, the fan and the condenser through pipelines. The concrete preparation method comprises the five steps of replacement, mixing, adding auxiliary material, granulating and drying. The invention adopts a circulating flow-condensing technology to overcome the production difficulties caused by reaction heat and generated water, has integral simple process and can decrease the production energy consumption.
Description
Technical field
The present invention relates to a kind of technique of producing glyphosate ammonium salt granules by the glyphosate wet-milling, belong to chemical field.
Background technology
Glyphosate is a kind of good steriland herbicide, after all (Monsanto) at first develops, is promoted rapidly in market by U.S. Meng Shan from 1971.Be mainly used in resistance glyphosate genetically modified crops field weeding, uncultivated area weeding, no-tillage crop-planting.At present, the global agrochemical market sales volume is up to 30,000,000,000 dollars, and wherein weed killer herbicide is about 15,000,000,000 dollars, accounts for 50% of whole pesticide market, and China's weed killer herbicide accounts for about 30% of whole pesticide market.There are 600 kinds in the weed killer herbicide whole world altogether approximately, and wherein glyphosate accounts for global weed killer herbicide total amount up to 30%.In recent years, it is the first that glyphosate occupies the world pesticide sales volume always, estimates that global demand amount in 2010 will reach 1,000,000 tons.Be widely used after early 1980s is trial-produceed successfully in China, become at present the weed killer herbicide kind of China's output maximum.Glyphosate is large-tonnage inner sucting conduction type steriland herbicide, and China has been glyphosate production big country, and product is existing certain influence in the international market.Because the significantly expansion of global genetically modified crops sowing area makes the weed killer herbicide market demand powerful, directly promotes the glyphosate sales volume to increase substantially.From international agricultural chemicals law of industry development, the industry profit shifts to finished product preparation and Sales Channel by making former medicine.Same one ton of glyphosate herbicidal, domestic enterprise only can obtain 3～40,000 yuan income from sales and several thousand yuan gross profit with former medicine form outlet; In the world some companies then the preparation by selling various concentration, dilution auxiliary agent and dispenser equipment obtain income from sales and the gross profit of several times even ten times.Only have the upwards enterprise of downstream extension future, could obtain competitive advantage.The solvability of glyphosate in water very low (1.0～1.2g/100g, 25) need to be made glyphosate the salt preparation in actual applications usually, and main formulation has: aqua, emulsion, soluble powder, soluble granula, sustained release agent; Several formulations are compared, and soluble granula more is convenient to packing, is transported and use.Glyphosate salt has ammonium salt, isopropyl amine salt, sylvite and sodium salt.Reaction control during ammonium glyphosate is produced is difficult and dry difficulty is large and the large 2008.04.02 of energy consumption, Patent Office of the People's Republic of China discloses the patent of invention (notification number: CN101151971) of a kind of " a kind of production method of glyphosate ammonium salt solid preparation " by name, its technical scheme is the mother liquor that the glyphosate mixed liquor that the PMIDA oxidation obtains is gone out 20-80% through standing separation, the control reaction pressure-0.04MPa～-0.095MPa between, reaction temperature is at 60 ℃～95 ℃, add ammonia in the glyphosate mixed liquor that obtains and make ammonium glyphosate, and utilize reaction heat to steam part water; In the ammonium glyphosate mixed liquor, add the auxiliary agent that accounts for ammonium glyphosate mixed liquor quality 5%～30%, the filler that adding accounts for ammonium glyphosate mixed liquor quality 2%～15%, carry out mist projection granulating after stirring and to obtain the ammonium glyphosate granule; Still there are the following problems for above-mentioned patent: the solvability of ammonium glyphosate in water is very large, adds reaction and can generate water simultaneously, and amount of water is difficult to control in the reaction, and the wet product that obtain after the reaction are difficult for dry, and the crystallisation by cooling time is longer after the reaction.Reaction need to consume the larger energy consumption of dry glyphosate in earlier stage in addition, and the redundant complexity of post-treating and other steps of adding solvent and solvent, the reaction heat that produces in the technical process and generation water can cause produces difficulty.Therefore and dry difficulty difficult for the reaction control in producing greatly and the large problem of energy consumption can not solve.
Summary of the invention
The present invention provides a kind of production technology of glyphosate ammonium salt granules for solving the problems referred to above of prior art existence.The present invention directly makes glyphosate ammonium salt granules with the intermediate product glyphosate wet-milling in the glyphosate production and ammonia gas react, directly adopts the reaction of glyphosate wet-milling, has simplified technological process, enhances productivity.Employing circulating current condensation technology has overcome reaction heat and has generated the production difficulty that water causes, integrated artistic is simple, can reduce energy consumption,
For realizing above-mentioned technique effect, the technical solution used in the present invention is as follows:
A kind of preparation method of glyphosate ammonium salt granules, it is characterized in that: described preparation method directly makes glyphosate ammonium salt granules for glyphosate wet-milling and ammonia are reacted in the gas-solid phase reaction device, wherein the gas-solid phase reaction device comprises boiling reactor with filter screen, is located at spray gun, the heater in the reactor and the blower fan of power is provided, path in reactor and heater and blower fan formation is provided with condenser, form a peripheral passage by pipeline between described reactor and heater, blower fan, the condenser, concrete preparation method comprises the steps:
A, displacement: the boiling reaction dryer that is provided with the circulating current passage is continued to pass into nitrogen, with the oxygen in the nitrogen replacement dryer, reduce below the oxygen content to 1% in the dryer, guarantee the safety that ammonia passes into;
B, mixing: in finishing the boiling drier of displacement, add glyphosate wet-milling and ammonia, the mole proportioning of the glyphosate of adding and ammonia is 1: 1～1.5, and glyphosate and ammonia react under fluidized state, generates ammonium glyphosate; Circulating current is taken away reaction heat and is removed moisture content in the air-flow through condenser and overcome reaction heat and generated water and cause the unmanageable problem of reacting rear material, to the reaction end, the criterion finished of reaction is for after closing circulating pump, in 5 minutes in the ebullated bed temperature of charge maintenance unchanged;
C, add auxiliary material: add the glyphosate special assistant in the reactant mixture and filler mixes after reaction finishes, wherein the weight ratio that feeds intake of glyphosate, auxiliary agent, filler is 100: 10～50: 0～100;
D, granulation: 10% APG liquid is sprayed into ebullated bed by spray gun carry out spraying granulation and make the ammonium glyphosate salt particle;
E, drying: open heater, the wet granular that the upper step was made carries out drying, and 50～150 ℃ of baking temperatures make glyphosate ammonium salt solid preparation.
Glyphosate wet-milling water content is 5%～12% in the steps A, and its moisture content is beneficial to absorbing ammonia and glyphosate reaction.
Described condenser opening is provided with the liquid collecting tank of collecting condensate liquid.The cold temperature of medium of going is lower than 8 ℃.
Described condenser is located between reactor outlet and the blower fan import.
Described heater is located between fan outlet and the boiling reactor import.
Between condenser and blower fan switch valve is set, the needs of one-way gas flow when satisfying drying.
The nozzle of described spray gun is located between the filter screen, the entrance of nitrogen and the injection of granulating with bonding slurry when being used for displacement.
The present invention compared with prior art directly adopts the semi-finished product wet-milling reaction in the glyphosate technicals production, has save the energy consumption of dry glyphosate and the post-treating and other steps of adding solvent and solvent; The condensation cooling dewaters and has overcome reaction heat and generated the production difficulty that water causes, technique is simple, can reduce energy consumption, enhances productivity.The drying and granulating process is used the special equipment boiling drier, can overcome on the one hand reaction heat and generate the production difficulty that water causes, the peripheral passage can reduce energy consumption on the other hand, enhances productivity.The utility model overall structure is simple, and is easy and simple to handle, and production cost is low, the characteristics that product yield is high.
Figure of description
Fig. 1 is the structural principle schematic diagram of device.
Embodiment
A kind of preparation method of glyphosate ammonium salt granules, described preparation method directly makes glyphosate ammonium salt granules for glyphosate wet-milling and ammonia are reacted in the gas-solid phase reaction device, wherein the gas-solid phase reaction device comprises the boiling reactor 1 with filter screen 10, be located at the spray gun 7 in the reactor 1, heater 5 and the blower fan 6 that power is provided, passage in reactor 1 and heater 5 and blower fan 6 formation is provided with condenser 3, described reactor 1 and heater 5, blower fan 6, condenser 3 and between form a peripheral passage by pipeline 9, concrete preparation method comprises the steps:
A, displacement: the boiling reactor 1 that is provided with the circulating current passage is continued to pass into nitrogen, with the oxygen in the nitrogen replacement reactor 1, reduce the oxygen content to 0.8% in the reactor 1, guarantee the safety that ammonia passes into;
B, mixing: in the boiling reactor 1 of finishing displacement, add glyphosate wet-milling and ammonia, the mole proportioning of the glyphosate of adding and ammonia is 1: 1, and glyphosate and ammonia react under fluidized state, generates ammonium glyphosate; Circulating current is taken away reaction heat and is removed moisture content in the air-flow through condenser 3 and overcome reaction heat and generated water and cause the unmanageable problem of reacting rear material, to the reaction end, the criterion finished of reaction is for after closing circulating pump, in 5 minutes in the ebullated bed temperature of charge maintenance unchanged;
C, add auxiliary material: add the glyphosate special assistant in the reactant mixture and mix after reaction finishes, wherein the weight ratio that feeds intake of glyphosate and auxiliary agent is 100: 10;
D, granulation: 10% APG liquid is sprayed into ebullated bed by spray gun carry out spraying granulation and make the ammonium glyphosate salt particle;
E, drying: open heater 5, the wet granular that the upper step was made carries out drying, and 50 ℃ of baking temperatures make glyphosate ammonium salt solid preparation.
Glyphosate wet-milling water content is 5% in the steps A, and its moisture content is beneficial to absorbing ammonia and glyphosate reaction.Condenser 3 lower openings are provided with the liquid collecting tank 4 of collecting condensate liquid, and the cold temperature of medium of going is lower than 8 ℃.Condenser 3 is located between the import of reactor 1 outlet and blower fan 6, heater 5 is located between the import of the outlet of blower fan 6 and boiling reactor 1,6 of condenser 3 and blower fans arrange switch valve 12, the needs of one-way gas flow when satisfying drying, the nozzle of spray gun 7 is located between the filter screen 10, the entrance of nitrogen and the injection of granulating with bonding slurry when being used for displacement.
Embodiment 2
A kind of preparation method of glyphosate ammonium salt granules, described preparation method directly makes glyphosate ammonium salt granules for glyphosate wet-milling and ammonia are reacted in the gas-solid phase reaction device, wherein the gas-solid phase reaction device comprises boiling reactor 1 with filter screen 10, is located at spray gun 7, the heater 5 in the reactor 1 and the blower fan 6 of power is provided, path in reactor 1 and heater 5 and blower fan 6 formation is provided with condenser 3, form a peripheral passage by pipeline between described reactor 1 and heater 5, blower fan 6, the condenser 3, concrete preparation method comprises the steps:
A, displacement: the boiling reactor 1 that is provided with the circulating current passage is continued to pass into nitrogen, with the oxygen in the nitrogen replacement reactor 1, reduce the oxygen content to 0.2% in the reactor 1, guarantee the safety that ammonia passes into.
B, mixing: in the boiling reactor 1 of finishing displacement, add glyphosate wet-milling and ammonia, the mole proportioning of the glyphosate of adding and ammonia is 1: 1.5, and glyphosate and ammonia react under fluidized state, generates ammonium glyphosate; Circulating current is taken away reaction heat and is removed moisture content in the air-flow through condenser 3 and overcome reaction heat and generated water and cause the unmanageable problem of reacting rear material, to the reaction end, the criterion finished of reaction is for after closing circulating pump, in 5 minutes in the ebullated bed temperature of charge maintenance unchanged;
C, add auxiliary material: after reaction finishes, add glyphosate special assistant and filler in the reactant mixture and mix, wherein between glyphosate and auxiliary agent and the filler the weight ratio that feeds intake be 100: 50: 100;
D, granulation: 10% APG liquid is sprayed into ebullated bed by spray gun carry out spraying granulation and make the ammonium glyphosate salt particle;
E, drying: open heater 5, the wet granular that made through the upper step is carried out drying, 150 ℃ of baking temperatures make glyphosate ammonium salt solid preparation.
Glyphosate wet-milling water content is 12% in the steps A, its moisture content is beneficial to absorbing ammonia and glyphosate reaction, condenser 3 lower openings are provided with the liquid collecting tank 4 of collecting condensate liquid, the cold temperature of medium of going is lower than 8 ℃, condenser 3 is located between the import of the outlet of reactor 1 and blower fan 6, heater 5 is located between the import of the outlet of blower fan 6 and boiling reactor 1,6 of condenser 3 and blower fans arrange switch valve 12, the needs of one-way gas flow when satisfying drying, the nozzle of spray gun 7 is located between the filter screen 10, the entrance of nitrogen and the injection of granulating with bonding slurry when being used for displacement.
Be that 5.3% glyphosate wet-milling is packed in the reactor 1 with the 100g water content, the ON cycle air pump is in wet-milling to float the dress attitude under the effect of air-flow, open the brine ice switch of condenser 1.The ammoniacal liquor of heating 10% makes the ammonia evaporation pass into reactor 1 by pipeline.React consistent with the circulating current temperature to temperature of charge, close circulating pump, temperature was unchanged in 5 minutes, then judge to react and finish, drop into ammonium sulfate 2g, the rear manual granulation of sieving of surfactant 3g, APG 10g (APG) mixing, the particle that makes places porcelain dish dry at baking oven, 105 ℃ of temperature, 200 minutes time, get soluble granule of glyhosate ammonium 116g.
Be 8.1% glyphosate wet-milling 150kg to reactor 1 interior input water content, pass into nitrogen from the bottom of reactor 1 and bed of material top and replace that the air in the eliminating system stops to replace after making oxygen content be reduced to 1% below.The ON cycle air pump, after the material boiling, the valve of opening ammonia bottle 8 passes into ammonia makes its reaction, and it is that valve-off stops ventilation that intake reaches 17kg.It is consistent with the circulating current temperature to temperature of charge to continue circular response, closes circulating pump, (temperature was unchanged in 5 minutes, then judged to react and finished).Add ammonium sulfate 2kg, surfactant 5kg.APG 10 (APG) is made into underflow and carries out mist projection granulating, then opens heater 5, and the conversion air flow switch is to introducing new wind shelves, by after the heater 5 rising temperature to 150 ℃ material is carried out drying, namely obtains soluble granule of glyhosate ammonium.
Claims (4)
1. the preparation method of a glyphosate ammonium salt granules, it is characterized in that: described preparation method directly makes glyphosate ammonium salt granules for glyphosate wet-milling and ammonia are reacted in gas-solid phase reaction device, wherein gas-solid phase reaction device comprises with the boiling reactor of filter screen (10) (1), be located at the spray gun (7) in the reactor (1), heater (5) and the blower fan (6) of power is provided, passage (9) in reactor (1) and heater (5) and blower fan (6) formation is provided with condenser (3), described reactor (1) and heater (5), blower fan (6), form a peripheral passage by pipeline between the condenser (3), described condenser (3) is located between the import of reactor (1) outlet and blower fan (6), described heater (5) is located between blower fan (6) outlet and boiling reactor (1) import, the nozzle of described spray gun (7) is located between the filter screen (10), the entrance of nitrogen and the injection of granulating with bonding slurry when being used for displacement, concrete preparation method comprises the steps:
A, displacement: to be provided with the circulating current passage boiling reactor (1) continue to pass into nitrogen, with the oxygen in nitrogen replacement reactor (1), reduce below the oxygen content to 1% in the reactor (1); Guarantee passing into of ammonia safety;
B, mixing: in finishing the boiling reactor of displacement (1), add glyphosate wet-milling and ammonia, the mole proportioning of the glyphosate of adding and ammonia is 1:1 ~ 1.5, and glyphosate and ammonia react under fluidized state to the reaction end, generate ammonium glyphosate; The criterion finished of reaction is for after closing circulating pump, in 5 minutes in the ebullated bed temperature of charge maintenance unchanged;
C, add auxiliary material: add the glyphosate special assistant in the reactant mixture and filler mixes after reaction finishes, wherein the weight ratio that feeds intake of glyphosate, auxiliary agent, filler is 100:10 ~ 50:0 ~ 100;
D, granulation: 10% APG liquid is sprayed into ebullated bed by spray gun (7) carry out spraying granulation and make the ammonium glyphosate salt particle;
E, drying: open heater, the wet granular that the upper step was made carries out drying, and 50 ~ 150 ℃ of baking temperatures make glyphosate ammonium salt solid preparation.
2. the preparation method of a kind of glyphosate ammonium salt granules according to claim 1, it is characterized in that: glyphosate wet-milling water content is 5% ~ 12% among the described step B.
3. the preparation method of a kind of glyphosate ammonium salt granules according to claim 1 is characterized in that: described condenser (3) lower openings is provided with the liquid collecting tank (4) of collecting condensate liquid.
4. the preparation method of a kind of glyphosate ammonium salt granules according to claim 1 is characterized in that: between condenser (3) and blower fan (6) switch valve (12) is set, the needs of one-way gas flow when dry to satisfy.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101905143A (en) * | 2010-07-12 | 2010-12-08 | 张惠明 | Batch ammonium glyphosate reactor, ammonium glyphosate water-soluble granule production device and application thereof |
| CN102396522A (en) * | 2011-12-09 | 2012-04-04 | 四川省乐山市福华通达农药科技有限公司 | Glyphosate-ammonium granule aid and preparation method thereof |
| CN103651340B (en) * | 2013-12-25 | 2016-01-20 | 四川省乐山市福华通达农药科技有限公司 | A kind of production technology of glyphosate salt granule |
| CN105039682A (en) * | 2015-08-07 | 2015-11-11 | 辽宁科技大学 | Magnetizing roast and magnetic separation method of refractory iron ores |
| CN105994259A (en) * | 2016-05-20 | 2016-10-12 | 沙隆达集团公司 | Method for rapidly preparing soluble ammonium glyphosate granules |
| CN108094423A (en) * | 2018-02-12 | 2018-06-01 | 江阴市昌盛药化机械有限公司 | The production system and preparation method of soluble granule of glyhosate ammonium |
| CN115594712B (en) * | 2022-10-08 | 2023-12-19 | 湖北泰盛化工有限公司 | Method for continuously ammonifying gas-solid heterogeneous glyphosate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1365252A (en) * | 1999-07-29 | 2002-08-21 | 孟山都技术有限公司 | Process for making ammonium glyphosate powder |
| CN101151971A (en) * | 2006-09-28 | 2008-04-02 | 浙江龙游绿得农药化工有限公司 | Method for producing glyphosate ammonium salt solid preparations |
| CN101401585A (en) * | 2008-09-27 | 2009-04-08 | 浙江金帆达生化股份有限公司 | Method for producing glyphosate ammonium salt solid preparation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1365252A (en) * | 1999-07-29 | 2002-08-21 | 孟山都技术有限公司 | Process for making ammonium glyphosate powder |
| CN101151971A (en) * | 2006-09-28 | 2008-04-02 | 浙江龙游绿得农药化工有限公司 | Method for producing glyphosate ammonium salt solid preparations |
| CN101401585A (en) * | 2008-09-27 | 2009-04-08 | 浙江金帆达生化股份有限公司 | Method for producing glyphosate ammonium salt solid preparation |
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Address after: 614803 Jinsu Town, Wutongqiao District, Leshan City, Sichuan Province Patentee after: Fuhua Tongda Chemical Co.,Ltd. Address before: Qiaogou Town, Wutongqiao, Leshan, Sichuan, 614000 Patentee before: Sichuan Leshan Fuhua Tongda Pesticide Technology Co.,Ltd. |