CN102060872A - Continuous production method of acephate - Google Patents
Continuous production method of acephate Download PDFInfo
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- CN102060872A CN102060872A CN2010105751545A CN201010575154A CN102060872A CN 102060872 A CN102060872 A CN 102060872A CN 2010105751545 A CN2010105751545 A CN 2010105751545A CN 201010575154 A CN201010575154 A CN 201010575154A CN 102060872 A CN102060872 A CN 102060872A
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Abstract
The invention relates to a continuous production method of acephate, which comprises the steps of: continuously acylating in a reactor, hydrolyzing, neutralizing, extracting, desolventizing, crystallizing and recycling mother liquor. The invention solves the problem of low production yield of an acephate device, improves the production capacity by near 300 percent and ensures that the yield reaches 10 thousands t/year. The production process realizes the advanced process technology that the ammonia is used for carrying out neutralization, thereby greatly reducing the emission of wastewater. The continuous production process ensures that the yield of 97 percent acephate raw powder is improved to near 24t/day from 6t/day compared with the batch production process. The device has the advantages of stable production, high automation, greatly reduced labor intensity of operators and greatly improved product yield.
Description
Technical field
The present invention relates to a kind of agricultural chemicals product production method, the preparation method that specifically a kind of acephate serialization is produced.
Background technology
Because country has banned use of high malicious organophosphorus pesticide, originally the shared market of riskiest pesticide must be substituted by some higher effective and lower toxic pesticide, and as organophosphorus pesticide---the acephate of high-efficiency low-toxicity, be the sterilant of output maximum in each insecticide variety in the world at present.The acephate agricultural chemicals is the production development through more than ten years in China, and state of the art improves day by day, and cost descends gradually, and in recent years, its market requirement was great-jump-forward and rises, and has shown good market outlook at present.
Acephate producing process mainly contains two: one is transposition after the first acidylate, and the present domestic pilot scale technology report that has only is not realized industrialization; Another is an acidylate after the first transposition, and domestic nearly all acephate manufacturer all adopts this method at present, but production technology level differs greatly.Reason is that acephate is produced the route complexity, needs through all too many levels such as transposition, acidylate, hydrolysis, neutralization, extraction, precipitation, crystallization, mother liquor recovery set usefulness, wastewater treatments.Because each link all has the optimization of processing condition, and relates to the optimization of engineering equipment, all can cause very big otherness, so the acephate production technology level has very big room for promotion.Analyze the otherness of domestic manufacturer's production technology, and in conjunction with my company's production practical experience and research experiment for many years, reach a conclusion, promptly its production technology level most critical part is embodied in five aspects: the one, and the acidylate state of the art; The 2nd, in and abstraction technique; The 3rd, the precipitation crystallization technique; The 4th, mother liquor recovery set technology; The 5th, the full operation serialization of acephate is produced.Adopting the automatic control technology and the serialization production of full operation is the trend of acephate production development from now on, the report that does not also have the acephate serialization to produce at present.
Summary of the invention
Purpose of the present invention is exactly the defective at existing acephate producing process, the preparation method who provides a kind of acephate serialization to produce by continuous process production, reaches safety, environmental protection production, and reduce discharge of wastewater to greatest extent, realize recycling economy production.
Technical scheme of the present invention is achieved in that it may further comprise the steps:
(1), the acidylate serialization produces: add acephatemet solution 600kg by metering in the import of reaction pump earlier, start reaction pump, slowly add aceticanhydride 370kg in the import of reaction pump; After adding aceticanhydride, import in reaction pump slowly drips catalyzer 15kg, control reaction temperature is at 40～60 ℃, be added dropwise to complete the back 60～70 ℃ of insulations 2 hours, after finishing, the bed material preparation begins continuous dosing production, acephatemet solution input amount 1200kg/h, aceticanhydride 740kg/h, catalyzer 30kg/h, temperature of reaction is controlled at 50 ℃～60 ℃, and reaction mass enters the insulation jar from the tundish overflow, and an insulation jar temperature is controlled at 60～70 ℃, the material acidylate liquid of finishing at last enters the transfer jar from an insulation jar overflow, and acidylate liquid is as the raw material of subsequent processing;
(2), hydrolysis serialization is produced: the import in reaction pump adds acidylate liquid 2000kg, start reaction pump, import in reaction pump adds acidylate liquid, water or mother liquor, control acidylate liquid add-on 2000kg/h, water 1000L/h or mother liquor 2000L/h, control reaction temperature is at 20 ℃～40 ℃, and the hydrolyzed solution that has reacted enters the transfer jar from the tundish overflow, and hydrolyzed solution is as the raw material of subsequent processing;
(3), in and serialization production: the import in reaction pump adds hydrolyzed solution 2000kg, start reaction pump, import in reaction pump adds hydrolyzed solution, solvent and ammonia, control hydrolysis liquid add-on 4000kg/h, solvent 1000L/h, the control pH value is 6～9, and control reaction temperature is at 20 ℃～40 ℃, the neutralizer that has reacted enters the transfer jar from the tundish overflow, and neutralizer is as the raw material of subsequent processing;
(4), extraction serialization production: control neutralizer inlet amount 4000L/h enters the layering tower, the clear liquid that comes out from layering tower top enters the extraction tower bottom, add quantity of solvent 2000L/h simultaneously on extraction tower top, the material that comes out from the extraction tower top is as wastewater treatment operation raw material, becomes the raw material of extraction liquid as subsequent processing after the mixing of materials of coming out in material that comes out from the extraction tower bottom and layering tower bottom;
(5), the precipitation serialization produces: control extraction liquid inlet amount 5000L/h enters well heater, 60 ℃～80 ℃ of control heater temperature, the gas phase of coming out from separator enters condenser condenses and reclaims solvent, liquid phase enters crystallizer and carries out crystallization;
(6), mother liquor is handled serialization production: the mother liquor after the adding crystallization of extraction tower top is centrifugal, inlet amount 2000L/h, add entry 1000L/h～2000L/h in the extraction tower bottom, the jellyfish liquid that comes out from the extraction tower top enters hydrolysis and applies mechanically, and back recovery solvent comes out in the oily room that comes out from the extraction tower bottom.
The present invention's technical scheme preferably is: the processing unit that described acidylate serialization is produced comprises reaction pump, the reaction pump outlet is connected with the import of reactor, the outlet of reactor is connected with the import of tundish, the overflow port of tundish is connected by the import of pipeline with the insulation jar, and the outlet of insulation jar is connected with the import of transfer jar; Described hydrolysis continuous production technology equipment comprises reaction pump, and the reaction pump outlet is connected with the import of reactor, and the outlet of reactor is connected with the import of tundish, and the overflow port of tundish is connected by the import of pipeline with the transfer jar; Comprise reaction pump with continuous production technology equipment in described, the reaction pump outlet is connected with the import of reactor, and the outlet of reactor is connected with the import of tundish, and the overflow port of tundish is connected by the import of pipeline with the transfer jar; Described extraction continuous production technology equipment comprises layering tower and extraction tower, and layering tower top is connected by the opening for feed of pipeline with the extraction tower bottom; Described precipitation continuous production technology equipment comprises well heater, the discharge port at well heater top is connected with the opening for feed of separator, the top discharge mouth of separator is connected with the opening for feed of condenser by pipeline, and the bottom discharge mouth of separator is connected with the crystallizer opening for feed by pipeline.
Because acylation reaction is a faster reaction in earlier stage; the later stage be one than long response time; therefore in continuous reaction; design temperature of reaction in early stage and late phase reaction temperature; adopt low early and high after order; the raising and the apparatus minimizes of favourable shortening reaction times and reaction yield reach the purpose that investment is little, production capacity is big.
Another key problem is the influence of bed material to acylation reaction, because serialization production is to carry out having under the situation of bed material, initial reaction concentration will descend, and certainly will influence reaction process.By a large amount of experiments, we have found and have effectively overcome the factor of bed material to the acylation reaction influence.By control bed material amount and other material inlet amount, make serialization acidylate stable yield more than 97%, improve 2 percentage points of reaction yields.It is steady to observe the continuous acylation reaction process by reaction, and temperature is easy to control, and industrialization can be considered to be cooled with circulating water, and can save a large amount of colds, thereby can reduce the cooling plant related investment significantly.
The intermittent type hydrolysis is fairly simple; but the continuous hydrolyzing situation has just changed; at first be to contain partial solvent in the acidylate liquid; when the acidylate liquid that contains solvent with after water mixes; will form tiny oil droplet; the aceticanhydride that a part has neither part nor lot in reaction will take place wrapped up by oil droplet, do not reach the purpose of thorough hydrolysis.Thereby cause that operation down---neutralization reaction generates the ethanamide content overproof, influences quality product.Therefore,, must control bed material amount and certain residence time, thereby guarantee the thoroughness of hydrolysis around continuous hydrolyzing.
Employing is logical ammonia in hydrolyzed solution, realize the serialization neutralization reaction by control PH=6～9, the benefit of doing like this is that the neutralization reaction endpoint is easy, can save to join the ammoniacal liquor operation, reduce the loss of ammonia, and reduce relevant labour cost and relevant device investment.
Present batch process extraction tower, throughput is little, and the waste water after the extraction contains acephate 1.5～2.5%, and by adopting the layering of neutralizer elder generation, extraction mixes layering liquid then with extraction liquid again, the extraction liquid of formation specific concentrations.In this process, owing to contained a large amount of solvents in the neutralizer, again by layering behind a certain amount of solvent of adding, just can reduce the neutralizer that major part is advanced extraction tower, alleviate the extraction tower load, by this technological improvement, just can improve extraction tower ability twice, reduce nearly 1,000,000 yuan of investment.After improving, extraction back waste water contains acephate and is reduced to 0.3～0.8%, thereby can improve 2 percentage points of yields.
Because batch production is taked thin-film evaporator negative pressure precipitation mode, thin-film evaporator equipment can not maximize, and employing normal pressure precipitation, pass through equipment enlarging, can realize the serialization distillation, thereby continuous crystallization becomes possibility, in addition by crystallization condition optimization, can produce 97% former powder and the former powder of 98.5% high-content, satisfy the high-end market customer demand.
It is a difficult problem that mother liquor is handled: general treatment process is by three precipitations, and the former powder of part acephate is regained in three crystallizations, remaining waste liquid just have to emit, and shortcoming is by three precipitations, complex process, lose greatlyyer, equipment is many, is unfavorable for that throughput enlarges.Handle serialization production by mother liquor, adopt the phase-splitting extraction to remove impurity, thereby simplify the mother liquor aftertreatment technology, reach and enhance productivity and yield, reduce the purpose of discharging of waste liquid.
Generally speaking, this invention has solved the production output bottleneck of acephate device, improves throughput nearly 300%.Make output reach 10,000 tons/year.This production technique has realized that wastewater discharge reduces greatly with ammonia neutral advanced technologies technology; This continuous production technology comparison batch production technology makes the former powder yield of 97% acephate bring up to nearly 24 tons/day from 6 tons/day, and this device is produced stable, the level of automation height, and labor intensity of operating staff significantly reduces, and product production significantly improves.
Description of drawings
Accompanying drawing 1: be acidylate continuous production process synoptic diagram of the present invention
Accompanying drawing 2: be hydrolysis continuous production process synoptic diagram of the present invention
Accompanying drawing 3: among the present invention and the continuous production process synoptic diagram
Accompanying drawing 4: for the present invention extracts the continuous production process synoptic diagram
Accompanying drawing 5: be precipitation continuous production process synoptic diagram of the present invention
Accompanying drawing 6: for mother liquor of the present invention is handled the continuous production process synoptic diagram
Embodiment
The invention will be further described below in conjunction with example and schematic flow sheet:
1, the acidylate serialization is produced
1.1 embodiment one
Earlier add acephatemet solution 600kg in the import of reaction pump 1.1, start reaction pump 1.1, slowly add aceticanhydride 370kg in the import of reaction pump 1.1 by metering; After adding aceticanhydride, slowly drip catalyzer 15kg in the import of reaction pump, open the recirculated water terminal valve of water cooler simultaneously, the temperature of controlling reactor 1.2 is at 60 ℃.Be added dropwise to complete the back 60～70 ℃ of insulations 2 hours; after finishing, the bed material preparation begins continuous dosing production; acephatemet solution input amount 1200kg/h; aceticanhydride 740kg/h, catalyzer 30kg/h, temperature of reaction is controlled at 60 ℃; reaction mass enters insulation jar 1.4 from tundish 1.3 overflows; an insulation jar temperature is controlled at 60～70 ℃, and the material acidylate liquid of finishing at last enters transfer jar 1.5 from insulation jar 4 overflows, and acidylate liquid is as the raw material of subsequent processing.Reaction yield 97.8%.
1.2 embodiment two
Earlier add acephatemet solution 600kg in the import of reaction pump 1.1, start reaction pump 1.1, slowly add aceticanhydride 370kg in the import of reaction pump 1.1 by metering; After adding aceticanhydride, slowly drip catalyzer 15kg in the import of reaction pump 1.1, open the recirculated water terminal valve of water cooler simultaneously, controlling reactor 1.2 temperature are at 50 ℃.Be added dropwise to complete the back 50～60 ℃ of insulations 2 hours; after finishing, the bed material preparation begins continuous dosing production; acephatemet solution input amount 1200kg/h; aceticanhydride 740kg/h, catalyzer 30kg/h, temperature of reaction is controlled at 50 ℃; reaction mass enters insulation jar 1.4 from tundish 1.3 overflows; an insulation jar temperature is controlled at 50～60 ℃, and the material acidylate liquid of finishing at last enters transfer jar 1.5 from insulation jar 1.4 overflows, and acidylate liquid is as the raw material of subsequent processing.Reaction yield 97.2%.
1.3 embodiment three
Earlier add acephatemet solution 600kg in the import of reaction pump 1.1, start reaction pump 1.1, slowly add aceticanhydride 370kg in the import of reaction pump 1.1 by metering; After adding aceticanhydride, slowly drip catalyzer 15kg in the import of reaction pump 1.1, open the recirculated water terminal valve of water cooler simultaneously, controlling reactor 1.2 temperature are at 40 ℃.Be added dropwise to complete the back 40～50 ℃ of insulations 2 hours; after finishing, the bed material preparation begins continuous dosing production; acephatemet solution input amount 1200kg/h; aceticanhydride 740kg/h, catalyzer 30kg/h, temperature of reaction is controlled at 40 ℃; reaction mass enters insulation jar 1.4 from tundish 1.3 overflows; an insulation jar temperature is controlled at 40～50 ℃, and the material acidylate liquid of finishing at last enters transfer jar 1.5 from insulation jar 1.4 overflows, and acidylate liquid is as the raw material of subsequent processing.Reaction yield 96.5%.
2, hydrolysis serialization is produced
2.1 embodiment one
Import in reaction pump 2.1 adds acidylate liquid 2000kg; start reaction pump 2.1; import in reaction pump 2.1 adds acidylate liquid and water (or mother liquor); control acidylate liquid add-on 2000kg/h; water 1000L/h (or mother liquor 2000L/h); open the recirculated water terminal valve of water cooler simultaneously, controlling reactor 2.2 temperature are at 40 ℃.The material hydrolyzed solution that reaction is finished enters transfer jar 2.4 from tundish 2.3 overflows, and hydrolyzed solution is as the raw material of subsequent processing.Reaction yield 99.0%.
2.2 embodiment two
Import in reaction pump 2.1 adds acidylate liquid 2000kg; start reaction pump 2.1; import in reaction pump 2.1 adds acidylate liquid and water (or mother liquor); control acidylate liquid add-on 2000kg/h; water 1000L/h (or mother liquor 2000L/h); open the recirculated water terminal valve of water cooler simultaneously, controlling reactor 2.2 temperature are at 30 ℃.The material hydrolyzed solution that reaction is finished enters transfer jar 2.4 from tundish 2.3 overflows, and hydrolyzed solution is as the raw material of subsequent processing.Reaction yield 98.6%.
2.3 embodiment three
Import in reaction pump 2.1 adds acidylate liquid 2000kg; start reaction pump 2.1; import in reaction pump 2.1 adds acidylate liquid and water (or mother liquor); control acidylate liquid add-on 2000kg/h; water 1000L/h (or mother liquor 2000L/h); open the salt solution terminal valve of water cooler simultaneously, controlling reactor 2.2 temperature are at 20 ℃.The material hydrolyzed solution that reaction is finished enters transfer jar 2.4 from tundish 2.3 overflows, and hydrolyzed solution is as the raw material of subsequent processing.Reaction yield 99.3%.
3, in and serialization production
3.1 embodiment one
Import in reaction pump 3.1 adds hydrolyzed solution 2000kg, start reaction pump 3.1, import in reaction pump 3.1 adds hydrolyzed solution, solvent and ammonia, control hydrolysis liquid add-on 4000kg/h, solvent 1000L/h, add ammonia control pH value 9, open the salt solution terminal valve of water cooler simultaneously, controlling reactor 3.2 temperature are at 40 ℃.The material neutralizer that reaction is finished enters transfer jar 3.4 from tundish 3.3 overflows, and neutralizer is as the raw material of subsequent processing.Reaction yield 97.0%.
3.2 embodiment two
Import in reaction pump 3.1 adds hydrolyzed solution 2000kg, start reaction pump 3.1, import in reaction pump 3.1 adds hydrolyzed solution, solvent and ammonia, control hydrolysis liquid add-on 4000kg/h, solvent 1000L/h, add ammonia control pH value 6, open the salt solution terminal valve of water cooler simultaneously, controlling reactor 3.2 temperature are at 30 ℃.The material neutralizer that reaction is finished enters transfer jar 3.4 from tundish 3.3 overflows, and neutralizer is as the raw material of subsequent processing.Reaction yield 97.2%.
3.3 embodiment three
Import in reaction pump 3.1 adds hydrolyzed solution 2000kg, start reaction pump 3.1, import in reaction pump 3.1 adds hydrolyzed solution, solvent and ammonia, control hydrolysis liquid add-on 4000kg/h, solvent 1000L/h, add ammonia control pH value 7, open the salt solution terminal valve of water cooler simultaneously, controlling reactor 3.2 temperature are at 20 ℃.The material neutralizer that reaction is finished enters transfer jar 3.4 from tundish 3.3 overflows, and neutralizer is as the raw material of subsequent processing.Reaction yield 97.5%.
4, extraction serialization production
4.1 embodiment one
Control neutralizer inlet amount 4000L/h enters layering tower 4.1, the clear liquid that comes out from layering tower 4.1 tops enters extraction tower 4.2 bottoms, add quantity of solvent 2000L/h simultaneously on extraction tower top, the material that comes out from extraction tower 4.2 tops is as wastewater treatment operation raw material, becomes the raw material of extraction liquid as subsequent processing after the mixing of materials of coming out in material that comes out from extraction tower 4.2 bottoms and layering tower 4.1 bottoms.Reaction yield 99.0%.
4.2 embodiment two
Control neutralizer inlet amount 3000L/h enters layering tower 4.1, the clear liquid that comes out from layering tower 4.1 tops enters extraction tower 4.2 bottoms, add quantity of solvent 1500L/h simultaneously on extraction tower top, the material that comes out from extraction tower 4.2 tops is as wastewater treatment operation raw material, becomes the raw material of extraction liquid as subsequent processing after the mixing of materials of coming out in material that comes out from extraction tower 4.2 bottoms and layering tower 4.1 bottoms.Reaction yield 99.2%.
5, the precipitation serialization is produced
5.1 embodiment one
Control extraction liquid inlet amount 5000L/h enters well heater 5.1,60 ℃ of control heater temperature, and the gas phase of coming out from separator 5.2 enters condenser 5.4 condensations recovery solvent, and liquid phase enters crystallizer 5.3 and carries out crystallization.Precipitation yield 99.1%.
5.2 embodiment two
Control extraction liquid inlet amount 5000L/h enters well heater 5.1,70 ℃ of control heater temperature, and the gas phase of coming out from separator 5.2 enters condenser 5.4 condensations recovery solvent, and liquid phase enters crystallizer 5.3 and carries out crystallization.Precipitation yield 98.6%.
5.3 embodiment three
Control extraction liquid inlet amount 5000L/h enters well heater 5.1,80 ℃ of control heater temperature, and the gas phase of coming out from separator 5.2 enters condenser 5.4 condensations recovery solvent, and liquid phase enters crystallizer 5.3 and carries out crystallization.Precipitation yield 98.3%.
6, mother liquor is handled serialization production
6.1 embodiment one
Mother liquor after the adding crystallization of extraction tower 6 tops is centrifugal, inlet amount 2000L/h adds entry 2000L/h in extraction tower 6 bottoms.The jellyfish liquid that comes out from extraction tower 6 tops enters hydrolysis and applies mechanically, and reclaims solvent after the greasy dirt that comes out from extraction tower 6 bottoms comes out.Mother liquor is handled yield 100%.
6.2 embodiment two
Mother liquor after the adding crystallization of extraction tower 6 tops is centrifugal, inlet amount 2000L/h adds entry 1500L/h in extraction tower 6 bottoms.The jellyfish liquid that comes out from extraction tower 6 tops enters hydrolysis and applies mechanically, and reclaims solvent after the greasy dirt that comes out from extraction tower 6 bottoms comes out.Mother liquor is handled yield 100%.
6.3 embodiment three
Mother liquor after the adding crystallization of extraction tower 6 tops is centrifugal, inlet amount 2000L/h adds entry 1000L/h in extraction tower 6 bottoms.The jellyfish liquid that comes out from extraction tower 6 tops enters hydrolysis and applies mechanically, and reclaims solvent after the greasy dirt that comes out from extraction tower 6 bottoms comes out.Mother liquor is handled yield 100%.
Claims (6)
1. the preparation method that produces of an acephate serialization, it may further comprise the steps:
(1), the acidylate serialization produces: add acephatemet solution 600kg by metering in the import of reaction pump earlier, start reaction pump, slowly add aceticanhydride 370kg in the import of reaction pump; After adding aceticanhydride, import in reaction pump slowly drips catalyzer 15kg, control reaction temperature is at 40～60 ℃, be added dropwise to complete the back 60～70 ℃ of insulations 2 hours, after finishing, the bed material preparation begins continuous dosing production, acephatemet solution input amount 1200kg/h, aceticanhydride 740kg/h, catalyzer 30kg/h, temperature of reaction is controlled at 50 ℃～60 ℃, and reaction mass enters the insulation jar from the tundish overflow, and an insulation jar temperature is controlled at 60～70 ℃, the material acidylate liquid of finishing at last enters the transfer jar from an insulation jar overflow, and acidylate liquid is as the raw material of subsequent processing;
(2), hydrolysis serialization is produced: the import in reaction pump adds acidylate liquid 2000kg, start reaction pump, import in reaction pump adds acidylate liquid, water or mother liquor, control acidylate liquid add-on 2000kg/h, water 1000L/h or mother liquor 2000L/h, control reaction temperature is at 20 ℃～40 ℃, and the hydrolyzed solution that has reacted enters the transfer jar from the tundish overflow, and hydrolyzed solution is as the raw material of subsequent processing;
(3), in and serialization production: the import in reaction pump adds hydrolyzed solution 2000kg, start reaction pump, import in reaction pump adds hydrolyzed solution, solvent and ammonia, control hydrolysis liquid add-on 4000kg/h, solvent 1000L/h, the control pH value is 6～9, and control reaction temperature is at 20 ℃～40 ℃, the neutralizer that has reacted enters the transfer jar from the tundish overflow, and neutralizer is as the raw material of subsequent processing;
(4), extraction serialization production: control neutralizer inlet amount 4000L/h enters the layering tower, the clear liquid that comes out from layering tower top enters the extraction tower bottom, add quantity of solvent 2000L/h simultaneously on extraction tower top, the material that comes out from the extraction tower top is as wastewater treatment operation raw material, becomes the raw material of extraction liquid as subsequent processing after the mixing of materials of coming out in material that comes out from the extraction tower bottom and layering tower bottom;
(5), the precipitation serialization produces: control extraction liquid inlet amount 5000L/h enters well heater, 60 ℃～80 ℃ of control heater temperature, the gas phase of coming out from separator enters condenser condenses and reclaims solvent, liquid phase enters crystallizer and carries out crystallization;
(6), mother liquor is handled serialization production: the mother liquor after the adding crystallization of extraction tower top is centrifugal, inlet amount 2000L/h, add entry 1000L/h～2000L/h in the extraction tower bottom, the jellyfish liquid that comes out from the extraction tower top enters hydrolysis and applies mechanically, and back recovery solvent comes out in the oily room that comes out from the extraction tower bottom.
2. the preparation method that a kind of acephate serialization according to claim 1 is produced; the processing unit that wherein said acidylate serialization is produced comprises reaction pump; the reaction pump outlet is connected with the import of reactor; the outlet of reactor is connected with the import of tundish; the overflow port of tundish is connected by the import of pipeline with the insulation jar, and the outlet of insulation jar is connected with the import of transfer jar.
3. the preparation method that a kind of acephate serialization according to claim 1 is produced, wherein said hydrolysis continuous production technology equipment comprises reaction pump, the reaction pump outlet is connected with the import of reactor, the outlet of reactor is connected with the import of tundish, and the overflow port of tundish is connected by the import of pipeline with the transfer jar.
4. the preparation method that a kind of acephate serialization according to claim 1 is produced, comprise reaction pump with continuous production technology equipment in wherein said, the reaction pump outlet is connected with the import of reactor, the outlet of reactor is connected with the import of tundish, and the overflow port of tundish is connected by the import of pipeline with the transfer jar.
5. the preparation method that a kind of acephate serialization according to claim 1 is produced, wherein said extraction continuous production technology equipment comprises layering tower and extraction tower, layering tower top is connected by the opening for feed of pipeline with the extraction tower bottom.
6. the preparation method that a kind of acephate serialization according to claim 1 is produced, wherein said precipitation continuous production technology equipment comprises well heater, the discharge port at well heater top is connected with the opening for feed of separator, the top discharge mouth of separator is connected with the opening for feed of condenser by pipeline, and the bottom discharge mouth of separator is connected with the crystallizer opening for feed by pipeline.
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| CN102389765A (en) * | 2011-10-12 | 2012-03-28 | 河南迈奇能源技术有限公司 | Electrolyte processing equipment |
| CN104262390A (en) * | 2014-09-26 | 2015-01-07 | 湖北沙隆达股份有限公司 | Continuous production method of high-efficiency and low-toxicity pesticide-acephate |
| CN106831859A (en) * | 2017-01-23 | 2017-06-13 | 湘潭大学 | The circulation recovery method of easy volatile solvent |
| CN110015986A (en) * | 2019-04-29 | 2019-07-16 | 山东汇盟生物科技股份有限公司 | A kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- |
| CN112592368A (en) * | 2020-12-10 | 2021-04-02 | 安道麦股份有限公司 | Method for synthesizing acephate |
| WO2021152443A1 (en) * | 2020-01-31 | 2021-08-05 | Upl Limited | A continuous flow process for preparation of acephate and its intermediates |
| CN116396325A (en) * | 2023-02-01 | 2023-07-07 | 浙江泰达作物科技有限公司 | Method for efficiently preparing acephate by continuous flow microreactor |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102389765A (en) * | 2011-10-12 | 2012-03-28 | 河南迈奇能源技术有限公司 | Electrolyte processing equipment |
| CN104262390A (en) * | 2014-09-26 | 2015-01-07 | 湖北沙隆达股份有限公司 | Continuous production method of high-efficiency and low-toxicity pesticide-acephate |
| CN106831859A (en) * | 2017-01-23 | 2017-06-13 | 湘潭大学 | The circulation recovery method of easy volatile solvent |
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| CN110015986A (en) * | 2019-04-29 | 2019-07-16 | 山东汇盟生物科技股份有限公司 | A kind of chloro- 2- chloromethyl -4- cyanobutyraldehyde cyclization device of 2- |
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| WO2021152443A1 (en) * | 2020-01-31 | 2021-08-05 | Upl Limited | A continuous flow process for preparation of acephate and its intermediates |
| EP4097114A4 (en) * | 2020-01-31 | 2024-03-13 | Upl Ltd | A continuous flow process for preparation of acephate and its intermediates |
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