CN104844414A - Equipment and process for recovering glyphosate solvent during production with glycine method - Google Patents
Equipment and process for recovering glyphosate solvent during production with glycine method Download PDFInfo
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Abstract
The invention provides equipment and a process for recovering a glyphosate solvent during production with glycine method, particularly relates to a glyphosate solvent recovery continuous production and gas-phase method recovery technology, and aims to overcome the defects of operation intermittence, high labor intensity, high energy consumption, low methyl chloride purity and the like in the prior art. Continuous production in an entire procedure is realized, so that the content of methyl chloride is increased to 99.9 percent, and the energy consumption is lowered. The equipment and process are widely applied to the field of glyphosate production.
Description
Technical field
The present invention relates to a kind of producing glyphosate by using glycine solvent recuperation new installation and technique thereof, be specifically related to vapor phase process recycling design technology.
Background technology
Glyphosate is a kind of efficient, the Uptake and translocation weedicide that low toxicity, wide spectrum go out natural disposition researched and developed in nineteen seventies by About Monsanto Chemicals, occupy the first place of world pesticide sales volume for years, along with transgenosis glyphosate resistant crops is as the establishing in large scale of soybean, corn etc. in recent years, the whole world continues to increase the demand of glyphosate.Current domestic glyphosate main flow production technique has two lines: glycine method (single stage method) and iminodiacetic acid (salt) acid system (two-step approach, first synthesize pmida98, again pmida98 oxidation is called glyphosate), the iminodiacetic acid (salt) acid system of external production technique then mainly About Monsanto Chemicals.Amino acetic acid in China synthetic route be first first in synthesis reactor through depolymerization, addition, condensation; Condensated liquid squeezes into that depickling still is hydrolyzed again, precipitation, depickling; The mixed gas (methyl chloride, dilute methanol) in hydrolysis precipitation stage is through three grades of condensations, and phlegma enters dilute methanol storage tank, and uncooled tail gas enters methyl chloride recovery system and reclaims.Enter Distallation systm after dilute methanol neutralizes again to reclaim; This technological operation is discontinuous, and labor intensive is large, and yield is low, and energy consumption is high.
Summary of the invention
The object of invention
The present invention is directed to existing existing glyphosate operational path long reaction time, operate discontinuous, yield is low, and energy consumption is high, and this invention can realize continuous prodution, reduces energy consumption, improves the quality of glyphosate yield and methyl chloride.
A kind of producing glyphosate by using glycine solvent reclaimer, glyphosate tail gas carrier pipe is connected with neutralizing tower through carrier pipe with diluted alkaline storage tank, neutralizing tower top is connected with gas mixture storage tank through carrier pipe, be connected with in the middle part of dehydration tower through carrier pipe again after the top of gas mixture storage tank is connected with dehydration tower ventilating fan, dehydration tower top is connected with dehydration tower condenser through carrier pipe, dehydration tower condenser is connected with dehydration tower gas-liquid separator through carrier pipe, dehydration tower gas-liquid separator is connected with methanol column ventilating fan through carrier pipe, be connected with the surge tank that refluxes with dehydration tower again after carrier pipe converges respectively bottom dehydration tower gas-liquid separator bottom dehydration tower condenser, point two-way after dehydration tower backflow surge tank is connected with dehydration tower reflux pump, one tunnel is connected with the middle part of methanol column, one tunnel is connected with dehydration tower top, form circulation loop,
In above-mentioned, from dehydration tower reflux pump carrier pipe with together enter in the middle part of methanol column from the carrier pipe of dehydration tower gas-liquid separator through methanol column ventilating fan, methanol column top through carrier pipe successively with methylal first-stage condenser, methylal secondary condenser connects, two-way is divided through carrier pipe in methylal secondary condenser top, directly be connected with methyl chloride withdrawing can after one tunnel is connected with gas-liquid separator, one tunnel is connected through carrier pipe and the methanol column surge tank that refluxes, methanol column backflow surge tank is connected with methanol column reflux pump through carrier pipe, methanol column reflux pump divides two-way through carrier pipe, one tunnel is connected with methanol column top through carrier pipe, form circulation loop, one tunnel is connected with methyl alcohol blowdown condenser through carrier pipe, methyl alcohol blowdown condenser is connected with methylal finished pot top through carrier pipe, methylal finished pot top is connected with methylal finished pot top after carrier pipe is connected with reflux exchanger again, form circulation loop.
Described neutralizing tower bottom is also provided with neutralizing tower well heater, be connected with neutralizing tower reflux pump after carrier pipe converges with neutralizing tower heater base bottom neutralizing tower, neutralizing tower reflux pump divides two-way through carrier pipe, one tunnel is connected with neutralizing tower top, form circulation loop, a road is connected with in the middle part of dehydration tower.
Two-way is divided through carrier pipe bottom described dehydration tower, carrier pipe bottom the carrier pipe at one tunnel and neutralizing tower well heater top, neutralizing tower, the carrier pipe of gas mixture storage tank are connected with sewage plant through carrier pipe after converging, one tunnel is connected with waste water discharging pump through carrier pipe, and waste water discharging pump divides two-way through carrier pipe; After the carrier pipe of one tunnel and gas mixture storage tank bottom, the carrier pipe of neutralizing tower well heater bottom converge, be connected with the carrier pipe retaining a percentage of the total profits for the enterprise's own use tower bottom from waste water, one tunnel is connected with waste water surge tank, after carrier pipe bottom waste water surge tank is connected with profit reduction and reserving tower fresh feed pump, then retains a percentage of the total profits for the enterprise's own use top of tower with waste water and be connected.
Described gas mixture tank bottom is connected with bottom dehydration tower after carrier pipe is connected with condenser discharging pump again.
Described waste water profit reduction and reserving top of tower is also connected with gas mixture storage tank bottom through carrier pipe; Waste water surge tank top is also provided with the backflow carrier pipe of waste water tank blowdown condenser.
Described dehydration tower backflow surge tank top also arranges the carrier pipe converged to dehydration tower gas-liquid separator carrier pipe with dehydration tower condenser.
Be connected with methyl alcohol finished product condenser after carrier pipe is connected with methyl alcohol discharging pump bottom described methanol column, methyl alcohol finished product condenser is connected with methyl alcohol finished pot through carrier pipe again, and methyl alcohol finished pot top is also provided with the backflow carrier pipe of methylal blowdown condenser.
Described methanol column bottom is also connected with methanol column reboiler, is connected bottom methanol column through carrier pipe with methanol column reboiler after carrier pipe converges with decontamination station.
A kind of producing glyphosate by using glycine solvent recovery process, specifically comprises the steps:
From glyphosate synthesis post comprise methyl chloride, methyl alcohol, methylal, water vapour mixture and mass concentration be 25%-30% liquid caustic soda together with blast neutralizing tower to be neutralized to pH be 7-8, in and materials at bottom of tower squeeze into dehydration tower through neutralizing tower heater heats to 60-80 DEG C of rear portion, a part squeezes into neutralizing tower top, form circulation, neutralizing tower overhead gas enters gas mixture surge tank, then blasts dehydration tower;
Dehydration column overhead gas is after condensation, gas-liquid separator separates, gas enters methanol column through methanol column ventilating fan, liquid gets back to dehydration tower backflow surge tank through condensation, liquid in dehydration tower backflow surge tank also enters methanol column through dehydration tower reflux pump, enters dehydration tower completely form circulation without dehydration;
At the bottom of dehydration tower tower, mixed solution enters waste water surge tank; Dehydration column overhead gas also enters dehydration tower backflow surge tank through condenser condenses, part backflow, and a part delivers to methanol column through dehydration tower reflux pump again after condensation;
At the bottom of methanol column tower, mixed solution is through condensation, and phlegma reclaims and obtains methyl alcohol, and the gas that methanol column tower top is not condensed reclaims and obtains methyl chloride after condensed in two stages, gas-liquid separation; For condensation, gas-liquid separation are delivered to methylal return tank residual night completely, after emptying methyl alcohol, methylal is obtained through reflux rear portion extraction gas, a part delivers to methanol column top, carry out next step circulation, in whole process, it is 65 ± 5 DEG C that temperature bottom methanol column controls, and the temperature on methanol column top controls to be 35 ± 2 DEG C;
The waste liquid of dehydration tower inner bottom part is delivered to waste water profit reduction and reserving tower through waste water surge tank, and after profit reduction and reserving, mixed gas sends into gas mixture storage tank, and neutralizing tower well heater delivered to by the mixed solution after profit reduction and reserving;
The waste water that neutralizing tower well heater, neutralizing tower, gas mixture storage tank, dehydration tower, methanol column produce enters waste water station and processes.
By the linking of continuous device, be that whole Production Flow Chart can continual continuous prodution.Thus in existing situation, can realize expanding production dilatation, save freezing energy consumption and steam energy consumption.Methyl chloride first goes out to remove impurity through Distallation systm, and the main content of methyl chloride can bring up to 99.9%.Continuous prodution level of automation is high, decreases the safety and environmental protection accident that human factor causes.High-temperature tail gas enters the temperature of dehydration tower utilization itself, and low-boiling-point substance is gone out from tower top automatically, and high boiling material falls at the bottom of tower and enters sewage works, which decreases the COD of waste water, decreases the pollution of waste water to environment.Overall theory, this invention has good economy, environmental protection and social benefit, and application prospect is extensive.
Accompanying drawing explanation
Fig. 1 is producing glyphosate by using glycine solvent recovery unit.
Wherein, 1. neutralizing tower, 2. gas mixture storage tank, 3. dehydration tower ventilating fan, 4. dehydration tower, 5. dehydration tower condenser, 6. dehydration tower gas-liquid separator, 7. methanol column ventilating fan, 8. dehydration tower backflow surge tank, 9. dehydration tower reflux pump, 10. methanol column, 11. methylal first-stage condenser, 12. methylal secondary condensers, 13. gas-liquid separators, 14. methanol column reflux accumulator, 15. methanol column reflux pumps, 16. methyl alcohol blowdown condensers, 17. methylal finished pots, 18. condensers, 19. neutralizing tower well heaters, 20. neutralizing tower reflux pumps, 21. waste water discharging pumps, 22. waste water profit reduction and reserving towers, 23. waste water surge tanks, 24. profit reduction and reserving tower fresh feed pumps, 25. condenser discharging pumps, 26. waste water tank blowdown condensers, 27. methyl alcohol discharging pumps, 28. methanol column reboilers, 29. methyl alcohol finished pots, 30. methyl alcohol finished product water coolers, 31. methylal emptying water coolers, 32. diluted alkaline storage tanks.
Embodiment
Embodiment 1
Producing glyphosate by using glycine can produce a large amount of mixed gass such as methyl chloride and methyl alcohol, methylal, water vapor in precipitation, deacidification.Traditional technique is by mixed gas through three grades of condensations, and methyl alcohol, methylal, water (dilute methanol) are condensed and enter storage tank, and the methyl chloride (carrying methyl alcohol, methylal secretly) not having condensation to get off enters Chloromethane recovery device.Dilute methanol with liquid caustic soda in and, neutralizer is squeezing into distillation system, reclaims methyl alcohol methylal.Traditional process energy consumption is high, in methyl chloride removal process every consumption higher, and methyl chloride content is on the low side.By research of technique, invent a kind of vapor phase process recovery process.This technique is that the mixed gas in precipitation, deacidification is directly entered neutralizing tower, dehydration tower, methanol column recovery methyl alcohol without condensation, methylal, waste water at the bottom of dehydration tower tower enters waste water rectifying tower and again extracts methyl alcohol, methylal, and at the bottom of high temperature tower, waste water enters neutralizing tower preheater and temperature rise heat exchanger.This technique is low, the heat energy recycling of energy consumption not only, and the content of methyl chloride can bring up to more than 99.9%.First the invention provides a kind of producing glyphosate by using glycine solvent reclaimer, glyphosate tail gas carrier pipe is connected with neutralizing tower 1 through carrier pipe with diluted alkaline storage tank 32, neutralizing tower 1 top is connected with gas mixture storage tank 2 through carrier pipe, be connected with in the middle part of dehydration tower 4 through carrier pipe again after the top of gas mixture storage tank 2 is connected with dehydration tower ventilating fan 3, dehydration tower 4 top is connected with dehydration tower condenser 5 through carrier pipe, dehydration tower condenser 5 is connected with dehydration tower gas-liquid separator 6 through carrier pipe, dehydration tower gas-liquid separator 6 is connected with methanol column ventilating fan 7 through carrier pipe, be connected with the surge tank 8 that refluxes with dehydration tower again after carrier pipe converges respectively bottom dehydration tower gas-liquid separator 6 bottom dehydration tower condenser 5, point two-way after dehydration tower backflow surge tank 8 is connected with dehydration tower reflux pump 9, one tunnel is connected with the middle part of methanol column 10, one tunnel is connected with dehydration tower 4 top, form circulation loop, in above-mentioned, from dehydration tower reflux pump 9 carrier pipe with together enter in the middle part of methanol column 10 from dehydration tower gas-liquid separator 6 through the carrier pipe of methanol column ventilating fan 7, methanol column 10 top through carrier pipe successively with methylal first-stage condenser 11, methylal secondary condenser 12 connects, two-way is divided through carrier pipe in methylal secondary condenser 12 top, one tunnel is connected with gas-liquid separator 13 and is directly connected with methyl chloride withdrawing can afterwards, one tunnel is connected through carrier pipe and the methanol column surge tank 14 that refluxes, methanol column backflow surge tank 14 is connected with methanol column reflux pump 15 through carrier pipe, methanol column reflux pump 15 divides two-way through carrier pipe, one tunnel is connected with methanol column 10 top through carrier pipe, form circulation loop, one tunnel is connected with methyl alcohol blowdown condenser 16 through carrier pipe, methyl alcohol blowdown condenser 16 is connected with methylal finished pot 17 top through carrier pipe, methylal finished pot 17 top is connected with methylal finished pot 17 top after carrier pipe is connected with reflux exchanger 18 again, form circulation loop.
Described neutralizing tower 1 bottom is also provided with neutralizing tower well heater 19, be connected with neutralizing tower reflux pump 20 after carrier pipe converges with bottom neutralizing tower well heater 19 bottom neutralizing tower 1, neutralizing tower reflux pump 20 divides two-way through carrier pipe, one tunnel is connected with neutralizing tower 1 top, form circulation loop, a road is connected with in the middle part of dehydration tower 4.
Two-way is divided through carrier pipe bottom described dehydration tower 4, carrier pipe bottom the carrier pipe at one tunnel and neutralizing tower well heater 19 top, neutralizing tower 1, the carrier pipe of gas mixture storage tank 2 are connected with sewage plant through carrier pipe after converging, one tunnel is connected with waste water discharging pump 21 through carrier pipe, and waste water discharging pump 21 divides two-way through carrier pipe; After the carrier pipe of one tunnel and gas mixture storage tank 2 bottom, the carrier pipe of neutralizing tower well heater 19 bottom converge, be connected with the carrier pipe retained a percentage of the total profits for the enterprise's own use bottom tower 22 from waste water, one tunnel is connected with waste water surge tank 23, after carrier pipe bottom waste water surge tank 23 is connected with profit reduction and reserving tower fresh feed pump 24, then retains a percentage of the total profits for the enterprise's own use tower 22 top with waste water and be connected.
Be connected again with bottom dehydration tower 4 after carrier pipe is connected with condenser discharging pump 25 bottom described gas mixture storage tank 2.
Described waste water profit reduction and reserving tower 22 top is also connected with gas mixture storage tank 2 bottom through carrier pipe; Waste water surge tank 23 top is also provided with the backflow carrier pipe of waste water tank blowdown condenser 26.
Described dehydration tower backflow surge tank 8 top also arranges the carrier pipe converged with dehydration tower condenser 5 to dehydration tower gas-liquid separator 6 carrier pipe.
Be connected with methyl alcohol finished product condenser 30 again after carrier pipe is connected with methyl alcohol discharging pump 27 bottom described methanol column 10, methyl alcohol finished product condenser 30 is connected with methyl alcohol finished pot 29 through carrier pipe, and methyl alcohol finished pot 29 top is also provided with the backflow carrier pipe of methylal blowdown condenser 31.
Described methanol column 10 bottom is also connected with methanol column reboiler 28, is connected bottom methanol column 10 through carrier pipe with methanol column reboiler 28 after carrier pipe converges with decontamination station.
Mixed gas from glyphosate synthesis post is blasted neutralizing tower by gas blower in the present invention and liquid caustic soda neutralizes, and materials at bottom of tower squeezes into dehydration tower after the heat exchange of neutralizing tower interchanger, and overhead gas enters mixing surge tank, then blasts dehydration tower; Dehydration column overhead gas is through gas-liquid separator separates, and gas enters methanol column, and liquid gets back to return tank through condensation, and at the bottom of tower, a waste liquid part enters sewage works, and a part enters wastewater storage tank; The liquid of gas and return tank enters methanol column, overhead gas enters return tank through condenser condenses, part backflow, a part is again through condensation, phlegma enters finished product methylal storage tank, at the bottom of methanol column tower, liquid is through condensation, and phlegma enters methyl alcohol finished product storage tank, and the gas that tower top is not condensed enters methyl chloride recovery system; The waste water of wastewater storage tank squeezes into the profit reduction and reserving tower that floods, and overhead gas enters mixing surge tank, and waste water at the bottom of tower enters temperature rise heat exchanger heating, recycle.
Specific as follows:
A kind of producing glyphosate by using glycine solvent recovery process, from glyphosate synthesis post comprise methyl chloride, methyl alcohol, methylal, water vapour mixture and mass concentration be 25%-30% liquid caustic soda together with blast neutralizing tower 1 to be neutralized to pH be 7-8, neutralizing tower 1 substrate material squeezes into dehydration tower 4 through neutralizing tower 1 heater heats to 60-80 DEG C of rear portion, a part squeezes into neutralizing tower 1 top, form circulation, neutralizing tower 1 overhead gas enters gas mixture surge tank 2, then blasts dehydration tower 4;
Dehydration tower 4 overhead gas is after condensation, gas-liquid separator separates, gas enters methanol column 10 through methanol column ventilating fan 7, liquid gets back to dehydration tower backflow surge tank 8 through condensation, liquid in dehydration tower backflow surge tank 8 also enters methanol column 10 through dehydration tower reflux pump 9, enters dehydration tower 4 completely form circulation without dehydration;
At the bottom of dehydration tower 4 tower, mixed solution enters waste water surge tank 23; Dehydration tower 4 overhead gas also enters dehydration tower backflow surge tank 8 through condenser condenses, part backflow, and a part delivers to methanol column 10 through dehydration tower reflux pump 9 again after condensation;
At the bottom of methanol column 10 tower, mixed solution is through condensation, and phlegma reclaims and obtains methyl alcohol, and the gas that methanol column 10 tower top is not condensed reclaims and obtains methyl chloride after condensed in two stages, gas-liquid separation; For condensation, gas-liquid separation are delivered to methylal return tank 14 residual night completely, after emptying methyl alcohol, methylal is obtained through reflux rear portion extraction gas, a part delivers to methanol column top, carry out next step circulation, it is 65 ± 5 DEG C that temperature bottom methanol column 10 controls, and the temperature on methanol column 10 top controls to be 35 ± 2 DEG C;
The waste liquid of dehydration tower 4 inner bottom part is delivered to waste water profit reduction and reserving tower 22 through waste water surge tank 23, and after profit reduction and reserving, mixed gas sends into gas mixture storage tank 2, and neutralizing tower well heater 19 delivered to by the mixed solution after profit reduction and reserving;
The waste water that neutralizing tower well heater 19, neutralizing tower 1, gas mixture storage tank 2, dehydration tower 3, methanol column 10 produce enters waste water station and processes.
Claims (10)
1. a producing glyphosate by using glycine solvent reclaimer, is characterized in that,
Glyphosate tail gas carrier pipe is connected with neutralizing tower (1) through carrier pipe with diluted alkaline storage tank (32), neutralizing tower (1) top is connected with gas mixture storage tank (2) through carrier pipe, be connected with dehydration tower (4) middle part through carrier pipe again after the top of gas mixture storage tank (2) is connected with dehydration tower ventilating fan (3), dehydration tower (4) top is connected with dehydration tower condenser (5) through carrier pipe, dehydration tower condenser (5) is connected with dehydration tower gas-liquid separator (6) through carrier pipe, dehydration tower gas-liquid separator (6) is connected with methanol column ventilating fan (7) through carrier pipe, the surge tank (8) that refluxes with dehydration tower again after carrier pipe converges respectively bottom dehydration tower condenser (5) and bottom dehydration tower gas-liquid separator (6) is connected, point two-way after dehydration tower backflow surge tank (8) is connected with dehydration tower reflux pump (9), one tunnel is connected with the middle part of methanol column (10), one tunnel is connected with dehydration tower (4) top, form circulation loop,
In above-mentioned, carrier pipe from dehydration tower reflux pump (9) together enters methanol column (10) middle part with from dehydration tower gas-liquid separator (6) through the carrier pipe of methanol column ventilating fan (7), methanol column (10) top through carrier pipe successively with methylal first-stage condenser (11), methylal secondary condenser (12) connects, two-way is divided through carrier pipe in methylal secondary condenser (12) top, directly be connected with methyl chloride withdrawing can after one tunnel is connected with gas-liquid separator (13), one tunnel is connected through carrier pipe and the methanol column surge tank (14) that refluxes, methanol column backflow surge tank (14) is connected with methanol column reflux pump (15) through carrier pipe, methanol column reflux pump (15) divides two-way through carrier pipe, one tunnel is connected with methanol column (10) top through carrier pipe, form circulation loop, one tunnel is connected with methyl alcohol blowdown condenser (16) through carrier pipe, methyl alcohol blowdown condenser (16) is connected with methylal finished pot (17) top through carrier pipe, methylal finished pot (17) top is connected with methylal finished pot (17) top after carrier pipe is connected with reflux exchanger (18) again, form circulation loop.
2. producing glyphosate by using glycine solvent reclaimer according to claim 1, it is characterized in that, neutralizing tower (1) bottom is also provided with neutralizing tower well heater (19), neutralizing tower (1) bottom is connected with neutralizing tower reflux pump (20) after carrier pipe converges with neutralizing tower well heater (19) bottom, neutralizing tower reflux pump (20) divides two-way through carrier pipe, one tunnel is connected with neutralizing tower (1) top, forms circulation loop, and a road is connected with dehydration tower (4) middle part.
3. producing glyphosate by using glycine solvent reclaimer according to claim 2, it is characterized in that, two-way is divided through carrier pipe in dehydration tower (4) bottom, the carrier pipe at one tunnel and neutralizing tower well heater (19) top, the carrier pipe of neutralizing tower (1) bottom, the carrier pipe of gas mixture storage tank (2) are connected with sewage plant through carrier pipe after converging, one tunnel is connected with waste water discharging pump (21) through carrier pipe, and waste water discharging pump (21) divides two-way through carrier pipe; After the carrier pipe of one tunnel and gas mixture storage tank (2) bottom, the carrier pipe of neutralizing tower well heater (19) bottom converge, be connected with the carrier pipe retaining a percentage of the total profits for the enterprise's own use tower (22) bottom from waste water, one tunnel is connected with waste water surge tank (23), the carrier pipe of waste water surge tank (23) bottom with retain a percentage of the total profits for the enterprise's own use tower fresh feed pump (24) be connected after, then retain a percentage of the total profits for the enterprise's own use tower (22) top with waste water and be connected.
4. producing glyphosate by using glycine solvent reclaimer according to claim 1, is characterized in that, gas mixture storage tank (2) bottom is connected with dehydration tower (4) bottom after carrier pipe is connected with condenser discharging pump (25) again.
5. producing glyphosate by using glycine solvent reclaimer according to claim 3, is characterized in that, waste water profit reduction and reserving tower (22) top is also connected with gas mixture storage tank (2) bottom through carrier pipe; Waste water surge tank (23) top is also provided with the backflow carrier pipe of waste water tank blowdown condenser (26).
6. producing glyphosate by using glycine solvent reclaimer according to claim 3, is characterized in that, dehydration tower backflow surge tank (8) top also arranges the carrier pipe converged to dehydration tower gas-liquid separator (6) carrier pipe with dehydration tower condenser (5).
7. producing glyphosate by using glycine solvent reclaimer according to claim 1, it is characterized in that, methanol column (10) bottom is connected with methyl alcohol finished product condenser (30) after carrier pipe is connected with methyl alcohol discharging pump (27) again, methyl alcohol finished product condenser (30) is connected with methyl alcohol finished pot (29) through carrier pipe, and methyl alcohol finished pot (29) top is also provided with the backflow carrier pipe of methylal blowdown condenser (31).
8. producing glyphosate by using glycine solvent reclaimer according to claim 1, it is characterized in that, methanol column (10) bottom is also connected with methanol column reboiler (28), and methanol column (10) bottom is connected with decontamination station with methanol column reboiler (28) through carrier pipe after carrier pipe converges.
9. a producing glyphosate by using glycine solvent recovery process, is characterized in that,
From glyphosate synthesis post comprise methyl chloride, methyl alcohol, methylal, water vapour mixture and mass concentration be 25%-30% liquid caustic soda together with blast neutralizing tower (1) to be neutralized to pH be 7-8, neutralizing tower (1) substrate material squeezes into dehydration tower (4) through neutralizing tower (1) heater heats to 60-80 DEG C of rear portion, a part squeezes into neutralizing tower (1) top, form circulation, neutralizing tower (1) overhead gas enters gas mixture surge tank (2), then blasts dehydration tower (4);
Dehydration tower (4) overhead gas is after condensation, gas-liquid separator separates, gas enters methanol column (10) through methanol column ventilating fan (7), liquid gets back to dehydration tower backflow surge tank (8) through condensation, liquid in dehydration tower backflow surge tank (8) also enters methanol column (10) through dehydration tower reflux pump (9), enters dehydration tower (4) completely form circulation without dehydration;
At the bottom of dehydration tower (4) tower, mixed solution enters waste water surge tank (23); Dehydration tower (4) overhead gas also enters dehydration tower backflow surge tank (8) through condenser condenses, part backflow, and a part delivers to methanol column (10) through dehydration tower reflux pump (9) again after condensation;
At the bottom of methanol column (10) tower, mixed solution is through condensation, and phlegma reclaims and obtains methyl alcohol, and the gas that methanol column (10) tower top is not condensed reclaims and obtains methyl chloride after condensed in two stages, gas-liquid separation; For condensation, gas-liquid separation are delivered to methylal return tank (14) completely residual night, after emptying methyl alcohol, obtain methylal through reflux rear portion extraction gas, a part delivers to methanol column top, carries out next step circulation;
The waste liquid of dehydration tower (4) inner bottom part is delivered to waste water profit reduction and reserving tower (22) through waste water surge tank (23), and after profit reduction and reserving, mixed gas sends into gas mixture storage tank (2), and neutralizing tower well heater (19) delivered to by the mixed solution after profit reduction and reserving;
The waste water that neutralizing tower well heater (19), neutralizing tower (1), gas mixture storage tank (2), dehydration tower (3), methanol column (10) produce enters waste water station and processes.
10. producing glyphosate by using glycine solvent recovery process according to claim 9, is characterized in that, the temperature of methanol column (10) bottom controls to be 65 ± 5 DEG C, and the temperature on methanol column (10) top controls to be 35 ± 2 DEG C.
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| CN108380029B (en) * | 2018-04-20 | 2023-10-27 | 湖北泰盛化工有限公司 | Alkyl ester method glyphosate solvent recovery system and process |
| CN110922426A (en) * | 2019-11-22 | 2020-03-27 | 湖北泰盛化工有限公司 | Alkyl ester method glyphosate continuous production system and process |
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