CN116078339A - Continuous reaction system for glyphosate bulk drug - Google Patents
Continuous reaction system for glyphosate bulk drug Download PDFInfo
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- CN116078339A CN116078339A CN202210896459.9A CN202210896459A CN116078339A CN 116078339 A CN116078339 A CN 116078339A CN 202210896459 A CN202210896459 A CN 202210896459A CN 116078339 A CN116078339 A CN 116078339A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 302
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 65
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 65
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229940079593 drug Drugs 0.000 title claims abstract description 16
- 239000003814 drug Substances 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 239000002253 acid Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000005192 partition Methods 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 9
- 238000003860 storage Methods 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims description 58
- 239000007791 liquid phase Substances 0.000 claims description 44
- 238000011084 recovery Methods 0.000 claims description 44
- 239000002002 slurry Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 4
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 abstract description 22
- 238000012546 transfer Methods 0.000 abstract description 11
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 abstract description 9
- 238000005273 aeration Methods 0.000 abstract description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 96
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 30
- 238000000034 method Methods 0.000 description 21
- 239000000243 solution Substances 0.000 description 20
- 239000012295 chemical reaction liquid Substances 0.000 description 19
- 238000006460 hydrolysis reaction Methods 0.000 description 16
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000004471 Glycine Substances 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 125000005907 alkyl ester group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000002363 herbicidal effect Effects 0.000 description 2
- 239000004009 herbicide Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940088679 drug related substance Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/3804—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)] not used, see subgroups
- C07F9/3808—Acyclic saturated acids which can have further substituents on alkyl
- C07F9/3813—N-Phosphonomethylglycine; Salts or complexes thereof
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The continuous reaction system for the glyphosate bulk drug comprises a glyphosate mixed acid liquid storage tank, an acidolysis dealcoholization reactor, a first reaction functional section, a second reaction functional section, a third reaction functional section and a fourth reaction functional section which are arranged from top to bottom, wherein the first reaction functional section is a filler section, other adjacent reaction functional sections are separated by a partition board, and the partition board cannot realize up-and-down movement of materials. The upper layer of the liquid level of the fourth reaction functional section is connected with the upper end of the third reaction functional section through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section is connected with the upper end of the second reaction functional section through a gas phase pipeline. In each functional section, each level of gas phase flows upwards from bottom to top by pressure difference, and the gas-liquid contact at a certain height is kept in the previous section for mass transfer and heat transfer, the gas-liquid mass transfer and heat transfer are enhanced by steam stripping and aeration, and the gas stripping function is realized, so that the formaldehyde, methylal, chloromethane and other materials in the materials are rapidly removed.
Description
Technical Field
The invention relates to the technical field of glyphosate production, in particular to a continuous reaction system of glyphosate bulk drug in the continuous acidolysis dealcoholization process of glyphosate.
Background
Glyphosate is a highly effective, low-toxic, broad-spectrum, biocidal, nonselective herbicide with excellent biological properties, and is the herbicide variety with the greatest global yield. At present, the main production process of the domestic glyphosate has two routes: alkyl ester process (glycine process) and iminodiacetic acid process (IDA process). The foreign production process is mainly the iminodiacetic acid method of Monsanto company in the United states. The production capacity of 70% of glyphosate in China is produced by adopting an alkyl ester method which takes glycine and dimethyl phosphite as main raw materials, methanol is used as a reaction solvent, and glycine, paraformaldehyde and dimethyl phosphite react in the presence of triethylamine as a catalyst to obtain a synthetic liquid (glyphosate synthetic liquid). Mixing the synthetic solution with acid to obtain mixed acid solution (also known as mixed solution, acidolysis solution and hydrolysis solution in industry), heating to reaction end temperature with steam, hydrolyzing and acidolysis reaction with temperature rise to generate glyphosate and byproducts such as methylal and chloromethane, and steaming out the methylal, methanol, chloromethane and other steam from the reactor. And (3) crystallizing, separating, washing and drying the residual liquid phase after the acidolysis reaction is finished to obtain the glyphosate raw material which accords with the national standard.
The main components of gas phase tail gas (namely light components extracted by a fan) of acidolysis reaction are water, methylal, methanol, hydrogen chloride and chloromethane mixture, the tail gas is sent to a gas phase tail gas recovery device for recovery treatment, and the recovery process is called solvent recovery and chloromethane recovery for short in the glyphosate industry: the distilled mixed gas is treated by a multi-stage condensation, condensate (dilute methanol) solvent removal and recovery device and non-condensable gas chloromethane removal and recovery device; or condensing or absorbing the tail gas of the high temperature section independently to recover dilute hydrochloric acid; or neutralizing the distilled mixed gas by a neutralizing tower, and removing methanol and methylal from the neutralized gas, and treating by a non-condensable gas and chloromethane recovery device. Methanol is used as a solvent to be recycled to the synthesis link of glyphosate, and methylal and chloromethane are used as byproducts to be sold.
The production of glyphosate by a glycine method has been carried out for more than 30 years, and the processes of solvent recovery, triethylamine recovery, chloromethane recovery and the like are industrially continuous, and the acidolysis dealcoholization process is still an intermittent stirred tank method due to the limitation of factors such as the acidolysis reaction characteristics of glyphosate.
The batch hydrolysis process of glyphosate has the following problems: 1. low production efficiency, high comprehensive energy consumption and high labor intensity of workers. 2. The single device has small capability, the number of reaction kettles per unit capacity is large, the number of instrument control points is large, the effective continuity is lacking before and after, the problems of unstable product quality and the like caused by artificial factors exist in operation, and the amplification and the intrinsically safe improvement of the production device are restricted. The continuous production of glyphosate can be controlled automatically, and the defects can be completely overcome. Therefore, the development of the continuous acid dealcoholization device of the glyphosate is one of the main research directions of glyphosate production enterprises.
Patent CN111205319A discloses a continuous synthesis method and system of glyphosate by a glycine method, wherein a glyphosate mixed acid solution obtained by acidifying a synthetic solution is subjected to a primary hydrolysis reaction and a secondary hydrolysis reaction, and slurry obtained after the secondary hydrolysis reaction is crystallized to obtain glyphosate. The primary hydrolysis reaction device comprises a primary hydrolysis reaction tower and a primary hydrolysis reaction kettle; the secondary hydrolysis reaction device comprises a secondary hydrolysis reaction kettle, and a gas outlet of the secondary hydrolysis reaction device is connected with a hydrolysis tail gas condenser. The tail gas of the primary hydrolysis reaction device, condensate of the primary hydrolysis reaction device and the tail gas are treated by a methanol recovery device. The hydrolysis reaction device of the method is divided into multiple stages, the device is complex, the flow is long, the acidolysis reaction time is long, and the yield is low. The process also still relies on an enamel kettle as a reactor.
Disclosure of Invention
Aiming at the technical problems, the invention provides a continuous reaction system for glyphosate bulk drugs, a glyphosate mixed acid liquid storage tank is connected with an acidolysis dealcoholization reactor, the acidolysis dealcoholization reactor is provided with 2-10 sections of functional reaction sections from top to bottom, a first reaction functional section is a filler section, when the functional reaction section is more than 3 sections, adjacent reaction functional sections are separated by a baffle, and the baffle can not realize up-and-down movement of materials.
The technical scheme can be realized when the functional reaction sections are 3, 4, 5, 6, 7, 8, 9, 10 and sections. As an embodiment of this application, this application will the functional reaction section design be 4 sections, first reaction function section, second reaction function section, third reaction function section, fourth reaction function section promptly, first reaction function section is the filler section, separates through the baffle between other adjacent reaction function sections, the baffle can not realize the material reciprocates.
The lower part of the second reaction functional section is connected with the circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction functional section.
The lower part of the third reaction functional section is connected with the circulating pump through a liquid phase pipeline and then connected with a heater, and the heater is connected to the middle part of the third reaction functional section.
The bottom of the fourth reaction functional section is provided with a slurry discharge hole, the slurry discharge hole is connected with a circulating pump through a liquid phase pipeline, the circulating pump is divided into two paths through the liquid phase pipeline, one path is connected to a crystallizer, and the other path is connected to the middle part of the fourth reaction functional section through a heater II.
The 1/5-2/5 part of the upper end of the second reaction functional section is connected with the 3/5-4/5 part of the upper part of the third reaction functional section through a liquid phase pipeline.
The 1/5-2/5 part of the upper end of the third reaction functional section is connected with the 3/5-4/5 part of the upper part of the fourth reaction functional section through a liquid phase pipeline.
The upper layer of the liquid level of the fourth reaction functional section is connected with the 3/5-4/5 position of the upper end of the third reaction functional section through a gas phase pipeline.
The upper layer of the liquid level of the third reaction functional section is connected with the 3/5-4/5 position of the upper end of the second reaction functional section through a gas phase pipeline.
The partition plate can also be an overflow plate.
Under the condition that an overflow plate or a sieve plate is obtained, the upper layer of the liquid level of the fourth reaction functional section is connected with the 3/5-4/5 position of the upper end of the third reaction functional section through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section is connected with the 3/5-4/5 position of the upper end of the second reaction functional section through a gas phase pipeline, and the first reaction functional section is connected to a gas recovery device through a gas phase pipeline.
In the case of a sieve plate, the upper layer of the liquid level of the fourth reaction functional section is connected to a gas recovery device through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section is connected to the gas recovery device through a gas phase pipeline, and the first reaction functional section is connected to the gas recovery device through a gas phase pipeline.
In the case of an overflow plate, the upper layer of the liquid level of the fourth reaction functional section is connected with the 3/5-4/5 position of the upper end of the third reaction functional section and a gas recovery device through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section is connected with the 3/5-4/5 position of the upper end of the second reaction functional section through a gas phase pipeline and a gas recovery device;
the first reaction functional section is connected to a gas recovery device via a gas phase conduit.
In each functional section, the liquid phase from which the light components are removed overflows to the next section from top to bottom by gravity. The material steam from the second-stage reaction functional section at the lower part of the tower and the mixed acid liquid entering from the top of the tower are in countercurrent contact in the first-stage reaction functional section to carry out mass transfer, heat exchange, reaction and degassing. After preheating and preliminary dealcoholization in the first stage reaction functional section, the liquid phase enters the second stage reaction functional section, the temperature of the section is maintained by heat energy brought by non-condensable gas and saturated steam with higher temperature generated in the next stage reaction functional section, the heat energy consumed by vaporization of methanol and water in the section reaches balance, and volatile methylal and methanol components are vaporized and leave the reactor along with rising non-condensable gas. And the reaction liquid sequentially passes through overflow and bottom flow and enters a third-stage and fourth-stage reaction functional section for heating reaction. The temperature of the third-stage reaction functional section is controlled by heat energy brought by non-condensable gas and saturated steam with higher temperature generated by the fourth-stage reaction functional section and a heater on an external circulation pipeline; the temperature of the fourth stage reaction functional section is maintained and controlled by a heater on the external circulation pipeline.
Alternatively, or in addition, a portion of the liquid phase is automatically flowed to the next stage through an underflow pipe, and as an auxiliary liquid stream, a self-control valve is used to adjust the flow rate to balance the liquid level and pressure in each reaction function area. As a special case, when the valve opening of the underflow pipe is 0% or when the underflow passage is not provided in the present stage of the reactor, the liquid flow entirely enters the next stage reaction functional section through the overflow pipe.
In the case of dividing the functional zone using sieve plates, a small portion of the liquid flows automatically through the sieve openings of the plates to the next stage.
In each functional section, each level of gas phase flows upwards from bottom to top by pressure difference, and the gas-liquid contact at a certain height is kept in the previous section for mass transfer and heat transfer, the gas-liquid mass transfer and heat transfer are enhanced by steam stripping and aeration, and the gas stripping function is realized, so that the formaldehyde, methylal, chloromethane and other materials in the materials are rapidly removed.
The light components (methanol, water, hydrogen chloride and methylal and chloromethane generated in the acidolysis reaction process) in the reaction solution form gas phases which are respectively discharged from gas phase pipes at the upper parts of the first-stage reaction functional section, the second-stage reaction functional section, the third-stage reaction functional section and the fourth-stage reaction functional section. Wherein the upper part of the first reaction functional section is the top of the tower. And the gas phase tail gas generated by the second-stage reaction functional section is discharged from the top of the tower after mass transfer and heat transfer of the first-stage reaction functional section.
Alternatively, or in addition, part of the gas phase is directly sent to a gas phase main pipe through a gas phase pipeline, and as auxiliary gas flow, a self-control valve is used for adjusting the flow so as to balance the pressure of each reaction functional area. As a specific example, when the opening of the auxiliary gas flow pipeline valve of the reaction section of the present stage is 0% or the auxiliary gas flow passage is not arranged in the present stage of the reactor, the gas flows from bottom to top to the previous reaction functional section by the pressure difference.
Solves the problem of back mixing in the continuous intermittent stirring kettle process reformation process, solves the problems of incomplete reaction (raw material occurrence) and the like of the original continuous technology. Therefore, the acidolysis hydrolysis chemical reaction process is complete and thorough, the continuous operation is stable and reliable, and all acidolysis reactions are completed in one reactor without further auxiliary reaction of an enamel kettle; compared with the original intermittent stirring process, the method has the advantages of high yield, gradient heat utilization and low steam energy consumption.
Drawings
FIG. 1 is a schematic illustration of a glyphosate drug substance continuity reaction system of example 1, wherein 1 a glyphosate acid-mixing liquid storage tank, 2 an acid-stripping reactor, 3 a first reaction functional section, 4 a second reaction functional section, 5 a third reaction functional section, 6a fourth reaction functional section, 7 a first heater, 8 a second heater, 9a gas recovery device, 10 a crystallizer, 11-1, 11-2, 11-3, 11-4, 11-5, 11-6 are circulation pumps, 12 a separator.
Fig. 2 is a structural view of the separator.
FIG. 3 is a schematic illustration of a continuous reaction system for glyphosate crude drug in example 2, wherein the 1'. Glyphosate acid mixture tank, the 2'. Acid dealcoholization reactor, the 3'. First reaction function section, the 4'. Second reaction function section, the 5'. Third reaction function section, the 6'. Fourth reaction function section, the 7'. First heater, the 8'. Second heater, the 9'. Gas recovery device, the 10'. Crystallizer, the 11-1', 11-2', 11-3', 11-4', 11-5', 11-6' are circulation pumps, and the 12'. Separator.
FIG. 4 is a schematic illustration of a continuous reaction system for glyphosate crude drug in example 3, wherein 1". Glyphosate mixed acid liquid storage tank, 2". Acid dealcoholization reactor, 3". First reaction function section, 4". Second reaction function section, 5". Third reaction function section, 6". Fourth reaction function section, 7". Heater one, 8". Heater two, 9". Gas recovery device, 10". Crystallizer, 11-1", 11-2", 11-3", 11-4", 11-5", 11-6" are circulation pump, 12". Separator.
FIG. 5 is a continuous reaction system for glyphosate crude drug of example 4, wherein, 1'. 6', a fourth reaction function section, 7', a heater I, 8', a heater II, 9', a gas recovery device, 10', a crystallizer, 8', a heater II, 9', a gas recovery device, 10', a crystallizer.
Fig. 6 is a flow diagram of a separator plate.
Detailed Description
In the continuous synthesis process of the glyphosate mixed acid solution by a glycine method, the mixed acid solution obtained by acidifying the synthetic solution, such as reference CN1037396A, CN111205319A and the like, is obtained, and the glyphosate mixed acid solution is a mixed acid solution which is difficult to treat and is well known to a person skilled in the art.
Example 1
The continuous reaction system of the glyphosate bulk drug comprises a glyphosate mixed acid liquid storage tank 1, an acidolysis dealcoholization reactor 2, wherein the acidolysis dealcoholization reactor 2 is provided with a first reaction functional section 3, a second reaction functional section 4, a third reaction functional section 5 and a fourth reaction functional section 6 from top to bottom, the first reaction functional section 3 is a filler section, other adjacent reaction functional sections are separated by a partition 12, and the partition 12 cannot realize up-and-down movement of materials.
The lower part of the second reaction functional section 4 is connected with a circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction functional section 4.
The lower part of the third reaction functional section 5 is connected with the circulating pump through a liquid phase pipeline and then connected with a first heater 7, and the first heater 7 is connected to the middle part of the third reaction functional section 5.
The bottom of the fourth reaction functional section 6 is provided with a slurry discharge hole, the slurry discharge hole is connected with a circulating pump through a liquid phase pipeline, the circulating pump is divided into two paths through the liquid phase pipeline, one path is connected to a crystallizer 10, and the other path is connected to the middle part of the fourth reaction functional section 6 through a heater II 8.
The 1/5 part of the upper end of the second reaction functional section 4 is connected with the 3/5 part of the upper part of the third reaction functional section 5 through a liquid phase pipeline.
The 1/5 part of the upper end of the third reaction functional section 5 is connected with the 3/5 part of the upper part of the fourth reaction functional section 6 through a liquid phase pipeline.
The upper layer of the liquid level of the fourth reaction functional section 6 is connected with the 3/5 position of the upper end of the third reaction functional section 5 through a gas phase pipeline.
The upper layer of the liquid level of the third reaction functional section 5 is connected with the 3/5 position of the upper end of the second reaction functional section 4 through a gas phase pipeline.
The first reaction function section 3 is connected to a gas recovery device 9 via a gas phase conduit.
Glyphosate mixed acid solution according to the proportion of 4m 3 H into the acid dealcoholization reactorAfter one reaction functional section, the liquid phase enters the second reaction functional section through the filler of the first reaction functional section, and after the reaction liquid reacts in the second reaction section for about half an hour, the reaction liquid enters the third reaction functional section through an overflow pipe, wherein the flow is 3.0m 3 About/h; after the reaction liquid reacts in the third reaction section for about 1 hour, the reaction liquid enters the fourth reaction functional section through an overflow pipe, and the flow is 1.6m 3 About/h; controlling the flow of the second, third and fourth sections of circulating pumps to be 10m 3 And (h) carrying out full circulation of the second, third and fourth sections of reaction liquid; controlling the temperature of the third section and the fourth section to be 100 ℃ and 130 ℃ by controlling the steam quantity of the heater, and measuring the temperature of the first section and the second section to be 46 ℃ and 72 ℃; the reaction solution stays in the acidolysis dealcoholization reactor for 1-4 hours; the gas phase operation pressure control range of the first and second stage reaction functional sections of the reactor is-10 kPa; the operating pressure of the third reaction functional section of the reactor is 0-50kPa, and the DCS should be provided with ultra-high limit alarm; the operating pressure of the fourth reaction functional section of the reactor is 10-50kPa, and the DCS is required to set ultra-high limit alarm, so that the gas phase of the fourth reaction functional section enters the third reaction functional section, the third reaction functional section enters the second reaction functional section, and the gas phase of the second reaction functional section is connected to the gas recovery device through the gas phase pipeline by the first reaction functional section. At 35d, the flow rate of the extracted glyphosate slurry is 1.09m 3 And/h, the glyphosate content is 22.61 percent, and the total yield is 84.94 percent.
Example 2
The continuous reaction system of the glyphosate bulk drug comprises a glyphosate mixed acid liquid storage tank 1 'and an acidolysis dealcoholization reactor 2', wherein the acidolysis dealcoholization reactor 2 'is provided with a first reaction functional section 3', a second reaction functional section 4', a third reaction functional section 5', a fourth reaction functional section 6 'from top to bottom, the first reaction functional section 3' is a filler section, other adjacent reaction functional sections are separated by a partition 12', and the partition 12' can not realize up-and-down movement of materials.
The lower part of the second reaction functional section 4 'is connected with a circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction functional section 4'.
The lower part of the third reaction functional section 5 'is connected with the circulating pump through a liquid phase pipeline and then connected with a first heater 7', and the first heater 7 'is connected to the middle part of the third reaction functional section 5'.
The bottom of the fourth reaction functional section 6 'is provided with a slurry discharge port, the slurry discharge port is connected with a circulating pump through a liquid phase pipeline, the circulating pump is divided into two paths through the liquid phase pipeline, one path is connected to the crystallizer 10', and the other path is connected to the middle part of the fourth reaction functional section 6 'through a heater II 8'.
The 1/5 part of the upper end of the second reaction functional section 4 'is connected with the 4/5 part of the upper part of the third reaction functional section 5' through a liquid phase pipeline.
The 1/5 part of the upper end of the third reaction functional section 5 'is connected with the 4/5 part of the upper part of the fourth reaction functional section 6' through a liquid phase pipeline.
The upper liquid level layer of the fourth reaction functional section 6 'is connected to a gas recovery device 9' through a gas phase pipeline; the upper liquid level layer of the third reaction functional section 5 'is connected to a gas recovery device 9' through a gas phase pipeline.
The first reaction function 3 'is connected to a gas recovery device 9' via a gas phase conduit.
Glyphosate mixed acid solution according to the proportion of 4m 3 After entering the first reaction functional section of the acid dealcoholization reactor, the liquid phase enters the second reaction functional section through the filler of the first reaction functional section, and after the reaction liquid reacts in the second reaction section for about half an hour, the reaction liquid enters the third reaction functional section through an overflow pipe, wherein the flow is 3.2m 3 About/h; after the reaction liquid reacts in the third reaction section for about 1 hour, the reaction liquid enters the fourth reaction functional section through an overflow pipe, and the flow is 1.7m 3 About/h; controlling the flow of the second, third and fourth sections of circulating pumps to be 10m 3 And (h) carrying out full circulation of the second, third and fourth sections of reaction liquid; controlling the temperature of the third section and the fourth section to be 100 ℃ and 130 ℃ by controlling the steam quantity of the heater, and measuring the temperature of the first section and the second section to be 44 ℃ and 70 ℃; the reaction solution stays in the acidolysis dealcoholization reactor for 1-4 hours; the gas phase operation pressure control range of the first and second stage reaction functional sections of the reactor is-10 kPa; the operating pressure of the third reaction functional section of the reactor is 0-50kPa, and the DCS should be provided with ultra-high limit alarm; the operating pressure of the fourth reaction functional section of the reactor is 10-50kPa, the DCS is provided with an ultra-high limit alarm, and the gas phases of the first reaction functional section, the third reaction functional section and the fourth reaction functional section are connected to a gas recovery device through gas phase pipelines. At 35d, the flow rate of the extracted glyphosate slurry is1.10m 3 And/h, the glyphosate content is 22.00%, and the total yield is 83.48%.
Example 3
A continuous reaction system of glyphosate raw material medicines, a glyphosate mixed acid liquid storage tank 1' is connected with an acidolysis dealcoholization reactor 2', the acidolysis dealcoholization reactor 2 is provided with a first reaction functional section 3', a second reaction functional section 4', a third reaction functional section 5', and a fourth reaction functional section 6', the first reaction functional section 3 is a filling section, other adjacent reaction functional sections are separated by an overflow plate 12', and the overflow plate 12 "can realize the self-up and down movement of materials and can not realize the bottom-up movement.
The lower part of the second reaction functional section 4 'is connected with the circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction functional section 4'.
The lower part of the third reaction functional section 5 'is connected with the circulating pump through a liquid phase pipeline and then connected with a first heater 7', and the first heater 7 'is connected to the middle part of the third reaction functional section 5'.
The bottom of the fourth reaction functional section 6 'is provided with a slurry discharge port, the slurry discharge port is connected with a circulating pump through a liquid phase pipeline, the circulating pump is divided into two paths through the liquid phase pipeline, one path is connected to the crystallizer 10', and the other path is connected to the middle part of the fourth reaction functional section 6 'through a heater II 8'.
The upper end 2/5 of the second reaction functional section 4 'is connected with the upper part 3/5 of the third reaction functional section 5' through a liquid phase pipeline.
The upper end 2/5 of the third reaction functional section 5 'is connected with the upper part 3/5 of the fourth reaction functional section 6' through a liquid phase pipeline.
The upper layer of the liquid level of the fourth reaction functional section 6 'is connected with the 3/5 position of the upper end of the third reaction functional section 5' through a gas phase pipeline.
The upper layer of the liquid level of the third reaction functional section 5 'is connected with the 3/5 position of the upper end of the second reaction functional section 4' through a gas phase pipeline.
The first reaction function section 3 "is connected to the gas recovery device 9" via a gas phase conduit.
Glyphosate mixed acid solution according to 2.5m 3 After the/h speed enters the first reaction functional section of the acid dealcoholization reactor, the liquid phase passes through the first reaction functional sectionThe filling material enters the second reaction functional section and enters the third and fourth reaction functional sections through the overflow plate, after the reaction liquid reacts in the second reaction section for about 1.5 hours, the liquid level rises to the downcomer and enters the third reaction functional section, and the flow is 1.5m 3 About/h; after the reaction liquid reacts in the third reaction section for about 3 hours, the reaction liquid enters the fourth reaction functional section through a downcomer with the flow rate of 1m 3 About/h; controlling the flow of the second, third and fourth sections of circulating pumps to be 8m 3 And (h) carrying out full circulation of the second, third and fourth sections of reaction liquid; controlling the temperature of the third section and the fourth section to be 100 ℃ and 130 ℃ by controlling the steam quantity of the heater, and measuring the temperature of the first section and the second section to be 48 ℃ and 73 ℃; the reaction solution stays in the acidolysis dealcoholization reactor for 5-7 hours; the gas phase of the fourth reaction functional section enters the third reaction functional section, the gas phase of the third reaction functional section enters the second reaction functional section, and the gas phase of the second reaction functional section is connected to the gas recovery device through the gas phase pipeline by the first reaction functional section. At 35d, the flow rate of the extracted glyphosate slurry is 0.81m 3 And/h, the glyphosate content is 23.31 percent, and the total yield is 87.04 percent.
Example 4
A continuous reaction system of glyphosate raw material medicines, a glyphosate mixed acid liquid storage tank 1' is connected with an acidolysis dealcoholization reactor 2', the acidolysis dealcoholization reactor 2' is provided with a first reaction functional section 3', a second reaction functional section 3', a third reaction functional section and a fourth reaction functional section from top to bottom a second reaction functional section 4', a third reaction functional section 5', a fourth reaction functional section 6', the first reaction functional section 3' is a filling section, other adjacent reaction functional sections are separated by an overflow plate 12', the overflow plate 12' "can move up and down from the material, and cannot move from bottom to top.
The lower part of the second reaction functional section 4 'is connected with a circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction functional section 4'.
The lower part of the third reaction functional section 5 'is connected with the circulating pump through a liquid phase pipeline and then connected with the heater 7', the heater one 7 '"is connected to the middle of the third reactive functional section 5'".
The bottom of the fourth reaction functional section 6 'is provided with a slurry discharge port which is connected with a circulating pump through a liquid phase pipeline, the circulating pump is divided into two paths through a liquid phase pipeline, one path is connected to the crystallizer 10', one path is connected to the middle part of the fourth reaction functional section 6 'through the second heater 8'.
The upper end 2/5 of the second reaction functional section 4 'is connected with the upper part 4/5 of the third reaction functional section 5' through a liquid phase pipeline.
The upper end 2/5 of the third reaction functional section 5 'is connected with the upper part 4/5 of the fourth reaction functional section 6' through a liquid phase pipeline.
Fourth reaction functional section 6' liquid surface upper layer gas phase pipeline and third reaction the upper end 4/5 of the functional section 5' is connected with the gas recovery device 9'; the upper layer of the liquid surface of the third reaction functional section 5' is connected with the second reaction functional section through a gas phase pipeline the upper end 4/5 of the reaction functional section 4' is connected with a gas recovery device 9';
the first reaction function section 3 '"is connected via a gas phase conduit to a gas recovery means 9'".
Glyphosate mixed acid solution according to 2.5m 3 After the/h speed enters the first reaction functional section of the acid dealcoholization reactor, the liquid phase enters the second reaction functional section through the filler of the first reaction functional section, enters the third and fourth reaction functional sections through the overflow plate, and after the reaction liquid reacts in the second reaction section for about 1.5 hours, the liquid level rises to the downcomer to enter the third reaction functional section, and the flow is 1.7m 3 About/h; after the reaction liquid reacts in the third reaction section for about 3 hours, the reaction liquid enters the fourth reaction functional section through a downcomer with the flow of 1.2m 3 About/h; controlling the flow of the second, third and fourth sections of circulating pumps to be 8m 3 And (h) carrying out full circulation of the second, third and fourth sections of reaction liquid; controlling the temperature of the third section and the fourth section to be 100 ℃ and 130 ℃ by controlling the steam quantity of the heater, and measuring the temperature of the first section and the second section to be 45 ℃ and 70 ℃; the reaction solution stays in the acidolysis dealcoholization reactor for 5-7 hours; the gas phase of the fourth reaction functional section enters the third reaction functional section, the gas phase of the third reaction functional section enters the second reaction functional section, the gas phase of the second reaction functional section is connected to the gas recovery device through the gas phase pipeline by the first reaction functional section, and the gas phases of the third reaction functional section and the fourth reaction functional section are connected to the gas recovery device through the gas phase pipeline. At 35d, the flow rate of the extracted glyphosate slurry is 0.80m 3 H, glyphosateThe content was 22.75% and the total yield was 85.42%.
Claims (10)
1. The continuous reaction system for the glyphosate bulk drug is characterized in that a glyphosate mixed acid liquid storage tank (1) is connected with an acidolysis dealcoholization reactor (2), 2-10 functional reaction sections are arranged on the acidolysis dealcoholization reactor (2) from top to bottom, a first reaction functional section (3) is a filler section, when the functional reaction section is more than 3 sections, adjacent reaction functional sections are separated by a partition plate (12), and the partition plate (12) cannot realize up-and-down movement of materials.
2. The continuous reaction system of glyphosate bulk drug according to claim 1, wherein the functional reaction sections are 4 sections, namely a first reaction functional section (3), a second reaction functional section (4), a third reaction functional section (5) and a fourth reaction functional section (6), the first reaction functional section (3) is a filling section, other adjacent reaction functional sections are separated by a partition plate (12), and the partition plate (12) cannot realize up-and-down movement of materials.
3. The continuous reaction system of glyphosate raw materials as claimed in claim 2, wherein the lower part of the second reaction functional section (4) is connected with the circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction functional section (4).
4. The continuous reaction system for glyphosate raw materials according to claim 3, wherein the lower part of the third reaction functional section (5) is connected with the circulating pump through a liquid phase pipeline and then connected with a first heater (7), and the first heater (7) is connected to the middle part of the third reaction functional section (5).
5. The continuous reaction system for glyphosate raw materials according to claim 4, wherein a slurry discharge port is arranged at the bottom of the fourth reaction functional section (6), the slurry discharge port is connected with a circulating pump through a liquid phase pipeline, the circulating pump is divided into two paths through the liquid phase pipeline, one path is connected to a crystallizer (10), and the other path is connected to the middle part of the fourth reaction functional section (6) through a heater II (8).
6. The continuous reaction system of glyphosate raw materials according to claim 5, wherein the 1/5-2/5 part of the upper end of the second reaction functional section (4) is connected with the 3/5-4/5 part of the upper part of the third reaction functional section (5) through a liquid phase pipeline, and the 1/5-2/5 part of the upper end of the third reaction functional section (5) is connected with the 3/5-4/5 part of the upper part of the fourth reaction functional section (6) through a liquid phase pipeline.
7. The continuous reaction system of glyphosate raw material according to claim 6, wherein said partition plate is replaced by an overflow plate.
8. The continuous reaction system of glyphosate bulk drug according to claim 6 or 7, characterized in that the upper layer of the liquid level of the fourth reaction functional section (6) is connected with the 3/5-4/5 position of the upper end of the third reaction functional section (5) through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section (5) is connected with the 3/5-4/5 part of the upper end of the second reaction functional section (4) through a gas phase pipeline, and the first reaction functional section (3) is connected to a gas recovery device (9) through a gas phase pipeline.
9. The continuous reaction system of glyphosate raw materials according to claim 6, wherein the upper layer of the liquid surface of the fourth reaction functional section (6) is connected to a gas recovery device (9) through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section (5) is connected to the gas recovery device (9) through a gas phase pipeline, and the first reaction functional section (3) is connected to the gas recovery device (9) through a gas phase pipeline.
10. The continuous reaction system of glyphosate bulk drug according to claim 6 or 7, characterized in that the upper layer of the liquid level of the fourth reaction functional section (6) is connected with the 3/5-4/5 position of the upper end of the third reaction functional section (5) and a gas recovery device (9) through a gas phase pipeline; the upper layer of the liquid level of the third reaction functional section (5) is connected with the 3/5-4/5 position of the upper end of the second reaction functional section (4) through a gas phase pipeline and a gas recovery device (9);
the first reaction functional section (3) is connected to a gas recovery device (9) via a gas phase conduit.
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