CN216630778U - Glyphosate bulk drug serialization reaction system - Google Patents
Glyphosate bulk drug serialization reaction system Download PDFInfo
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- CN216630778U CN216630778U CN202123166114.8U CN202123166114U CN216630778U CN 216630778 U CN216630778 U CN 216630778U CN 202123166114 U CN202123166114 U CN 202123166114U CN 216630778 U CN216630778 U CN 216630778U
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Abstract
The utility model provides a continuous reaction system for glyphosate bulk drugs, wherein a glyphosate mixed acid liquid storage tank is connected with an acidolysis dealcoholization reactor, the acidolysis dealcoholization reactor is provided with a first reaction functional section, a second reaction functional section, a third reaction functional section and a fourth reaction functional section from top to bottom, the first reaction functional section is a filler section, other adjacent reaction functional sections are separated by a partition plate, and the partition plate can not realize the up-and-down movement of materials. The upper liquid level layer 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 liquid level layer 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, gas phases at all stages flow to the upper section from bottom to top by pressure difference, gas-liquid contact at a certain height is kept at the upper section for mass transfer and heat transfer, the gas-liquid mass transfer and heat transfer are enhanced by the action of steam stripping and aeration, and the gas stripping effect is realized, so that materials such as formaldehyde, methylal, methyl chloride and the like in the materials are quickly removed.
Description
Technical Field
The utility model relates to the technical field of glyphosate production, in particular to a continuous reaction system for glyphosate bulk drug in the continuous acidolysis dealcoholization process of glyphosate.
Background
Glyphosate is a high-efficiency, low-toxicity, broad-spectrum, biocidal and non-selective herbicide, has excellent biological characteristics, and is the herbicide variety with the largest global yield. At present, the domestic main stream production process of 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 in America. 70 percent of the capacity of glyphosate in China is produced by adopting an alkyl ester method which takes glycine and dimethyl phosphite as main raw materials, methanol is taken as a reaction solvent, and glycine, paraformaldehyde and dimethyl phosphite react in the presence of a catalyst triethylamine to obtain a synthetic liquid (glyphosate synthetic liquid). Mixing the synthetic solution with acid in a certain proportion to prepare mixed acid solution (also called mixed solution, acidolysis solution and hydrolysis solution in the industry), heating the mixed acid solution to the reaction end temperature by using steam, carrying out hydrolysis and acidolysis reaction along with the temperature rise to generate glyphosate and byproducts such as methylal and chloromethane, and steaming out the methylal, methanol, chloromethane and the like from a reactor. The residual liquid phase after the acidolysis reaction is glyphosate slurry, and glyphosate technical product meeting the national standard is obtained by crystallization, separation, washing and drying.
The main components of the gas phase tail gas (namely the light component extracted by the fan) of the acidolysis reaction are water, methylal, methanol, hydrogen chloride and methyl chloride mixture, the tail gas goes to a gas phase tail gas recovery device for recovery treatment, and the recovery process is referred to as solvent recovery and methyl chloride recovery in the glyphosate industry: the distilled mixed gas is subjected to multi-stage condensation, condensate (dilute methanol) is removed from a solvent recovery device, and noncondensable gas is removed from a chloromethane recovery device for treatment; or independently condensing or absorbing the tail gas of the high-temperature section to recover the dilute hydrochloric acid; or neutralizing the distilled mixed gas in a neutralizing tower, recovering methanol and methylal from the neutralized gas, and treating the non-condensable gas in a chloromethane recovery device. The methanol is used as a solvent to be recycled to the glyphosate synthesis link, and the methylal and the chloromethane are sold as byproducts.
The production of glyphosate by a glycine method has a production history of more than 30 years, the procedures of solvent recovery, triethylamine recovery, chloromethane recovery and the like are industrially realized continuously, and the acidolysis dealcoholization process is still an intermittent stirred tank method due to the limitation of factors such as the characteristics of the acidolysis reaction of glyphosate and the like.
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 capacity of a single set of device is small, the number of reaction kettles with unit capacity is large, the number of instrument control points is large, effective continuity is not available in the front and the back, the problem that the product quality is unstable due to human factors during operation is solved, and the amplification and the improvement of intrinsic safety of a production device are restricted. The continuous production of glyphosate can be controlled automatically, and the defects can be completely overcome. Therefore, the development of a continuous acid hydrolysis and dealcoholization device for glyphosate is one of the main research directions of glyphosate production enterprises.
Patent CN 111205319 a discloses a continuous synthesis method and system for glyphosate by using glycine method, wherein mixed acid obtained by acidifying synthetic liquid is subjected to primary hydrolysis reaction and 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 second-stage hydrolysis reaction device comprises a second-stage hydrolysis reaction kettle, and a gas outlet of the second-stage hydrolysis reaction device is connected with the hydrolysis tail gas condenser. And tail gas of the primary hydrolysis reaction device, condensate of the primary hydrolysis reaction device and tail gas are sent to a methanol recovery device for treatment. 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 not high. And the method still relies on an enamel kettle as a reactor.
Disclosure of Invention
Aiming at the technical problem, the utility model provides a glyphosate bulk drug continuous reaction system, wherein a glyphosate mixed acid liquid storage tank is connected with an acidolysis dealcoholization reactor, the acidolysis dealcoholization reactor is provided with a first reaction functional section, a second reaction functional section, a third reaction functional section and a fourth reaction functional section from top to bottom, the first reaction functional section is a filling section, other adjacent reaction functional sections are separated by a partition plate, and the partition plate can not realize the up-and-down movement of materials.
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 a circulating pump through a liquid phase pipeline and then connected with a heater I, and the heater I is connected to the middle part of the third reaction functional section.
And a slurry discharge port is formed in the bottom of the fourth reaction functional section and 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 of the circulating pump is connected to the crystallizer, and the other path of the circulating pump is connected to the middle of the fourth reaction functional section through a second heater.
The upper end 1/5-2/5 of the second reaction functional section is connected with the upper part 3/5-4/5 of the third reaction functional section through a liquid phase pipeline.
The upper end 1/5-2/5 of the third reaction functional section is connected with the upper part 3/5-4/5 of the fourth reaction functional section through a liquid phase pipeline.
The upper liquid level layer of the fourth reaction functional section is connected with the upper end 3/5-4/5 of the third reaction functional section through a gas phase pipeline.
The upper liquid level layer of the third reaction functional section is connected with the upper end 3/5-4/5 of the second reaction functional section through a gas phase pipeline.
The baffle 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 upper end 3/5-4/5 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 3/5-4/5 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.
Under the condition of the sieve plate, the upper layer of the liquid surface of the fourth reaction functional section is connected to a gas recovery device through a gas phase pipeline; the upper layer of the liquid surface of the third reaction functional section is connected to a 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.
Under the condition 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 part at 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 upper end 3/5-4/5 of the second reaction functional section and a gas recovery device through a gas phase pipeline;
the first reaction functional section is connected to a gas recovery device through a gas phase pipeline.
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 acid mixture 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 the preheating and the primary dealcoholization of the first-stage reaction functional section, the liquid phase enters a second-stage reaction functional section, the temperature of the second-stage reaction functional section is maintained by heat energy brought by the non-condensable gas and saturated steam with higher temperature generated by the next-stage reaction functional section, the heat energy is balanced with the heat energy consumed by the vaporization of methanol and water in the second-stage reaction functional section, and volatile methylal and methanol components are vaporized and leave the reactor along with the rising non-condensable gas. The reaction liquid enters a third stage reaction functional section and a fourth stage reaction functional section for temperature rise reaction sequentially through overflow and underflow. The temperature of the third stage reaction functional section is maintained and controlled by the heat energy brought by the non-condensable gas and the saturated steam with higher temperature generated by the fourth stage reaction functional section and the heater on the 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 part of the liquid phase can be automatically flowed to the next section through the underflow pipeline to be used as an auxiliary liquid flow, and the flow rate is adjusted by using an automatic control valve to balance the liquid level and the pressure of each reaction functional area. As a special example, when the valve opening of the underflow pipe is 0% or the underflow passage is not arranged at the current stage of the reactor, all the liquid flow enters the next stage reaction functional section through the overflow pipe.
In the case of a sieve plate for dividing the functional zone, a small part of the liquid flows automatically to the next stage through the sieve holes of the tower plate.
In each functional section, gas phases at all stages flow to the upper section from bottom to top by pressure difference, gas-liquid contact at a certain height is kept at the upper section for mass transfer and heat transfer, the gas-liquid mass transfer and heat transfer are enhanced by the action of steam stripping and aeration, and the gas stripping effect is realized, so that materials such as formaldehyde, methylal, methyl chloride and the like in the materials are quickly removed.
The light components (methanol, water, hydrogen chloride, methylal and methyl chloride generated in the acidolysis reaction process) in the reaction liquid form gas phase, and 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 gas phase tail gas generated by the second-stage reaction functional section is discharged from the tower top after mass transfer and heat transfer of the first-stage reaction functional section.
Alternatively, or part of the gas phase is directly sent to a gas phase main pipe through a gas phase pipeline to be used as auxiliary gas flow, and the flow rate is adjusted by using an automatic control valve to balance the pressure of each reaction functional area. As a special example, when the valve opening of the auxiliary gas flow pipeline of the reaction section of the stage is 0% or no auxiliary gas flow passage is arranged at the stage of the reactor, the gas flow flows to the reaction functional section from bottom to top by the pressure difference.
Solves the problem of 'back mixing' in the process of continuous batch stirred tank process modification and solves the problems of incomplete reaction (raw material generation) and the like of the original continuous technology. Therefore, the acidolysis hydrolysis chemical reaction process is complete and complete, the continuous operation is stable and reliable, the whole acidolysis reaction is completed in one reactor, and an enamel kettle is not needed for further auxiliary reaction; compared with the original intermittent stirring process, the method has the advantages of high yield, gradient utilization of heat and low steam energy consumption.
Drawings
Fig. 1 is a continuous reaction system for glyphosate bulk drug according to example 1, wherein 1, a glyphosate mixed acid liquid storage tank, 2, an acidolysis dealcoholization reactor, 3, a first reaction functional section, 4, a second reaction functional section, 5, a third reaction functional section, 6, a fourth reaction functional section, 7, a first heater, 8, a second heater, 9, a gas recovery device, 10, a crystallizer, 11-1, 11-2, 11-3, 11-4, 11-5, and 11-6 are circulation pumps, and 12 is a partition plate.
Fig. 2 is a structural view of the separator.
Fig. 3 is a glyphosate bulk drug continuous reaction system of example 2, wherein 1 '. glyphosate mixed acid liquid storage tank, 2 '. acidolysis dealcoholization reactor, 3 '. first reaction functional section, 4 '. second reaction functional section, 5 '. third reaction functional section, 6 '. fourth reaction functional section, 7 '. first heater, 8 '. second heater, 9 '. gas recovery device, 10 '. crystallizer, 11-1 ', 11-2 ', 11-3 ', 11-4 ', 11-5 ', 11-6 ' are all circulation pumps, 12 '. partition plate.
FIG. 4 shows a continuous reaction system for glyphosate bulk drug of example 3, wherein 1 ''. glyphosate mixed acid liquid storage tank, 2 ''. acidolysis dealcoholization reactor, 3 ''. first reaction functional stage, 4 ''. second reaction functional stage, 5 ''. third reaction functional stage, 6 ''. fourth reaction functional stage, 7 ''. first heater, 8 ''. second heater, 9 ''. gas recovery device, 10 ''. crystallizer, 11-1 '', 11-2 '', 11-3 '', 11-4 '', 11-5 '', 11-6 '' are all circulation pumps, 12 ''. partition plate.
FIG. 5 shows a continuous reaction system for glyphosate bulk drug according to example 4, wherein 1 ' ' '. glyphosate mixed acid liquid storage tank, 2 ' ' '. acidolysis dealcoholization reactor, 3 ' ' '. first reaction functional section, 4 ' ' '. second reaction functional section, 5 ' ' '. third reaction functional section, 6 ' ' '. fourth reaction functional section, 7 ' ' '. first heater, 8 ' ' '. second heater, 9 ' ' '. gas recovery device, 10 ' ' '. crystallizer, 11-1 ' ' ', 11-2 ' ' ', 11-3 ' ' ', 11-4 ' ' ', 11-5 ' ' ', 11-6 ' ' ' are each a circulation pump, 12 ' ' '. partition plate.
FIG. 6 is a baffle overflow pattern.
Detailed Description
Example 1
A glyphosate bulk drug continuous reaction system is characterized in that 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 from top to bottom, the first reaction functional section 3 is a filler section, other adjacent reaction functional sections are separated by a partition plate 12, and the partition plate 12 cannot realize the 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 a first heater 7 after being connected with a circulating pump through a liquid phase pipeline, 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 the heater II 8.
The upper end 1/5 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 1/5 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 upper end 3/5 of the third reaction functional section 5 through a gas phase pipeline.
The position of the upper layer of the liquid level of the third reaction functional section 5 is connected with the upper end 3/5 of the second reaction functional section 4 through a gas phase pipeline.
The first reaction functional section 3 is connected to a gas recovery device 9 via a gas phase pipe.
8000kg of glyphosate mixed acid liquid enters a first reaction functional section of an acidolysis dealcoholization reactor according to the speed of 4 m/h, and the liquid phase operation temperature of the first reaction functional section of the reactor is controlled at 40 ℃; the liquid phase enters a second reaction functional section through the filler of the first reaction functional section, the discharged liquid phase of the second reaction functional section is sent into the second reaction functional section according to 3.8 m/h, circulation is realized, and the liquid phase operation temperature of the second reaction functional section is controlled at 70 ℃; after the reaction liquid reacts for about half an hour in the second reaction section, about 20% of the liquid phase enters a third reaction functional section through a liquid phase pipeline, the liquid phase discharged from the third reaction functional section is heated by a heater for one hour according to 3.0m and then is sent into the third reaction functional section, circulation is realized, and the operating temperature of the third reaction functional section of the reactor is controlled at 100 ℃; after the reaction liquid reacts for about 1 hour in the third reaction section, about 30% of liquid phase enters a fourth reaction functional section through a liquid phase pipeline, liquid phase discharging of the fourth reaction functional section is driven into the fourth reaction functional section after being heated by a second heater according to the speed of 1.6 m/h, circulation is realized, and the operating temperature of the fourth reaction functional section of the reactor is controlled at 130 ℃ until the reaction end point; the reaction liquid stays in the acidolysis dealcoholization reactor for 1 to 4 hours; the gas phase operation pressure control range of the first and second 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 is required to set an ultra-high limit alarm; the operating pressure of the fourth reaction functional section of the reactor is 10-50kPa, the DCS is set with an ultra-high limit alarm to realize 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 a gas recovery device through a gas phase pipeline by the first reaction functional section. 3100kg of glyphosate slurry is finally obtained, the glyphosate content is 22.6 percent, and the total yield is 84.9 percent.
Example 2
A glyphosate bulk drug continuous reaction system is characterized in that a glyphosate mixed acid 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', 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 plate 12 ', and the partition plate 12' cannot realize the 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 is 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 a first heater 7' after being connected with a circulating pump through a liquid phase pipeline, and the first heater 7 'is connected to the middle part of the third reaction functional section 5'.
And a slurry discharge port is formed in 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 the crystallizer 10', and the other path is connected to the middle of the fourth reaction functional section 6 'through the heater II 8'.
The upper end 1/5 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 1/5 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.
The upper layer of the liquid level 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 functional section 3 'is connected to a gas recovery device 9' via a gas phase conduit.
8000kg of glyphosate mixed acid liquid enters a first reaction functional section of an acidolysis dealcoholization reactor according to the speed of 4 m/h, and the liquid phase operation temperature of the first reaction functional section of the reactor is controlled at 40 ℃; the liquid phase enters a second reaction functional section through the filler of the first reaction functional section, the discharged liquid phase of the second reaction functional section is sent into the second reaction functional section according to 3.8 m/h, circulation is realized, and the liquid phase operation temperature of the second reaction functional section is controlled at 70 ℃; after the reaction liquid reacts for about half an hour in the second reaction section, about 20% of the liquid phase enters a third reaction functional section through a liquid phase pipeline, the liquid phase discharged from the third reaction functional section is heated by a heater for one hour according to 3.0m and then is sent into the third reaction functional section, circulation is realized, and the operating temperature of the third reaction functional section of the reactor is controlled at 100 ℃; after the reaction liquid reacts for about 1 hour in the third reaction section, about 30% of liquid phase enters the fourth reaction functional section through a liquid phase pipeline, the liquid phase discharged from the fourth reaction functional section is heated by a second heater according to 1.6 m/h and then is sent into the fourth reaction functional section, circulation is realized, and the operating temperature of the fourth reaction functional section of the reactor is controlled at 130 ℃ until the reaction end point; the reaction liquid stays in the acidolysis dealcoholization reactor for 1 to 4 hours; the gas phase operation pressure control range of the first and second 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 needs to set an ultra-high limit alarm; the operating pressure of the fourth reaction functional section of the reactor is 10-50kPa, the DCS is required to set an ultra-high limit alarm, and the gas phases of the first, third and fourth reaction functional sections are connected to a gas recovery device through gas phase pipelines. Finally, 3170kg of glyphosate slurry is obtained, the content of glyphosate is 22.0 percent, and the total yield is 83.5 percent.
Example 3
Glyphosate bulk drug serialization reaction system, glyphosate mixed acid liquid storage tank 1 "is connected with acidolysis dealcoholization reactor 2", and acidolysis dealcoholization reactor 2 top-down is provided with first reaction function section 3 ", second reaction function section 4", third reaction function section 5 ", fourth reaction function section 6", and first reaction function section 3 is the filler section, separates through overflow plate 12 "between other adjacent reaction function sections, overflow plate 12" realizes the material from and reciprocates, can not realize the removal 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 is 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 a circulating pump through a liquid phase pipeline and then connected with a heater I7', and the heater I7 'is connected with 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 the heater two 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 upper end 3/5 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 upper end 3/5 of the second reaction functional section 4' through a gas phase pipeline.
The first reaction functional section 3 'is connected to a gas recovery device 9' through a gas phase pipeline.
8000kg of glyphosate mixed acid liquid enters a first reaction functional section of the acidolysis dealcoholization reactor at the speed of 2.5 m/h, and the liquid phase operation temperature of the first reaction functional section of the reactor is controlled at 40 ℃; liquid phase enters a second reaction functional section through the filler of the first reaction functional section and enters a third reaction functional section and a fourth reaction functional section through an overflow plate, liquid phase discharge of the second reaction functional section is planted into the second reaction functional section according to 2m cultivation/h, liquid phase discharge of the third reaction functional section and the fourth reaction functional section is planted into the third reaction functional section and the fourth reaction functional section according to 1.5m cultivation/h and 1m cultivation/h is planted through a first heater and a second heater and then is planted into the third reaction functional section and the fourth reaction functional section, internal circulation of the reaction functional sections is realized, the operation temperatures of the third reaction functional section and the fourth reaction functional section of the reactor are controlled to be 100 ℃ and 130 ℃ respectively until the reaction end point; the reaction liquid stays for 5 to 7 hours in the acidolysis dealcoholization reactor; the gas phase of the fourth reaction functional section enters a third reaction functional section, the gas phase of the third reaction functional section enters a second reaction functional section, and the gas phase of the second reaction functional section is connected to a gas recovery device through a gas phase pipeline through the first reaction functional section. Finally, 3050kg of glyphosate slurry is obtained, the content of glyphosate is 23.3 percent, and the total yield is 87.0 percent.
Example 4
A continuous reaction system for glyphosate bulk drugs is characterized in that a glyphosate mixed acid 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' '', 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' '' realizes the up-and-down movement of materials and cannot realize the movement 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 is 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 a circulating pump through a liquid phase pipeline and then is connected with a heater I7' '', and the heater I7 '' 'is connected with 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 the heater two 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.
The upper liquid level layer of the fourth reaction functional section 6 ' is connected with the upper end 4/5 of the third reaction functional section 5 ' and the gas recovery device 9 '; the upper liquid level layer of the third reaction functional section 5 ' is connected with the upper end 4/5 of the second reaction functional section 4 ' and the gas recovery device 9 ';
the first reaction functional section 3 '' 'is connected to a gas recovery device 9' '' via a gas phase conduit.
8000kg of glyphosate mixed acid liquid enters a first reaction functional section of the acidolysis dealcoholization reactor at the speed of 2.5 m/h, and the liquid phase operation temperature of the first reaction functional section of the reactor is controlled at 40 ℃; liquid phase enters a second reaction functional section through the filler of the first reaction functional section and enters a third reaction functional section and a fourth reaction functional section through an overflow plate, liquid phase discharge of the second reaction functional section is planted into the second reaction functional section according to 2m cultivation/h, liquid phase discharge of the third reaction functional section and the fourth reaction functional section is planted into the third reaction functional section and the fourth reaction functional section according to 1.5m cultivation/h and 1m cultivation/h is planted through a first heater and a second heater and then is planted into the third reaction functional section and the fourth reaction functional section, internal circulation of the reaction functional sections is realized, the operation temperatures of the third reaction functional section and the fourth reaction functional section of the reactor are controlled to be 100 ℃ and 130 ℃ respectively until the reaction end point; the reaction liquid stays for 5 to 7 hours in the acidolysis dealcoholization reactor; the gas phase of the fourth reaction functional section enters a third reaction functional section, the gas phase of the third reaction functional section enters a second reaction functional section, the gas phase of the second reaction functional section is connected to a gas recovery device through a gas phase pipeline through 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 a gas phase pipeline. 3080kg of glyphosate slurry is finally obtained, the content of glyphosate is 22.8 percent, and the total yield is 85.4 percent.
Claims (10)
1. The glyphosate bulk drug continuous reaction system is characterized in that 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) from top to bottom, 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) can not realize the up-and-down movement of materials.
2. The glyphosate bulk drug continuous reaction system according to claim 1, wherein 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).
3. The glyphosate bulk drug continuous reaction system according to claim 2, wherein the lower part of the third reaction functional section (5) is connected with a first heater (7) after being connected with a circulating pump through a liquid phase pipeline, and the first heater (7) is connected to the middle part of the third reaction functional section (5).
4. The glyphosate bulk drug continuous reaction system according to claim 3, 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 the crystallizer (10), and the other path is connected to the middle part of the fourth reaction functional section (6) through the second heater (8).
5. The glyphosate bulk drug continuous reaction system according to claim 4, wherein the upper end of the second reaction functional section (4) is connected with the upper part of the third reaction functional section (5) through a liquid phase pipeline.
6. The glyphosate raw material medicine serialization reaction system according to claim 5, wherein the upper end of the third reaction functional section (5) is connected with the upper portion of the fourth reaction functional section (6) through a liquid phase pipeline.
7. The glyphosate bulk drug serialization reaction system of claim 6, wherein said baffle is replaced with an overflow plate.
8. The glyphosate bulk drug continuous reaction system according to claim 6 or 7, wherein the upper liquid level layer of the fourth reaction functional section (6) is connected with the upper end of the third reaction functional section (5) through a gas phase pipeline; the upper layer of the liquid surface of the third reaction functional section (5) is connected with 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 glyphosate bulk drug continuous reaction system according to claim 6, wherein 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 layer of the liquid level of the third reaction functional section (5) is connected to a 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 glyphosate bulk drug continuous reaction system according to claim 6 or 7, wherein the upper liquid level layer of the fourth reaction functional section (6) is connected with the upper end of the third reaction functional section (5) and the gas recovery device (9) through a gas phase pipeline; the upper layer of the liquid surface of the third reaction functional section (5) is connected with the upper end of the second reaction functional section (4) and a gas recovery device (9) through a gas phase pipeline;
the first reaction functional section (3) is connected to a gas recovery device (9) through a gas phase pipeline.
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