Continuous reaction system for glyphosate bulk drug

Abstract

The continuous reaction system of glyphosate raw material medicine is connected with acidolysis and dealcoholization reactor, and the acidolysis and dealcoholization reactor is provided with first reaction function section, second reaction function section, third reaction function section and fourth reaction function section from top to bottom, the first reaction function section is a filler section, the adjacent reaction function sections are separated by partition plates, and the partition plates cannot realize the up and down movement of materials. The upper layer of the liquid surface of the fourth reaction function section is connected with the upper end of the third reaction function section through a gas phase pipeline; the upper layer of the liquid surface of the third reaction function section is connected with the upper end of the second reaction function section through a gas phase pipeline. In each function section, each stage of gas phase flows to the upper section from the lower section by pressure difference, and a certain height of gas-liquid contact is maintained in the upper section to carry out mass transfer and heat transfer, the gas-liquid mass transfer and heat transfer are strengthened through stripping and aeration, and the stripping effect is achieved to quickly remove formaldehyde, methylal, chloromethane and other materials in the materials.

Description

TECHNICAL FIELD

[0001] The application relates to a glyphosate production technology field, in particular to a glyphosate raw material continuous reaction system in a continuous acidolysis dealcoholization process of glyphosate. BACKGROUND

[0002] Glyphosate is a high-efficiency, low-toxicity, broad-spectrum, non-selective herbicide with excellent biological characteristics, and is the largest herbicide variety in the world. At present, there are two routes for the mainstream production process of glyphosate in China: alkyl ester method (glycine method) and imino diacetic acid method (IDA method). The production process abroad is mainly the imino diacetic acid method of the American Monsanto Company. In China, 70% of the glyphosate production capacity is produced by the alkyl ester method which takes glycine and dimethyl phosphite as main raw materials. In the presence of a catalyst triethylamine, the glycine, formaldehyde, and dimethyl phosphite are reacted to obtain a synthesis liquid (glyphosate synthesis liquid). A certain proportion of the synthesis liquid is mixed with acid to obtain a mixed acid liquid (also known as mixed liquid, acidolysis liquid, or hydrolysis liquid in the industry), which is heated to the reaction endpoint temperature using steam, and hydrolysis and acidolysis reactions occur as the temperature rises, generating glyphosate and byproducts methylal and chloromethane. The steam of methylal, methanol, chloromethane, and the like is evaporated from the reactor. After the acidolysis reaction is completed, the remaining liquid phase is a glyphosate slurry, which is crystallized, separated, washed, and dried to obtain glyphosate raw material that meets the national standard.

[0003] The main components of the gas phase tail gas of the acidolysis reaction (i.e., the light components extracted by the fan) are water, methylal, methanol, hydrogen chloride, and chloromethane mixture. The tail gas is sent to a gas phase tail gas recovery device for recovery and treatment. The recovery process is referred to as solvent recovery and chloromethane recovery in the glyphosate industry. The distilled mixed gas is condensed in multiple stages, the condensed liquid (dilute methanol) is sent to the solvent recovery device, and the incondensable gas is sent to the chloromethane recovery device for treatment. Or the high-temperature section tail gas is separately condensed or absorbed to recover dilute hydrochloric acid. Or the distilled mixed gas is first neutralized in a neutralization tower, and the neutralized gas is sent to recover methanol and methylal, and the incondensable gas is sent to the chloromethane recovery device for treatment. Methanol is reused as a solvent in the glyphosate synthesis link, and methylal and chloromethane are sold as byproducts.

[0004] Glyphosate production by the glycine method has a production history of more than 30 years. The processes of solvent recovery, triethylamine recovery, and chloromethane recovery have been realized in industry. Due to the limitations of the characteristics of the glyphosate acidolysis reaction and other factors, the acidolysis dealcoholization process is still an intermittent stirred tank method.

[0005] The intermittent hydrolysis process of glyphosate has the following problems: 1. Low production efficiency, high comprehensive energy consumption and high labor intensity of workers. 2. Small capacity of a single device, many reaction kettles per unit of production capacity, many instrument control points, lack of effective continuity before and after, and unstable product quality caused by human factors in operation, which also restricts the expansion of the production device and the improvement of intrinsic safety. The continuous production of glyphosate can overcome these shortcomings through automatic control. Therefore, the development of a continuous acidolysis and dealcoholization device for glyphosate is one of the main research directions of glyphosate production enterprises.

[0006] Patent CN 111205319 A discloses a continuous synthesis method and system for glycine method glyphosate. The synthesis liquid is acidified to obtain a glyphosate mixed acid liquid for first and second hydrolysis reactions. The slurry after the second hydrolysis reaction is crystallized to obtain glyphosate. The first hydrolysis reaction device includes a first hydrolysis reaction tower and a first hydrolysis reaction kettle. The second hydrolysis reaction device includes a second hydrolysis reaction kettle, and the gas outlet of the second hydrolysis reaction device is connected to a hydrolysis tail gas condenser. The tail gas of the first hydrolysis reaction device and the condensate and tail gas of the first hydrolysis reaction device are treated in a methanol recovery device. The hydrolysis reaction device of this method is divided into multiple stages, the device is complex, the process is long, the acidolysis reaction time is long, and the yield is not high. Moreover, this method still relies on enamel kettles as reactors. SUMMARY

[0007] To solve the above technical problems, the present application provides a continuous reaction system for glyphosate bulk drug, wherein a glyphosate mixed acid liquid storage tank is connected to an acidolysis and dealcoholization reactor, the acidolysis and dealcoholization reactor is provided with 2-10 functional reaction sections from top to bottom, the first reaction functional section is a packing section, when there are more than 3 functional reaction sections, adjacent reaction functional sections are separated by a partition, and the partition cannot realize the upward and downward movement of materials.

[0008] When the functional reaction section is 3, 4, 5, 6, 7, 8, 9, 10, or more, the technical solution of the present application can be realized. As an embodiment of the present application, the functional reaction section is designed to have 4 sections, i.e., a first reaction functional section, a second reaction functional section, a third reaction functional section, and a fourth reaction functional section. The first reaction functional section is a packing section, and adjacent reaction functional sections are separated by a partition, and the partition cannot realize the upward and downward movement of materials.

[0009] The lower part of the second reaction functional section is connected to the middle part of the second reaction functional section through a liquid phase pipeline and a circulating pump.

[0010] The lower part of the third reaction functional section is connected to the middle part of the third reaction functional section through a liquid phase pipeline and a circulating pump, and then connected to a heater I.

[0011] The fourth reaction function section is provided with a slurry discharge port at the bottom, 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, and the other path is connected to the middle part of the fourth reaction function section through a heater II.

[0012] The second reaction function section is connected with the upper 3 / 5-4 / 5 of the third reaction function section through a liquid phase pipeline at 1 / 5-2 / 5 of the upper end.

[0013] The third reaction function section is connected with the upper 3 / 5-4 / 5 of the fourth reaction function section through a liquid phase pipeline at 1 / 5-2 / 5 of the upper end.

[0014] The upper layer of the liquid surface of the fourth reaction function section is connected with the upper end 3 / 5-4 / 5 of the third reaction function section through a gas phase pipeline.

[0015] The upper layer of the liquid surface of the third reaction function section is connected with the upper end 3 / 5-4 / 5 of the second reaction function section through a gas phase pipeline.

[0016] The baffle can also be an overflow plate.

[0017] In the case of an overflow plate or sieve plate, the upper layer of the liquid surface of the fourth reaction function section is connected with the upper end 3 / 5-4 / 5 of the third reaction function section through a gas phase pipeline; the upper layer of the liquid surface of the third reaction function section is connected with the upper end 3 / 5-4 / 5 of the second reaction function section through a gas phase pipeline, and the first reaction function section is connected to a gas recovery device through a gas phase pipeline.

[0018] In the case of a sieve plate, the upper layer of the liquid surface of the fourth reaction function section is connected to a gas recovery device through a gas phase pipeline; the upper layer of the liquid surface of the third reaction function section is connected to a gas recovery device through a gas phase pipeline, and the first reaction function section is connected to a gas recovery device through a gas phase pipeline.

[0019] In the case of an overflow plate, the upper layer of the liquid surface of the fourth reaction function section is connected with the upper end 3 / 5-4 / 5 of the third reaction function section and a gas recovery device through a gas phase pipeline; the upper layer of the liquid surface of the third reaction function section is connected with the upper end 3 / 5-4 / 5 of the second reaction function section and a gas recovery device through a gas phase pipeline;

[0020] The first reaction function section is connected to a gas recovery device through a gas phase pipeline.

[0021] In each functional section, the liquid phase with light components removed flows from top to bottom by gravity to the next section. The material vapor from the second stage reaction functional section of the lower part of the tower is countercurrently contacted with the mixed acid liquid entering from the top in the first stage reaction functional section for mass transfer, heat exchange, reaction and degassing. After preheating and warming up in the first stage reaction functional section, the liquid phase enters the second stage reaction functional section, the temperature of which is maintained by the heat energy brought in by the higher temperature non-condensable gas and saturated vapor from the next stage reaction functional section and balanced with the heat energy consumed by the vaporization of methanol and water in this section, and the volatile methylal and methanol components are vaporized and removed from the reactor with the rising non-condensable gas. The reaction liquid then flows into the third and fourth stage reaction functional sections in turn by overflow and underflow for warming up and reaction. The temperature of the third stage reaction functional section is jointly maintained and controlled by the higher temperature non-condensable gas and saturated vapor brought in from 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 the heater on the external circulation pipeline.

[0022] Alternatively, or part of the liquid phase flows by underflow pipeline to the next section as auxiliary liquid flow, and the flow rate is adjusted by using automatic valves to balance the liquid level and pressure in each reaction functional zone. As a special case, when the underflow pipeline valve opening is 0% or the reactor does not have an underflow passage at this stage, the liquid flow enters the next stage reaction functional section entirely through the overflow pipeline.

[0023] In the case of using sieve plates to divide the functional zones, a small amount of liquid flows through the sieve holes of the tower plates to the next section.

[0024] In each functional section, the gas phase of each stage flows from bottom to top to the upper stage by pressure difference, and maintains a certain height of gas-liquid contact in the upper stage for mass transfer and heat transfer, and strengthens the gas-liquid mass transfer and heat transfer through stripping and aeration, and also plays a stripping role to quickly remove formaldehyde, methylal, chloromethane and other materials in the material.

[0025] The light components (methanol, water, hydrogen chloride and methylal, chloromethane generated in the acidolysis reaction process) in the reaction liquid form a gas phase, which is discharged from the upper gas phase pipe 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. Among them, the upper part of the first reaction functional section is the top of the tower. The gas phase tail gas generated in the second stage reaction functional section is discharged from the top of the tower after mass transfer and heat transfer in the first stage reaction functional section.

[0026] Alternatively, or part of the gas phase directly goes to the gas phase main pipe through the gas phase pipeline as auxiliary gas flow, and the flow rate is adjusted by using automatic valves to balance the pressure in each reaction functional zone. As a special case, when the auxiliary gas flow pipeline valve opening of the reactor at this stage is 0% or the reactor does not have an auxiliary gas flow passage at this stage, the gas flow entirely flows from bottom to top to the upper reaction functional section by pressure difference.

[0027] The "back mixing" problem faced in the continuous process of the batch stirred tank process is solved, and the problem of incomplete reaction (raw material) in the original continuous technology is solved. Therefore, the acid hydrolysis chemical reaction process is complete and stable, and the entire acid hydrolysis reaction is completed in one reactor without the need for a further auxiliary reaction in a porcelain tank; compared with the original batch stirring process, the yield is high, the heat is used in stages, and the steam energy consumption is low. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 For the glyphosate raw material continuous reaction system of Example 1, wherein 1. glyphosate mixed acid liquid storage tank, 2. acid hydrolysis and de-alcoholization 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 circulating pumps, and 12. partition.

[0029] Figure 2 It is a structure diagram of the partition.

[0030] Figure 3 For the glyphosate raw material continuous reaction system of Example 2, wherein 1'. glyphosate mixed acid liquid storage tank, 2'. acid hydrolysis and de-alcoholization 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 circulating pumps, and 12'. partition.

[0031] Figure 4 For the glyphosate raw material continuous reaction system of Example 3, wherein 1". glyphosate mixed acid liquid storage tank, 2". acid hydrolysis and de-alcoholization 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 circulating pumps, and 12". partition.

[0032] Figure 5The glyphosate raw material continuous reaction system of Example 4, wherein the 1''' glyphosate mixed acid liquid storage tank, the 2''' acidolysis de-alcoholization 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''' heater one, the 8''' heater two, the 9''' gas recovery device, the 10''' crystallizer, the 11-1''', 11-2''', 11-3''', 11-4''', 11-5''', 11-6''' are all circulating pumps, and the 12''' partition plate.

[0033] Figure 6 The overflow chart of the partition plate. DETAILED DESCRIPTION

[0034] The glyphosate mixed acid liquid is a mixed acid liquid obtained by acidifying the synthesis liquid in the continuous synthesis process of glyphosate by the glycine method. As disclosed in the references CN1037396A and CN111205319A, the glyphosate mixed acid liquid is obtained. This glyphosate mixed acid liquid is a mixed acid solution which is difficult to handle and is well known to those skilled in the art.

[0035] Example 1

[0036] The glyphosate raw material continuous reaction system, the glyphosate mixed acid liquid storage tank 1 is connected with the acidolysis de-alcoholization reactor 2, the acidolysis de-alcoholization reactor 2 is provided with the first reaction function section 3, the second reaction function section 4, the third reaction function section 5 and the fourth reaction function section 6 from top to bottom, the first reaction function section 3 is a packed section, the adjacent reaction function sections are separated by the partition plate 12, and the partition plate 12 cannot realize the upward and downward movement of the material.

[0037] The lower part of the second reaction function section 4 is connected with the circulating pump through the liquid phase pipeline and then connected to the middle part of the second reaction function section 4.

[0038] The lower part of the third reaction function section 5 is connected with the circulating pump through the liquid phase pipeline and then connected with the heater one 7, and the heater one 7 is connected to the middle part of the third reaction function section 5.

[0039] The fourth reaction function section 6 is provided with a slurry discharge port at the bottom, the slurry discharge port is connected with the circulating pump through the 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 function section 6 through the heater two 8.

[0040] The upper end 1 / 5 of the second reaction function section 4 is connected with the upper 3 / 5 of the third reaction function section 5 through the liquid phase pipeline.

[0041] The upper end 1 / 5 of the third reaction function section 5 is connected with the upper 3 / 5 of the fourth reaction function section 6 through the liquid phase pipeline.

[0042] The upper layer of the fourth reaction function section 6 is connected with the upper end 3 / 5 of the third reaction function section 5 through a gas phase pipeline.

[0043] The upper layer of the third reaction function section 5 is connected with the upper end 3 / 5 of the second reaction function section 4 through a gas phase pipeline.

[0044] The first reaction function section 3 is connected to the gas recovery device 9 through a gas phase pipeline.

[0045] The glyphosate mixed acid solution enters the first reaction function section of the acidolysis and dealcoholization reactor at a flow rate of 4m 3 / h, and the liquid phase enters the second reaction function section through the filler of the first reaction function section. After the reaction liquid in the second reaction section reacts for about half an hour, it enters the third reaction function section through an overflow pipe at a flow rate of 3.0m 3 / h or so. After the reaction liquid in the third reaction section reacts for about 1 hour, it enters the fourth reaction function section through an overflow pipe at a flow rate of 1.6m 3 / h or so. The circulating pump flow rates of the second, third and fourth sections are controlled at 10m 3 / h to realize full circulation of the reaction liquid in the second, third and fourth sections. The steam amount of the heater is controlled to control the temperatures of the third and fourth sections to be 100℃ and 130℃, and the temperatures of the first and second sections are measured to be 46℃ and 72℃. The residence time of the reaction liquid in the acidolysis and dealcoholization reactor is 1-4 hours. The gas phase operating pressure of the first and second reaction function sections of the reactor is controlled in the range of -10kPa. The operating pressure of the third reaction function section of the reactor is 0-50kPa, and the DCS should be set to alarm when the pressure is higher than the limit. The operating pressure of the fourth reaction function section of the reactor is 10-50kPa, and the DCS should be set to alarm when the pressure is higher than the limit, so that the gas phase of the fourth reaction function section enters the third reaction function section, the third reaction function section enters the second reaction function section, and the gas phase of the second reaction function section enters the first reaction function section through a gas phase pipeline and is connected to the gas recovery device. At 35d, the glyphosate slurry flow rate is 1.09m 3 / h, the glyphosate content is 22.61%, and the total yield is 84.94%.

[0046] Example 2

[0047] The glyphosate raw material medicine continuous reaction system is connected with the acidolysis and dealcoholization reactor 2' through the glyphosate mixed acid solution storage tank 1'. The acidolysis and dealcoholization reactor 2' is provided with a first reaction function section 3', a second reaction function section 4', a third reaction function section 5' and a fourth reaction function section 6' from top to bottom. The first reaction function section 3' is a filler section, and the adjacent reaction function sections are separated by a partition plate 12'. The partition plate 12' cannot realize the upward and downward movement of the material.

[0048] The lower part of the second reaction function section 4' is connected to the middle part of the second reaction function section 4' through a liquid phase pipeline and a circulating pump.

[0049] The lower part of the third reaction function section 5' is connected with the circulating pump through the liquid phase pipeline, and then connected with the heater 7'.

[0050] The bottom of the fourth reaction function section 6' is provided with a slurry discharge port, which is connected with the circulating pump through the liquid phase pipeline. The circulating pump is connected to the crystallizer 10' through the liquid phase pipeline in one way, and connected to the middle part of the fourth reaction function section 6' through the heater 2 8' in the other way.

[0051] The upper end 1 / 5 of the second reaction function section 4' is connected with the upper end 4 / 5 of the third reaction function section 5' through the liquid phase pipeline.

[0052] The upper end 1 / 5 of the third reaction function section 5' is connected with the upper end 4 / 5 of the fourth reaction function section 6' through the liquid phase pipeline.

[0053] The upper layer of the liquid surface of the fourth reaction function section 6' is connected to the gas recovery device 9' through the gas phase pipeline; the upper layer of the liquid surface of the third reaction function section 5' is connected to the gas recovery device 9' through the gas phase pipeline.

[0054] The first reaction function section 3' is connected to the gas recovery device 9' through the gas phase pipeline.

[0055] The glyphosate mixed acid solution enters the first reaction function section of the acidolysis de-alcoholization reactor at a flow rate of 4m 3 / h, and the liquid phase enters the second reaction function section through the filler of the first reaction function section. After the reaction liquid in the second reaction section reacts for about half an hour, it enters the third reaction function section through the overflow pipe at a flow rate of 3.2m 3 / h or so; after the reaction liquid in the third reaction section reacts for about 1 hour, it enters the fourth reaction function section through the overflow pipe at a flow rate of 1.7m 3 / h or so; the circulating pump flow rates of the second, third and fourth sections are controlled at 10m 3 / h; the third and fourth section temperatures are controlled at 100℃ and 130℃ by controlling the steam amount of the heater; the first and second section temperatures are measured to be 44℃ and 70℃; the reaction liquid stays in the acidolysis de-alcoholization reactor for 1-4 hours; the gas phase operating pressure of the first and second reaction function sections of the reactor is controlled in the range of -10kPa; the operating pressure of the third reaction function section of the reactor is 0-50kPa, and the DCS should set an over-limit alarm; the operating pressure of the fourth reaction function section of the reactor is 10-50kPa, and the DCS should set an over-limit alarm; the gas phases of the first, third and fourth reaction function sections are connected to the gas recovery device through the gas phase pipeline. At 35d, the glyphosate slurry flow rate is 1.10m 3 / h, the glyphosate content is 22.00%, and the total yield is 83.48%.

[0056] Example 3

[0057] The glyphosate raw material continuous reaction system is provided with an acid liquor tank 1" connected with an acidolysis and dealcoholization reactor 2". The acidolysis and dealcoholization reactor 2 is provided with a first reaction function section 3", a second reaction function section 4", a third reaction function section 5" and a fourth reaction function section 6" from top to bottom. The first reaction function section 3 is a filler section. The adjacent reaction function sections are separated by overflow plates 12". The overflow plates 12" enable the material to move from top to bottom but not from bottom to top.

[0058] The lower part of the second reaction function section 4" is connected with a circulating pump through a liquid phase pipeline and then connected to the middle part of the second reaction function section 4".

[0059] The lower part of the third reaction function section 5" is connected with a circulating pump through a liquid phase pipeline and then connected with a heater 1 7". The heater 1 7" is connected to the middle part of the third reaction function section 5".

[0060] The bottom of the fourth reaction function 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 connected to a crystallizer 10" through a liquid phase pipeline and connected to the middle part of the fourth reaction function section 6" through a heater 2 8".

[0061] The upper end 2 / 5 of the second reaction function section 4" is connected with the upper part 3 / 5 of the third reaction function section 5" through a liquid phase pipeline.

[0062] The upper end 2 / 5 of the third reaction function section 5" is connected with the upper part 3 / 5 of the fourth reaction function section 6" through a liquid phase pipeline.

[0063] The upper layer of the liquid surface of the fourth reaction function section 6" is connected with the upper end 3 / 5 of the third reaction function section 5" through a gas phase pipeline.

[0064] The upper layer of the liquid surface of the third reaction function section 5" is connected with the upper end 3 / 5 of the second reaction function section 4" through a gas phase pipeline.

[0065] The first reaction function section 3" is connected to a gas recovery device 9" through a gas phase pipeline.

[0066] The glyphosate acid liquor enters the first reaction function section of the acidolysis and dealcoholization reactor at a speed of 2.5 m 3 / h. The liquid phase enters the second reaction function section through the filler of the first reaction function section and enters the third and fourth reaction function sections through the overflow plates. After the reaction liquid is reacted in the second reaction section for about 1.5 hours, the liquid surface rises to the downcomer to enter the third reaction function section at a flow rate of about 1.5 m 3 / h. After the reaction liquid is reacted in the third reaction section for about 3 hours, it enters the fourth reaction function section through the downcomer at a flow rate of about 1 m 3 / h. The flow rates of the circulating pumps of the second, third and fourth sections are controlled to be 8 m 3The second, third and fourth reaction liquid is full-circulated; the steam amount of the heater is controlled to control the third and fourth reaction temperature at 100°C and 130°C, and the first and second reaction temperature is measured at 48°C and 73°C; the reaction liquid stays in the acidolysis and dealcoholization reactor for 5-7 hours; the gas phase of the fourth reaction function section enters the third reaction function section, the gas phase of the third reaction function section enters the second reaction function section, and the gas phase of the second reaction function section enters the first reaction function section through the gas phase pipeline and is connected to the gas recovery device. At 35d, the glyphosate slurry flow is 0.81m 3 / h, the glyphosate content is 23.31%, and the total yield is 87.04%.

[0067] Example 4

[0068] The glyphosate raw material medicine continuous reaction system is connected with the acidolysis and dealcoholization reactor 2”’ through the glyphosate mixed acid liquid storage tank 1”’, and the acidolysis and dealcoholization reactor 2”’ is provided with a first reaction function section 3”’, a second reaction function section 4”’, a third reaction function section 5”’, and a fourth reaction function section 6”’ from top to bottom. The first reaction function section 3”’ is a filler section, and the adjacent reaction function sections are separated by overflow plates 12”’, which realize the upward movement of the material and cannot realize the downward movement of the material.

[0069] The lower part of the second reaction function section 4”’ is connected to the middle part of the second reaction function section 4”’ through a liquid phase pipeline and a circulating pump.

[0070] The lower part of the third reaction function section 5”’ is connected to the middle part of the third reaction function section 5”’ through a liquid phase pipeline and a circulating pump and a heater 1 7”’.

[0071] The slurry discharge port of the fourth reaction function section 6”’ is provided at the bottom and is connected to the crystallizer 10”’ through a liquid phase pipeline and a circulating pump, and is connected to the middle part of the fourth reaction function section 6”’ through a heater 2 8”’.

[0072] The upper end 2 / 5 of the second reaction function section 4”’ is connected to the upper 4 / 5 of the third reaction function section 5”’ through a liquid phase pipeline.

[0073] The upper end 2 / 5 of the third reaction function section 5”’ is connected to the upper 4 / 5 of the fourth reaction function section 6”’ through a liquid phase pipeline.

[0074] The gas phase pipeline above the liquid surface of the fourth reaction function section 6”’ is connected to the upper end 4 / 5 of the third reaction function section 5”’ and the gas recovery device 9”’; the gas phase pipeline above the liquid surface of the third reaction function section 5”’ is connected to the upper end 4 / 5 of the second reaction function section 4”’ and the gas recovery device 9”’;

[0075] The first reaction function section 3" is connected to the gas recovery device 9" by a gas pipeline.

[0076] The glyphosate mixed acid solution enters the first reaction function section of the acidolysis de-alcoholization reactor at a speed of 2.5 m 3 / h. The liquid phase enters the second reaction function section through the packing of the first reaction function section, and enters the third and fourth reaction function sections through the overflow plate. After the reaction liquid is reacted in the second reaction section for about 1.5 hours, the liquid level rises to the downcomer to enter the third reaction function section, and the flow rate is about 1.7 m 3 / h. After the reaction liquid is reacted in the third reaction section for about 3 hours, it enters the fourth reaction function section through the downcomer, and the flow rate is about 1.2 m 3 / h. The circulating pump flow rates of the second, third and fourth sections are controlled to be 8 m 3 / h. The temperatures of the third and fourth sections are controlled to be 100°C and 130°C by controlling the steam amount of the heater, and the temperatures of the first and second sections are measured to be 45°C and 70°C. The residence time of the reaction liquid in the acidolysis de-alcoholization reactor is 5-7 hours. The gas phase of the fourth reaction function section enters the third reaction function section, the gas phase of the third reaction function section enters the second reaction function section, the gas phase of the second reaction function section enters the first reaction function section and is connected to the gas recovery device by a gas pipeline, and the gas phases of the third and fourth reaction function sections are connected to the gas recovery device by gas pipelines. At 35d, the glyphosate slurry flow rate is 0.80 m 3 / h, the glyphosate content is 22.75%, and the total yield is 85.42%.

[0077]

[0078]

Claims

1. A continuous reaction system for glyphosate bulk drug substance, characterized in that, The glyphosate mixed acid solution storage tank (1) is connected with the acidolysis de-alcoholization reactor (2), the acidolysis de-alcoholization reactor (2) is provided with four functional reaction sections from top to bottom, namely the first reaction functional section (3), the second reaction functional section (4), the third reaction functional section (5) and the fourth reaction functional section (6), the first reaction functional section (3) is a filler section, the adjacent reaction functional sections are separated by the partition plate (12), the partition plate (12) cannot realize the up and down movement of the material, the upper end 1 / 5-2 / 5 of the second reaction functional section (4) is connected with the upper 3 / 5-4 / 5 of the third reaction functional section (5) through the liquid phase pipeline, the upper end 1 / 5-2 / 5 of the third reaction functional section (5) is connected with the upper 3 / 5-4 / 5 of the fourth reaction functional section (6) through the liquid phase pipeline; The upper layer of the liquid surface of the fourth reaction functional section (6) is connected with the upper end 3 / 5-4 / 5 of the third reaction functional section (5) through the gas phase pipeline, the upper layer of the liquid surface of the third reaction functional section (5) is connected with the upper end 3 / 5-4 / 5 of the second reaction functional section (4) through the gas phase pipeline, and the first reaction functional section (3) is connected to the gas recovery device (9) through the gas phase pipeline.

2. The glyphosate bulk drug substance continuous reaction system of claim 1, wherein, The functional reaction section can also be any one of 5, 6, 7, 8, 9 or 10.

3. The glyphosate bulk drug substance continuous reaction system of claim 2, wherein, The lower part of the second reaction functional section (4) is connected to the middle part of the second reaction functional section (4) through the liquid phase pipeline and the circulating pump.

4. The glyphosate bulk drug substance continuous reaction system of claim 3, wherein, The lower part of the third reaction functional section (5) is connected to the middle part of the third reaction functional section (5) through the liquid phase pipeline and the circulating pump and the heater I (7), and the heater I (7) is connected to the middle part of the third reaction functional section (5).

5. The glyphosate bulk drug substance continuous reaction system of claim 4, wherein, The bottom of the fourth reaction functional section (6) is provided with a slurry discharge port, the slurry discharge port is connected to the circulating pump through the 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).

6. The glyphosate bulk drug substance continuous reaction system of claim 1, wherein, The partition plate is replaced by an overflow plate.

7. The glyphosate bulk drug substance continuous reaction system of claim 1, wherein, The upper layer of the liquid surface of the fourth reaction functional section (6) is connected to the gas recovery device (9) through the gas phase pipeline; the upper layer of the liquid surface of the third reaction functional section (5) is connected to the gas recovery device (9) through the gas phase pipeline, and the first reaction functional section (3) is connected to the gas recovery device (9) through the gas phase pipeline.

8. The glyphosate bulk drug substance continuous reaction system of claim 1, wherein, The upper layer of the liquid surface of the fourth reaction functional section (6) is connected with the upper end 3 / 5-4 / 5 of the third reaction functional section (5) and the gas recovery device (9) through the gas phase pipeline; the upper layer of the liquid surface of the third reaction functional section (5) is connected with the upper end 3 / 5-4 / 5 of the second reaction functional section (4) and the gas recovery device (9) through the gas phase pipeline; The first reaction functional section (3) is connected to the gas recovery device (9) through the gas phase pipeline.

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