CN116078339A - Continuous reaction system for glyphosate API - Google Patents

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

Glyphosate API continuous reaction system

Technical Field

The invention relates to the technical field of glyphosate production, in particular to a continuous reaction system for a glyphosate raw material drug in a continuous acidolysis and de-alcoholization process of glyphosate.

Background Art

Glyphosate is a highly efficient, low-toxic, broad-spectrum, lethal, non-selective herbicide with excellent biological properties. It is the largest herbicide variety in the world. At present, there are two mainstream production processes for glyphosate in China: the alkyl ester method (glycine method) and the iminodiacetic acid method (IDA method). The production process abroad is mainly the iminodiacetic acid method of Monsanto Company in the United States. 70% of my country's glyphosate production capacity is produced by the alkyl ester method with glycine and dimethyl phosphite as the main raw materials. This method uses methanol as the reaction solvent. In the presence of the catalyst triethylamine, glycine, polyformaldehyde, and dimethyl phosphite react to obtain a synthetic liquid (glyphosate synthetic liquid). A certain proportion of the synthetic liquid is mixed with acid to obtain a mixed acid liquid (also known as a mixed liquid, acidolysis liquid, and hydrolysis liquid in the industry). Steam is used to heat the mixture to the reaction end temperature. As the temperature rises, hydrolysis and acidolysis reactions occur to generate glyphosate and by-products methylal and chloromethane. Methylal, methanol, chloromethane and other vapors are evaporated from the reactor. The remaining liquid phase after the acid hydrolysis reaction is glyphosate slurry, which is crystallized, separated, washed and dried to obtain glyphosate technical that meets national standards.

The gaseous tail gas of the acidolysis reaction (i.e., the light component extracted by the fan) is mainly composed of water, methylal, methanol, hydrogen chloride and methyl chloride mixture. The tail gas is sent to the gaseous tail gas recovery device for recovery and treatment. The recovery process is referred to as solvent recovery and methyl chloride recovery in the glyphosate industry: the distilled mixed gas is condensed in multiple stages, the condensate (diluted methanol) is sent to the solvent recovery device, and the non-condensable gas is treated by the methyl chloride recovery device; or the high-temperature tail gas is 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 used to recover methanol and methylal, and the non-condensable gas is treated by the methyl chloride recovery device. Methanol is reused as a solvent in the glyphosate synthesis process, and methylal and methyl chloride are sold as by-products.

The production of glyphosate by the glycine method has a history of more than 30 years. The processes of solvent recovery, triethylamine recovery, and methyl chloride recovery have been realized continuously in the industry. Due to the limitations of factors such as the characteristics of the glyphosate acidolysis reaction, the acidolysis alcoholization process is still an intermittent stirred tank method.

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. The capacity of a single set of equipment is small, the number of reactors per unit production capacity is large, and there are many instrument control points. There is a lack of effective continuity before and after, and there are problems such as unstable product quality caused by human factors in operation, which also restricts the expansion of production equipment and the improvement of intrinsic safety. Continuous production of glyphosate can completely overcome these shortcomings through automated control. Therefore, the development of a continuous acid-dehydrolysis 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 of glyphosate by glycine method, wherein the glyphosate mixed acid liquid obtained by acidification of the synthetic liquid is subjected to primary hydrolysis reaction and secondary hydrolysis reaction, and the slurry 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 the gas outlet of the secondary hydrolysis reaction device is connected to a hydrolysis tail gas condenser. The tail gas of the primary hydrolysis reaction device and the condensate and tail gas of the primary hydrolysis reaction device 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 process is long, the acidolysis reaction time is long, and the yield is not high. Moreover, the method still relies on an enamel kettle as a reactor.

Summary of the invention

In view of the above technical problems, the present invention provides a continuous reaction system for glyphosate raw materials, wherein a glyphosate mixed acid liquid storage tank is connected to an acid dealcoholization reactor, and the acid dealcoholization reactor is provided with 2-10 functional reaction sections from top to bottom, the first reaction functional section is a packing section, and when the functional reaction sections are more than 3 sections, adjacent reaction functional sections are separated by partitions, and the partitions cannot realize the up and down movement of materials.

When the functional reaction section is 3, 4, 5, 6, 7, 8, 9, 10, the technical solution of this case can be realized. As an embodiment of the present application, the functional reaction section is designed as 4 sections, namely the first reaction functional section, the second reaction functional section, the third reaction functional section, and the fourth reaction functional section. The first reaction functional section is a packing section, and other adjacent reaction functional sections are separated by partitions, and the partitions cannot realize the up and down movement of materials.

The lower part of the second reaction functional section is connected to the circulation 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 to the circulation pump through a liquid phase pipeline and then connected to the heater 1, and the heater 1 is connected to the middle part of the third reaction functional section.

A slurry discharge port is provided at the bottom of the fourth reaction functional section, and the slurry discharge port is connected to a circulation pump via a liquid phase pipeline. The circulation 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 of the fourth reaction functional section via heater 2.

The upper end 1/5-2/5 of the second reaction functional section is connected to the upper part 3/5-4/5 of the third reaction functional section via a liquid phase pipeline.

The upper end 1/5-2/5 of the third reaction functional section is connected to the upper part 3/5-4/5 of the fourth reaction functional section through a liquid phase pipeline.

The upper layer of the liquid surface of the fourth reaction functional section is connected to 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 surface of the third reaction functional section is connected to the upper end 3/5-4/5 of the second reaction functional section through a gas phase pipeline.

The partition plate may also be an overflow plate.

When the overflow plate or sieve plate is obtained, the upper layer of the liquid surface of the fourth reaction functional section is connected to the upper end 3/5-4/5 of the third reaction functional section through a gas phase pipeline; the upper layer of the liquid surface of the third reaction functional section is connected to 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 the gas recovery device through a gas phase pipeline.

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

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

The first reaction functional section is connected to the gas recovery device via a gas phase pipeline.

In each functional section, the liquid phase with light components removed overflows from top to bottom to the next section by gravity. The material vapor from the second-stage reaction functional section at the bottom of the tower contacts the mixed acid liquid entering from the top of the tower in the first-stage reaction functional section in countercurrent 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 this section is maintained by the heat energy brought in by the higher-temperature non-condensable gas and saturated steam generated in the next-stage reaction functional section, and is balanced with the heat energy consumed by the vaporization of methanol and water in this section. The volatile methylal and methanol components are vaporized and leave the reactor with the rising non-condensable gas. The reaction liquid then enters the third and fourth-stage reaction functional sections through overflow and underflow in turn to heat up and react. The temperature of the third-stage reaction functional section is jointly maintained and controlled by the higher-temperature non-condensable gas and saturated steam generated in 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.

Alternatively, part of the liquid phase can flow to the next stage through the underflow pipe as an auxiliary liquid flow, and the flow rate can be adjusted by an automatic valve to balance the liquid level and pressure of each reaction functional area. As a special case, when the underflow pipe valve opening is 0% or the reactor is not provided with an underflow passage at this stage, all the liquid flows through the overflow pipe into the next stage reaction functional section.

When sieve plates are used to divide functional areas, a small amount of liquid flows through the sieve holes of the tower plate to the next section.

In each functional section, the gas phase of each level flows from bottom to top to the upper section by pressure difference, and maintains a certain height of gas-liquid contact in the upper section for mass transfer and heat transfer. The gas-liquid mass transfer and heat transfer are enhanced through stripping and aeration, and the gas stripping effect is played to quickly remove formaldehyde, methylal, methyl chloride and other materials in the material.

The light components in the reaction liquid (methanol, water, hydrogen chloride, and methylal and chloromethane generated during the acidolysis reaction) form a gas phase and are discharged from the gas phase pipes at the top of the first reaction functional section, the second reaction functional section, the third reaction functional section, and the fourth reaction functional section. Among them, the top of the first reaction functional section is the top of the tower. The gas phase tail gas generated in the second reaction functional section is discharged from the top of the tower after mass transfer and heat transfer in the first reaction functional section.

Alternatively, part of the gas phase can be directly sent to the gas phase main pipe through the gas phase pipeline as an auxiliary gas flow, and the flow rate can be adjusted by an automatic control valve to balance the pressure of each reaction functional zone. As a special case, when the valve opening of the auxiliary gas flow pipeline of the current reaction stage is 0% or the reactor is not provided with an auxiliary gas flow passage, the gas flow all flows from bottom to top to the next reaction functional stage by the pressure difference.

The "re-mixing" problem faced in the process of continuous batch stirring tank process improvement has been solved, and the problems of incomplete reaction (raw materials) of the original continuous technology have been solved. Therefore, the acid hydrolysis and hydrolysis chemical reaction process is fully and thoroughly, the continuous operation is stable and reliable, and the entire acid hydrolysis reaction is completed in one reactor, and no enamel kettle is required for further auxiliary reaction; compared with the original batch stirring process, the yield is high, the heat is cascaded, and the steam energy consumption is low.

BRIEF DESCRIPTION OF THE DRAWINGS

Figure 1 is a continuous reaction system for glyphosate API of Example 1, wherein: 1. glyphosate mixed acid liquid storage tank, 2. acid dealcoholization reactor, 3. first reaction functional section, 4. second reaction functional section, 5. third reaction functional section, 6. fourth reaction functional section, 7. heater 1, 8. heater 2, 9. gas recovery device, 10. crystallizer, 11-1, 11-2, 11-3, 11-4, 11-5, 11-6 are all circulation pumps, 12. partition.

Figure 2 is a structural diagram of the partition.

Fig. 3 is a continuous reaction system of glyphosate API of Example 2, wherein: 1'. glyphosate mixed acid liquid storage tank, 2'. acid deethanolation reactor, 3'. first reaction functional section, 4'. second reaction functional section, 5'. third reaction functional section, 6'. fourth reaction functional section, 7'. heater 1, 8'. heater 2, 9'. gas recovery device, 10'. crystallizer, 11-1', 11-2', 11-3', 11-4', 11-5', 11-6' are all circulation pumps, 12'. partition.

Fig. 4 is a continuous reaction system of glyphosate API of Example 3, wherein: 1". glyphosate mixed acid liquid storage tank; 2". acid deethanolation reactor; 3". first reaction functional section; 4". second reaction functional section; 5". third reaction functional section; 6". fourth reaction functional section; 7". heater 1; 8". heater 2; 9". gas recovery device; 10". crystallizer; 11-1", 11-2", 11-3", 11-4", 11-5", 11-6" are all circulation pumps; 12". partition.

Fig. 5 is a continuous reaction system of glyphosate API of Example 4, wherein 1"'. glyphosate mixed acid liquid storage tank, 2"'. acid deethanolation reactor, 3"'. first reaction functional section, 4"'. second reaction functional section, 5"'. third reaction functional section, 6"'. fourth reaction functional 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 all circulation pumps, 12"'. partition.

Figure 6 is a diagram of the overflow of the partition.

DETAILED DESCRIPTION

Glyphosate mixed acid solution is a mixed acid solution obtained by acidifying a synthetic liquid during the continuous synthesis of glyphosate by the glycine method. For example, references CN1037396A and CN111205319A all obtained glyphosate mixed acid solution. This glyphosate mixed acid solution is a mixed acid solution that is difficult to handle and is well known to those skilled in the art.

Example 1

The invention relates to a continuous reaction system for glyphosate raw materials. A glyphosate mixed acid liquid storage tank 1 is connected to an acid de-alcoholization reactor 2. The acid de-alcoholization 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 packing section. Other adjacent reaction functional sections are separated by a partition 12. The partition 12 cannot realize the up and down movement of materials.

The lower part of the second reaction functional section 4 is connected to the circulation 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 to the circulation pump through a liquid phase pipeline and then connected to the heater 7, and the heater 7 is connected to the middle part of the third reaction functional section 5.

A slurry discharge port is provided at the bottom of the fourth reaction functional section 6, and the slurry discharge port is connected to a circulation pump via a liquid phase pipeline. The circulation 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 via the heater 2 8.

The upper 1/5 of the second reaction functional section 4 is connected to the upper 3/5 of the third reaction functional section 5 via a liquid phase pipeline.

The upper 1/5 of the third reaction functional section 5 is connected to the upper 3/5 of the fourth reaction functional section 6 via a liquid phase pipeline.

The upper layer of the liquid surface of the fourth reaction functional section 6 is connected to the upper 3/5 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 to the upper 3/5 of the second reaction functional section 4 through a gas phase pipeline.

The first reaction functional section 3 is connected to the gas recovery device 9 via a gas phase pipeline.

After the glyphosate mixed acid solution enters the first reaction functional section of the acid de-alcoholization reactor at a rate of 4m ³ /h, the liquid phase enters the second reaction functional section through the filler of the first reaction functional section. After the reaction liquid reacts in the second reaction section for about half an hour, it enters the third reaction functional section through the overflow pipe with a flow rate of about 3.0m ³ /h; after the reaction liquid reacts in the third reaction section for about 1 hour, it enters the fourth reaction functional section through the overflow pipe with a flow rate of about 1.6m ³ /h; the flow rates of the second, third and fourth circulation pumps are controlled to be 10m ³ /h for the full circulation of the second, third and fourth stage reaction liquid; by controlling the steam volume of the heater, the temperature of the third and fourth stages is controlled to 100℃ and 130℃, and the temperature of the first and second stages is measured to be 46℃ and 72℃; the reaction liquid stays in the acid de-alcoholization reactor for 1-4 hours; the gas phase operating pressure control range of the first and second reaction functional sections of the reactor is -10kPa; the operating pressure of the third reaction functional section of the reactor is 0～50kPa, and the DCS should be set with an ultra-high limit alarm; the operating pressure of the fourth reaction functional section of the reactor is 10-50kPa, and the DCS should be set with an ultra-high limit alarm to achieve the gas phase of the fourth reaction functional section entering the third reaction functional section, the third reaction functional section entering 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 through the first reaction functional section. At 35 days, the flow rate of glyphosate slurry produced was ^1.09m3 /h, the glyphosate content was 22.61%, and the total recovery rate was 84.94%.

Example 2

The invention discloses a continuous reaction system for glyphosate raw materials, wherein a glyphosate mixed acid liquid storage tank 1' is connected to an acid decoholization reactor 2', and the acid decoholization 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, wherein the first reaction functional section 3' is a packing section, and other adjacent reaction functional sections are separated by a partition 12', and the partition 12' cannot realize the up and down movement of materials.

The lower part of the second reaction functional section 4' is connected to the circulation 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 to the circulation pump through the liquid phase pipeline and then connected to the heater 7', and the heater 7' is connected to the middle part of the third reaction functional section 5'.

A slurry discharge port is provided at the bottom of the fourth reaction functional section 6', and the slurry discharge port is connected to a circulation pump via a liquid phase pipeline. The circulation 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' via the heater 2 8'.

The upper 1/5 of the second reaction functional section 4' is connected to the upper 4/5 of the third reaction functional section 5' via a liquid phase pipeline.

The upper 1/5 of the third reaction functional section 5' is connected to the upper 4/5 of the fourth reaction functional section 6' via a liquid phase pipeline.

The upper layer of the liquid surface of the fourth reaction functional section 6' is connected to the gas recovery device 9' via a 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' via a gas phase pipeline.

The first reaction functional section 3' is connected to the gas recovery device 9' via a gas phase pipeline.

After the glyphosate mixed acid solution enters the first reaction functional section of the acid de-alcoholization reactor at a rate of 4m ³ /h, the liquid phase enters the second reaction functional section through the filler of the first reaction functional section. After the reaction liquid reacts in the second reaction section for about half an hour, it enters the third reaction functional section through the overflow pipe with a flow rate of about 3.2m ³ /h; after the reaction liquid reacts in the third reaction section for about 1 hour, it enters the fourth reaction functional section through the overflow pipe with a flow rate of about 1.7m ³ /h; the flow rates of the second, third and fourth circulation pumps are controlled to be 10m ³ /h for the full circulation of the second, third and fourth stage reaction liquid; by controlling the steam volume of the heater, the temperature of the third and fourth stages is controlled to 100℃ and 130℃, and the temperature of the first and second stages is measured to be 44℃ and 70℃; the reaction liquid stays in the acid de-alcoholization reactor for 1-4 hours; the gas phase operating pressure control range of the first and second reaction functional sections of the reactor is -10kPa; the operating pressure of the third reaction functional section of the reactor is 0～50kPa, and the DCS should be set with an ultra-high limit alarm; the operating pressure of the fourth reaction functional section of the reactor is 10-50kPa, and the DCS should be set with an ultra-high limit alarm, and the gas phase of the first, third and fourth reaction functional sections is connected to the gas recovery device through the gas phase pipeline. At 35 days, the flow rate of glyphosate slurry produced is ^1.10m3 /h, the glyphosate content is 22.00%, and the total recovery rate is 83.48%.

Example 3

The invention discloses a continuous reaction system for glyphosate raw materials. A glyphosate mixed acid liquid storage tank 1" is connected to an acid deethanolation reactor 2", and the acid deethanolation 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 packing section, and other adjacent reaction functional sections are separated by an overflow plate 12", and the overflow plate 12" enables the material to move up and down, but cannot move from bottom to top.

The lower part of the second reaction functional section 4" is connected to the circulation 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 to the circulation pump through a liquid phase pipeline and then connected to a heater 7", and the heater 7" is connected to the middle part of the third reaction functional section 5".

A slurry discharge port is provided at the bottom of the fourth reaction functional section 6", and the slurry discharge port is connected to a circulation pump via a liquid phase pipeline. The circulation 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" via the heater 2 8".

The upper 2/5 portion of the second reaction functional section 4" is connected to the upper 3/5 portion of the third reaction functional section 5" via a liquid phase pipeline.

The third reaction functional section 5" is connected at 2/5 of the upper end to the fourth reaction functional section 6" at 3/5 of the upper part via a liquid phase pipeline.

The upper layer of the liquid surface of the fourth reaction functional section 6" is connected to the upper end 3/5 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 to 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 the gas recovery device 9" via a gas phase pipeline.

After the glyphosate mixed acid solution enters the first reaction functional section of the acido-dealcoholization reactor at a rate of 2.5 m ³ /h, the liquid phase enters the second reaction functional section through the filler of the first 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 with a flow rate of about 1.5 m ³ /h; after the reaction liquid reacts in the third reaction section for about 3 hours, it enters the fourth reaction functional section through the downcomer with a flow rate of about 1 m ³ /h; the flow rate of the second, third and fourth circulation pumps is controlled to be 8 m ³ /h for the full circulation of the second, third and fourth stage reaction liquids; by controlling the steam volume of the heater, the temperature of the third and fourth stages is controlled to 100℃ and 130℃, and the temperature of the first and second stages is measured to be 48℃ and 73℃; the reaction liquid stays in the acid de-alcoholization reactor for 5-7 hours; the gas phase of the fourth reaction functional stage enters the third reaction functional stage, the gas phase of the third reaction functional stage enters the second reaction functional stage, and the gas phase of the second reaction functional stage is connected to the gas recovery device through the gas phase pipeline through the first reaction functional stage. At 35 days, the flow rate of glyphosate slurry produced is ^0.81m3 /h, the glyphosate content is 23.31%, and the total yield is 87.04%.

Example 4

The invention discloses a continuous reaction system for glyphosate raw materials, wherein a glyphosate mixed acid liquid storage tank 1'' is connected to an acid decoholization reactor 2'', wherein the acid decoholization 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, wherein the first reaction functional section 3'' is a packing section, and other adjacent reaction functional sections are separated by an overflow plate 12'', wherein the overflow plate 12'' enables the material to move up and down, but cannot achieve movement from bottom to top.

The lower part of the second reaction functional section 4'' is connected to the circulation pump via 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 to the circulation pump through the liquid phase pipeline and then connected to the heater 7''. The heater 7'' is connected to the middle part of the third reaction functional section 5''.

A slurry discharge port is provided at the bottom of the fourth reaction functional section 6”’, and the slurry discharge port is connected to a circulation pump via a liquid phase pipeline. The circulation 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”’ via the heater 2 8”’.

The second reaction functional section 4' ...

The third reaction functional section 5' ...

The gas phase pipeline of the upper layer of the liquid surface of the fourth reaction functional section 6"' is connected to the 4/5 position of the upper end of the third reaction functional section 5"' and the gas recovery device 9"'; the upper layer of the liquid surface of the third reaction functional section 5"' is connected to the 4/5 position of the upper end 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 a gas recovery device 9'' via a gas phase pipeline.

After the glyphosate mixed acid solution enters the first reaction functional section of the acido-dealcoholization reactor at a rate of 2.5m ³ /h, the liquid phase enters the second reaction functional section through the filler of the first 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 with a flow rate of about 1.7m ³ /h; after the reaction liquid reacts in the third reaction section for about 3 hours, it enters the fourth reaction functional section through the downcomer with a flow rate of about 1.2m ³ /h; the flow rate of the second, third and fourth circulation pumps is controlled to be 8m ³ /h for the full circulation of the second, third and fourth stage reaction liquids; by controlling the steam volume of the heater, the temperature of the third and fourth stages is controlled to be 100℃ and 130℃, and the temperature of the first and second stages is measured to be 45℃ and 70℃; the reaction liquid stays in the acid de-alcoholization reactor for 5-7 hours; the gas phase of the fourth reaction functional stage enters the third reaction functional stage, the gas phase of the third reaction functional stage enters the second reaction functional stage, the gas phase of the second reaction functional stage is connected to the gas recovery device through the gas phase pipeline through the first reaction functional stage, and the gas phase of the third and fourth reaction functional stages is connected to the gas recovery device through the gas phase pipeline. At 35 days, the flow rate of glyphosate slurry produced is ^0.80m3 /h, the glyphosate content is 22.75%, and the total yield is 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.

Images