CN219424366U - Device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid oxidation - Google Patents

Abstract

The utility model discloses a device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid oxidation, which comprises a loop reactor, a reaction device and a reaction device, wherein the loop reactor is used for material internal circulation mixing reaction; a preheating system for preheating the material entering the loop reactor; an external circulation system for circulating the mixed material in the loop reactor; the heat exchange system is used for removing the reaction heat of the loop reactor, performing strong external circulation under the action of the external circulation system, providing the reaction system for summarizing the oxygen solubility, improving the three-phase contact probability of gas, liquid and solid, mixing more fully, enhancing the oxygen content in liquid, increasing the gas-liquid contact area, thereby achieving the effect of enhancing mass transfer, further reducing the reaction time, improving the reaction efficiency, performing temperature and pressure on-line monitoring on the loop reactor by temperature monitoring and pressure monitoring, controlling the temperature and pressure in the reactor by the external circulation heat exchanger and the regulating valve, detecting the oxygen content in tail gas by the oxygen content detector, and judging the reaction end point by oxygen content change.

Description

Device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid oxidation

Technical Field

The utility model relates to the field of oxidation reaction devices for preparing glyphosate from N-phosphonomethyl iminodiacetic acid, in particular to a device for preparing glyphosate from N-phosphonomethyl iminodiacetic acid by oxidation, and provides equipment for preparing glyphosate from N-phosphonomethyl iminodiacetic acid by catalytic oxidation, which has higher mass transfer efficiency and higher efficiency and energy conservation.

Background

In the IDA method glyphosate production process, the N-phosphonomethyl iminodiacetic acid oxidation reaction is the most important reaction process, and the currently commonly adopted N-phosphonomethyl iminodiacetic acid oxidation reaction method in the industry is to add prepared materials into an oxidation reaction kettle with stirring and reel pipe cooling, and then to introduce compressed air to carry out intermittent reaction at a certain temperature and pressure.

The oxidation reaction device is a bottleneck in glyphosate production due to the problems of frequent reaction overtemperature alarm, long reaction time, material transfer blockage and the like caused by insufficient heat transfer (heat removal), particularly low mass transfer efficiency and poor oxygen dissolution effect due to insufficient stirring.

Disclosure of Invention

In order to solve the technical problems, the utility model provides a device for preparing glyphosate by oxidizing N- (phosphonomethyl) iminodiacetic acid, which comprises a loop reactor for internal circulation mixing reaction of materials; a preheating system for preheating the material entering the loop reactor; an external circulation system for circulating the mixed material in the loop reactor; and a heat exchange system for removing the heat of reaction of the loop reactor.

Preferably: the circulation reactor is internally provided with a flow guide pipe which is connected with an injection mixer, and the injection mixer is connected with an injection nozzle.

Preferably: the top end of the loop reactor is also provided with temperature monitoring and pressure monitoring.

Preferably: the preheating system comprises a preheater, and the heat source of the preheater is steam or hot water.

Preferably: the feed inlet of the preheater is connected with the batching kettle through a pipeline, and the discharge outlet of the preheater is connected with the spray nozzle through a pipeline.

Preferably: the external circulation system comprises an external circulation pump, a feed inlet of the external circulation pump is connected with the loop reactor through a pipeline, and a discharge outlet of the external circulation pump is connected with the jet mixer through a pipeline.

Preferably: the heat exchange system comprises an external circulation heat exchanger, and the external circulation heat exchanger is used for heat exchange.

Preferably: the top of the loop reactor is also provided with a tail gas outlet, and the tail gas outlet is provided with a regulating valve and an oxygen content detector.

Preferably: the jet mixer is connected with an air buffer tank through a pipeline, and the air buffer tank is connected with a compressed air conveying pipe outside the boundary.

Preferably: the air buffer tank is also provided with pressure monitoring for monitoring the internal pressure of the air buffer tank.

The utility model has the technical effects and advantages that:

the method has the advantages that the strong external circulation is carried out under the action of the external circulation system, the total oxygen solubility of the reaction system is provided, the gas-liquid-solid three-phase contact probability is improved, the mixing is more sufficient, the oxygen content in the liquid state is enhanced, the gas-liquid contact area is increased, the mass transfer enhancing effect is achieved, the reaction time is further reduced, and the reaction efficiency is improved.

Drawings

Fig. 1 is a schematic structural diagram of an apparatus for preparing glyphosate by oxidation of N-phosphonomethyl iminodiacetic acid according to an embodiment of the present application.

In the figure: 1. a loop reactor; 2. a flow guiding pipe; 3. a jet mixer; 4. a spray nozzle; 5. monitoring the temperature; 6. monitoring pressure; 7. an external circulation heat exchanger; 8. an external circulation pump; 9. an air buffer tank; 10. a preheater; 11. an oxygen content detector.

Detailed Description

The utility model will be described in further detail with reference to the drawings and the detailed description. The embodiments of the utility model have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the utility model in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments were chosen and described in order to best explain the principles of the utility model and the practical application, and to enable others of ordinary skill in the art to understand the utility model for various embodiments with various modifications as are suited to the particular use contemplated.

Referring to fig. 1, in this embodiment, an apparatus for preparing glyphosate by oxidation of N-phosphonomethyl iminodiacetic acid is provided, after oxygen-containing gas is introduced in the presence of a catalyst, the apparatus is reacted to prepare glyphosate, and the apparatus comprises a loop reactor 1, a preheating system, an external circulation system and a heat exchange system, wherein the loop reactor 1 is internally provided with a flow guide 2, the flow guide 2 is connected with a jet mixer 3, the jet mixer 3 is connected with a jet nozzle 4, the loop reactor 1 is used as a main reactor, circulating materials are jetted downwards from the jet nozzle 4, and after being fully mixed with oxygen or compressed air in the jet mixer 3, internal circulation is performed through the flow guide 2.

Further, a temperature monitor 5 and a pressure monitor 6 are also installed at the top end of the loop reactor 1 to monitor the temperature and pressure inside the loop reactor 1.

In this embodiment, the preheating system includes a preheater 10, the heat source of the preheater 10 is steam or hot water, the feed inlet of the preheater 10 is connected to the batch kettle through a pipeline, the discharge outlet of the preheater 10 is connected to the spray nozzle 4 through a pipeline, and the preheater 10 is used to preheat the material, so that the temperature of the material entering the loop reactor 1 from the preheater 10 reaches the reaction temperature range, and the reaction efficiency is improved.

In this embodiment, the external circulation system includes external circulation pump 8, the feed inlet of external circulation pump 8 passes through pipe connection loop reactor 1, the discharge gate of external circulation pump 8 passes through pipe connection jet mixer 3, carry out the external circulation through external circulation pump 8, carry out powerful external circulation under external circulation pump 8 effect, provide the reaction system and gather the oxygen solubility, improve the solid three-phase contact probability of gas-liquid, it is more abundant to mix, the oxygen content in the reinforcing liquid, increase gas-liquid area of contact, thereby reach the effect of reinforcing mass transfer, and then reduce reaction time, and improve reaction efficiency.

In this embodiment, the heat exchange system includes outer circulation heat exchanger 7, and outer circulation heat exchanger 7 is used for the heat transfer, and for traditional stirred tank reactor's heat transfer device, this outer circulation heat exchanger heat transfer area is not restricted, and heat transfer area is big, and the heat transfer is effectual, can in time remove the reaction heat, provides the guarantee for shortening reaction time, and reaction intrinsic safety factor improves.

The top of the loop reactor 1 is also provided with a tail gas outlet, the tail gas outlet is provided with a regulating valve and an oxygen content detector 11, the regulating valve regulates the pressure in the reactor, the oxygen content detector 11 judges the end point of the reaction through the on-line monitoring of the oxygen content in the tail gas, and when the reaction starts, the oxygen consumption is larger, and the oxygen content in the tail gas gradually decreases; when the reaction is gradually stable, the oxygen content in the tail gas keeps a lower stable value; when the reaction is finished, the oxygen consumption is reduced, the oxygen content in the tail gas is gradually increased, and when an ascending inflection point appears, the reaction end point is judged.

In this embodiment, the jet mixer 3 is connected to the air buffer tank 9 through a pipe, the air buffer tank 9 is connected to an external compressed air delivery pipe, and after compressed air or oxygen enters the air buffer tank 9, a buffering effect is achieved, and the air buffer tank 9 is further provided with a pressure monitor for monitoring the internal pressure of the air buffer tank 9.

The working principle of the utility model is as follows:

adding water, an active carbon catalyst and N- (phosphonomethyl) iminodiacetic acid into a batching kettle, stirring uniformly, then conveying the mixture to a loop reactor 1, heating the mixture to a set temperature through a preheater 10 in the conveying process, starting an outer circulation pump 8 for circulation after finishing conveying materials, conveying compressed air to a jet mixer 3 of the loop reactor 1 for mixing with the materials through an air buffer tank 9, circulating the mixture in the loop reactor 1 through a flow guide pipe 2 and performing outer circulation through an outer circulation pump 8, strengthening mass transfer, increasing the oxygen content in the system, removing a large amount of heat released by the reaction through the outer circulation heat exchanger 7, enhancing the heat transfer effect, controlling the temperature and the pressure in the reactor through the outer circulation heat exchanger 7 and a regulating valve, detecting the oxygen content in tail gas through the oxygen content detector 11, judging the end point of the reaction through oxygen content change, after the device is used, enabling the outer circulation heat exchanger 7 to perform heat exchange effect well, enabling the reaction to be removed in time, enabling the heat energy to be free of overtemperature alarm, shortening the oxidation reaction time by more than 40%, improving the glyphosate yield by more than 1% and improving the comprehensive energy consumption by more than 3.98%.

It will be apparent that the described embodiments are only some, but not all, embodiments of the utility model. All other embodiments, which can be made by those skilled in the art and which are included in the embodiments of the present utility model without the inventive step, are intended to be within the scope of the present utility model. Structures, devices and methods of operation not specifically described and illustrated herein, unless otherwise indicated and limited, are implemented according to conventional means in the art.

Claims (10)

1. The device for preparing the glyphosate by oxidizing N- (phosphonomethyl) iminodiacetic acid is characterized by comprising a loop reactor (1) for material internal circulation mixing reaction;

the preheating system comprises a preheater (10), wherein a feed inlet of the preheater (10) is connected with the batching kettle through a pipeline and is used for preheating materials entering the loop reactor (1);

the external circulation system comprises an external circulation pump (8), and a feed inlet of the external circulation pump (8) is connected with the loop reactor (1) through a pipeline and is used for circulating materials mixed in the loop reactor (1);

a heat exchange system comprising an external circulation heat exchanger (7) for removing heat of reaction from the loop reactor (1).

2. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 1, wherein a flow guide pipe (2) is arranged in the loop reactor (1), the flow guide pipe (2) is connected with a jet mixer (3), and the jet mixer (3) is connected with a jet nozzle (4).

3. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 1, wherein the top end of the loop reactor (1) is also provided with a temperature monitor (5) and a pressure monitor (6).

4. The device for preparing glyphosate by oxidation of N- (phosphonomethyl) iminodiacetic acid according to claim 1, wherein the heat source of the preheater (10) is steam or hot water.

5. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 4, wherein the discharge port of the preheater (10) is connected with the spray nozzle (4) through a pipeline.

6. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 1, wherein a discharge port of the external circulation pump (8) is connected with the jet mixer (3) through a pipeline.

7. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 1, wherein the external circulation heat exchanger (7) is used for heat exchange.

8. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 2, wherein a tail gas outlet is further arranged at the top of the loop reactor (1), and a regulating valve and an oxygen content detector (11) are arranged at the tail gas outlet.

9. The device for preparing glyphosate by N- (phosphonomethyl) iminodiacetic acid) oxidation according to claim 8, wherein the jet mixer (3) is connected with an air buffer tank (9) through a pipeline, and the air buffer tank (9) is connected with an external compressed air delivery pipe.

10. An apparatus for preparing glyphosate by oxidation of N-phosphonomethyl iminodiacetic acid as claimed in claim 9, wherein said air buffer tank (9) is further provided with pressure monitoring means for monitoring the internal pressure of the air buffer tank (9).