CN211190162U - Reactor for preparing diethyl methylphosphonite - Google Patents

Abstract

The utility model provides a reactor for preparing diethyl methylphosphonite, which comprises a kettle body, a kettle cover, a stirrer and a power device, wherein the kettle body and the kettle cover are buckled together; the power device is arranged above the kettle cover, and a power output shaft of the power device is in transmission connection with the top of the stirrer to provide stirring power for the stirrer; the stirrer is a double-layer paddle type stirrer; an upper jacket for cooling and a lower jacket for heating are arranged outside the kettle body, a heat exchange coil is further arranged in the lower jacket, and the heat exchange coil is coiled and attached to the outer wall of the kettle body; the heat exchange area of the upper jacket accounts for 15% of the total heat exchange area, and the heat exchange area of the lower jacket accounts for 85% of the total heat exchange area. The utility model discloses separate freezing salt solution and steam and come, be showing on the one hand and reduced chloride ion to the corruption that presss from both sides the cover, improved the life of reactor, on the other hand has improved heat transfer effect greatly, glues thick gradually at the material system, guarantees the accurate control of reaction temperature under the poor condition of heat transfer.

Description

Reactor for preparing diethyl methylphosphonite

Technical Field

The utility model relates to a reactor is used in preparation of methyl phosphinic acid diethyl ester belongs to pesticide synthesis technical field.

Background

Glufosinate is a high-efficiency, low-toxicity and non-selective contact-type organic phosphine herbicide developed by German Hoechst (Hoechst), is used for controlling annual and perennial dicotyledonous and gramineous weeds in orchards, vineyards, potato fields, uncultivated lands and the like, and is the second herbicide variety in the world. At present, the conventional preparation method of glufosinate-ammonium comprises a chemical method and a fermentation method, wherein the chemical method is more popular, such as the strecker method.

When preparing the key intermediate diethyl methylphosphonite of the glufosinate-ammonium pesticide, the raw materials are usually methyl magnesium chloride and diethyl phosphite chloride, firstly, the diethyl phosphite chloride is put into a reaction kettle, the temperature is reduced to 15 ℃, then, the methyl magnesium chloride is dripped, the temperature is controlled to be 15-20 ℃ in the whole dripping process, and then, the temperature is kept at 20-25 ℃ after the dripping is finished. The reaction is an exothermic reaction, the viscosity of the material is gradually increased along with the progress of the reaction, the heat transfer capacity of the material is gradually reduced, and the reaction requires precise reaction temperature and low temperature, so that steam/cooling brine is frequently used for controlling the temperature within a specified range in actual operation.

Under the frequent switching of steam/cooling brine, the reaction kettle jacket is in a repeated high-temperature/low-temperature environment, and the cooling brine contains a large amount of chloride ions, so that the reaction kettle jacket is accelerated and violent in corrosion, the reaction kettle jacket is extremely easy to damage, the service life of the equipment is shortened, and the maintenance cost of the equipment is increased.

SUMMERY OF THE UTILITY MODEL

In order to solve the problems in the prior art, the present invention provides a reactor for preparing diethyl methylphosphonite.

In order to solve the technical problem, the utility model discloses the technical scheme who adopts is:

a reactor for preparing diethyl methylphosphonite comprises a kettle body, a kettle cover, a stirrer and a power device, wherein the kettle body and the kettle cover are buckled together; the power device is arranged above the kettle cover, and a power output shaft of the power device is in transmission connection with the top of the stirrer to provide stirring power for the stirrer; the stirrer is a double-layer paddle type stirrer; an upper jacket for cooling and a lower jacket for heating are arranged outside the kettle body, a heat exchange coil is further arranged in the lower jacket, and the heat exchange coil is coiled and attached to the outer wall of the kettle body; the heat exchange area of the upper jacket accounts for 15% of the total heat exchange area, and the heat exchange area of the lower jacket accounts for 85% of the total heat exchange area.

The utility model discloses a further improvement lies in: the upper part of the upper jacket is provided with an upper jacket feed hole, the lower part of the upper jacket is provided with an upper jacket discharge hole, the upper jacket feed hole is connected with a cooling brine inlet pipe, and the upper jacket discharge hole is connected with a cooling brine return pipe.

The utility model discloses a further improvement lies in: the bottom of the upper jacket is provided with a residual liquid outlet, and the top of the upper jacket is provided with an exhaust port.

The utility model discloses a further improvement lies in: the lower jacket is provided with a lower jacket feed hole and a lower jacket discharge hole which are communicated with the inner cavity of the jacket, and a coil feed hole and a coil discharge hole which are communicated with the heat exchange coil; lower clamp cover feed port, coil pipe feed port all are linked together with the steam conduit of mill, and lower clamp cover discharge opening, coil pipe discharge opening all are linked together with condensation return water pipe.

The utility model discloses a further improvement lies in: the power device comprises a motor, a speed reducer and a mounting rack. The mounting bracket is fixed on the kettle cover, the motor is fixed above the mounting bracket, the power output shaft of the motor is connected with the speed reducer positioned in the mounting bracket, and the power output shaft of the speed reducer is connected with the stirring rod through a coupling in a transmission way after penetrating through the kettle cover.

The utility model discloses a further improvement lies in: the reactor is also provided with a temperature control device for monitoring the temperature of the reaction system in real time.

Due to the adoption of the technical scheme, the utility model discloses the technological progress who gains is:

the utility model provides a reactor is used in preparation of methyl phosphinic acid diethyl ester, simple structure, design benefit lets in frozen salt solution in pressing from both sides the cover, realize cooling function, let in steam in pressing from both sides the cover down, realize the heating function of rising temperature, separate frozen salt solution and steam, avoid direct contact, chloride ion in the frozen salt solution is difficult for corroding pressing from both sides the cover under the low temperature condition, reation kettle's life has been improved greatly, and chlorine ion's smuggleing secretly also can be avoided in the steam condensate water.

The utility model discloses a still be provided with heat exchange coil in the lower clamp cover, further strengthened the heat transfer effect, moreover, press from both sides the cover heat transfer and combine together the use with the coil pipe heat transfer, can realize the accurate control to material temperature, guarantee that reaction temperature is in the regulation within range.

The utility model discloses a double-deck paddle formula agitator can realize the intensive mixing between the upper and lower floor's material, especially when material viscosity increases the back temperature regulation, can be with the low temperature material on upper strata and the high temperature material of lower floor abundant contact, improve heat transfer effect, guarantee the homogeneous and the stability of reaction system temperature.

Drawings

Fig. 1 is a schematic view of the overall structure of the present invention;

the method comprises the following steps of 1-kettle body, 2-kettle cover, 3-stirrer, 41-motor, 42-speed reducer, 43-mounting rack, 5-kettle clamp, 6-upper jacket, 61-residual liquid outlet, 62-exhaust port, 63-upper jacket feed hole, 64-upper jacket discharge hole, 7-lower jacket, 71-lower jacket feed hole, 72-lower jacket discharge hole, 8-heat exchange coil, 81-coil feed hole, 82-coil discharge hole and 9-hanging ring.

Detailed Description

The present invention will be described in detail below with reference to the accompanying drawings.

A reactor for preparing diethyl methylphosphonite is shown in figure 1 and comprises a kettle body 1, a kettle cover 2, a stirrer 3 and a power device. The kettle body 1 and the kettle cover 2 are fastened and then fixed by a plurality of kettle clamps 5; the kettle clamps 5 are uniformly arranged along the circumferential direction and firmly connect the kettle body 1 and the kettle cover 2; a sealing gasket is arranged on the connecting surface of the kettle body 1 and the kettle cover 2 to ensure the sealing performance of the connecting part.

A power device is arranged above the kettle cover 2. The power device comprises a motor 41, a speed reducer 42 and a mounting frame 43. The mounting frame 43 is fixed on the kettle cover 2, the motor 41 is fixed above the mounting frame 43, a power output shaft of the motor is connected with a speed reducer positioned in the mounting frame 43, and a power output shaft of the speed reducer penetrates through the kettle cover 2 and is in transmission connection with the stirring rod through a coupler; the stirrer 3 is driven by the motor 41 to rotate, so that the materials in the reactor are uniformly mixed. The stirrer 3 is a double-layer paddle type stirrer 3, and after the reaction system is gradually thickened, the stirrer 3 in the form can ensure that the upper layer and the lower layer of the feed liquid are fully mixed and the heat transfer is uniform.

A jacket is arranged outside the kettle body 1, and specifically comprises an upper jacket 6 and a lower jacket 7, wherein the upper jacket 6 is used for cooling materials in the kettle, the lower jacket 7 is used for heating the materials in the kettle, and steam and saline water flow through different jackets to avoid doping; the heat exchange area of the upper jacket 6 accounts for 15% of the total heat exchange area, and the heat exchange area of the lower jacket 7 accounts for 85% of the total heat exchange area.

An upper jacket feeding hole 63 is formed in the upper portion of the upper jacket 6, an upper jacket discharging hole 64 is formed in the lower portion of the upper jacket 6, the upper jacket feeding hole 63 is connected with a cooling brine inlet pipe, the upper jacket discharging hole 64 is connected with a cooling brine return pipe, and cooling brine enters an inner cavity of the upper jacket 6 and cools materials in the kettle through partition wall heat exchange. And a residual liquid outlet is formed in the bottom of the upper jacket 6, the residual liquid outlet is closed during circulating cooling, and the residual brine is discharged after the cooling is stopped, so that the corrosion of chloride ions to the jacket is reduced. An exhaust port is arranged at the top of the upper clamping sleeve 6, so that the clamping sleeve is prevented from being damaged by pressure build-up.

The lower part of the kettle body 1 is coated by the lower clamping sleeve 7, the heat exchange coil 8 is further arranged in the lower clamping sleeve 7, and the heat exchange coil 8 is attached to the outer wall of the kettle body 1 and is coiled to enhance the heat transfer effect of the sticky system. A lower jacket feed hole 71 and a coil feed hole 81 are formed in the upper part of the lower jacket 7, a lower jacket discharge hole 72 and a coil discharge hole 82 are formed in the bottom of the lower jacket 7, wherein the lower jacket feed hole 71 and the lower jacket discharge hole 72 are communicated with the inner cavity of the lower jacket to form a jacket heat exchange channel; coil pipe feed opening 81, coil pipe discharge opening 82 all are linked together with heat transfer coil 8, form coil pipe heat transfer passageway. The lower jacket feed hole 71 and the coil feed hole 81 are communicated with a factory steam pipeline, and the lower jacket discharge hole 72 and the coil discharge hole 82 are communicated with a condensation water return pipeline; steam gets into down presss from both sides cover or heat exchange coil pipe, heats the material in the cauldron after by condensation return water pipe discharge, presss from both sides the cover heat transfer and combines together with the coil pipe heat transfer, can realize the accurate control to local temperature, is particularly useful for such more and more viscidity of diethyl methylphosphonite preparation system, the more and more poor system of heat transfer effect.

And the kettle cover 2 and the kettle body 1 are both provided with hoisting rings 9 for hoisting and assembling the kettle cover 2 and the kettle body 1. The number of the lifting rings 9 on the kettle cover 2 and the kettle body 1 is four, and the lifting rings are uniformly arranged along the circumference.

The reactor also comprises a temperature control device, the temperature control device comprises a thermometer and a digital display device connected with the thermometer, the thermometer is inserted into the middle of the reactor, the real-time temperature of the material in the middle is detected, data is transmitted to the digital display device, and the operator can accurately read the temperature through the digital display device so as to perform cooling or heating operation.

The utility model discloses the reactor is when using, through the cooling that the upper jacket 6 realized the material, the heating that the lower jacket 7 realized the material, through 3 misce benes of double-deck paddle agitator in the cauldron, guarantees that material temperature control is at 15 ℃ -20 ℃.

The above is only the preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.

Claims (6)

1. A reactor for preparing diethyl methylphosphonite is characterized in that: comprises a kettle body (1), a kettle cover (2), a stirrer (3) and a power device which are buckled together; the power device is arranged above the kettle cover (2), and a power output shaft of the power device is in transmission connection with the top of the stirrer (3) to provide stirring power for the stirrer (3); the stirrer (3) is a double-layer blade type stirrer (3); an upper jacket (6) for cooling and a lower jacket (7) for heating are arranged outside the kettle body (1), a heat exchange coil (8) is further arranged in the lower jacket (7), and the heat exchange coil (8) is coiled and attached to the outer wall of the kettle body (1); the heat exchange area of the upper jacket (6) accounts for 15% of the total heat exchange area, and the heat exchange area of the lower jacket (7) accounts for 85% of the total heat exchange area.

2. The reactor for the preparation of diethyl methylphosphonite according to claim 1, wherein: an upper jacket feeding hole (63) is formed in the upper portion of the upper jacket (6), an upper jacket discharging hole (64) is formed in the lower portion of the upper jacket feeding hole, the upper jacket feeding hole (63) is connected with a cooling brine inlet pipe, and the upper jacket discharging hole (64) is connected with a cooling brine return pipe.

3. The reactor for the preparation of diethyl methylphosphonite according to claim 2, wherein: the bottom of the upper jacket (6) is provided with a residual liquid outlet (61), and the top of the upper jacket (6) is provided with an exhaust port (62).

4. The reactor for the preparation of diethyl methylphosphonite according to claim 1, wherein: a lower jacket feed hole (71) and a lower jacket discharge hole (72) which are communicated with the inner cavity of the jacket, and a coil feed hole (81) and a coil discharge hole (82) which are communicated with the heat exchange coil (8) are formed in the lower jacket (7); lower jacket feed port (71), coil pipe feed port (81) all are linked together with the steam conduit of mill, and lower jacket discharge opening (72), coil pipe discharge opening (82) all are linked together with condensation return water pipe.

5. The reactor for the preparation of diethyl methylphosphonite according to claim 1, wherein: the power device comprises a motor (41), a speed reducer (42) and an installation frame (43), wherein the installation frame (43) is fixed on the kettle cover (2), the motor (41) is fixed above the installation frame (43), a power output shaft of the speed reducer is connected with the speed reducer inside the installation frame (43), and the power output shaft of the speed reducer is connected with the stirring rod through a coupling in a transmission mode after penetrating through the kettle cover (2).

6. The reactor for the preparation of diethyl methylphosphonite according to claim 1, wherein: the reactor is also provided with a temperature control device for monitoring the temperature of the reaction system in real time.

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