CN219984674U - Tubular reactor suitable for producing p-chlorophenylboronic acid - Google Patents

Tubular reactor suitable for producing p-chlorophenylboronic acid Download PDF

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Publication number
CN219984674U
CN219984674U CN202321387334.XU CN202321387334U CN219984674U CN 219984674 U CN219984674 U CN 219984674U CN 202321387334 U CN202321387334 U CN 202321387334U CN 219984674 U CN219984674 U CN 219984674U
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pipe body
pipe
tubular reactor
metering pump
quenching
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CN202321387334.XU
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张绪猛
李新
冯培良
毛洪军
郭振亚
王洋
苏毅
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Jinan Enlighten Biotechnology Co ltd
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Jinan Enlighten Biotechnology Co ltd
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Abstract

The utility model belongs to the technical field of chemical devices, and particularly relates to a tubular reactor suitable for producing p-chlorobenzoic acid, which comprises the following components: the quenching device comprises a first pipe body, a second pipe body, a quenching kettle, a first metering pump, a second metering pump and a pipeline mixer; the first pipe body and the second pipe body are coiled pipes, the coiled pipes are composed of inner pipes and outer pipes which are concentrically arranged, a cavity is formed between the inner pipes and the outer pipes, the outer surfaces of the inner pipes and the outer pipes are connected in a sealing mode, heat conducting medium inlets and heat conducting medium outlets are formed in the pipe walls of the outer pipes of the first pipe body and the second pipe body, and temperature detectors are arranged on the first pipe body and the second pipe body; one end of the first pipe body is connected with the first metering pump, and the other end of the first pipe body is connected with the pipeline mixer; one end of the second pipe body is connected with the pipeline mixer, and the other end of the second pipe body is connected with the quenching kettle; the second metering pump is connected with the pipeline mixer.

Description

Tubular reactor suitable for producing p-chlorophenylboronic acid
Technical Field
The utility model belongs to the technical field of chemical devices, and particularly relates to a tubular reactor suitable for producing p-chlorobenzoic acid.
Background
P-chlorophenylboronic acid is an important intermediate, can be used for preparing medicines such as tetrazolinone, boscalid, carbixamine and the like, and can also be applied to the preparation of novel organic electroluminescent materials. The preparation method of the p-chlorobenzeneboronic acid mainly comprises a catalytic boration method, an organolithium reagent method and a format reagent method, however, the catalytic boration method and the organolithium reagent method have higher cost and complex operation, and are not suitable for industrialized mass production.
At present, the Grignard reagent method is a relatively common production method of p-chlorobenzoic acid in industry. Chinese patent CN201910333205.4 discloses a method for synthesizing p-chlorobenzoic acid, which comprises preparing grignard reagent from p-dichlorobenzene, and adding boric acid ester dropwise into the grignard reagent to prepare p-chlorobenzoic acid. Chinese patent CN201410842468.5 discloses a method for synthesizing p-chlorobenzoic acid, which comprises preparing grignard reagent from p-dichlorobenzene, and dripping the grignard reagent into borate solution to prepare p-chlorobenzoic acid. In the prior art, the conventional reaction kettle type is used for preparing the p-chlorophenylboronic acid, which is an intermittent production mode, and has the advantages of complex operation, high energy consumption and poor safety. The grid reagent method needs to control low-temperature reaction to prevent side reaction, and is limited by the heat exchange capacity of a reaction kettle, the temperature difference is reduced, the temperature control difficulty is high, and the side reaction is more.
Disclosure of Invention
In order to solve the defects in the prior art, the utility model aims to provide a tubular reactor suitable for producing p-chlorophenylboronic acid. The pipe reactor is used for producing the p-chlorophenylboronic acid, so that the method can be used for continuous production, is easy to operate and implement, and has low energy consumption and high safety; the heat exchange is fast, the reaction temperature is easier to control, and the occurrence of side reaction can be effectively controlled.
In order to achieve the above object, the present utility model is realized by the following technical scheme:
in a first aspect, the present utility model provides a tubular reactor suitable for the production of p-chlorophenylboronic acid comprising: the quenching device comprises a first pipe body, a second pipe body, a quenching kettle, a first metering pump, a second metering pump and a pipeline mixer;
the first pipe body and the second pipe body are coiled pipes, the coiled pipes are composed of inner pipes and outer pipes which are concentrically arranged, a cavity is formed between the inner pipes and the outer pipes, the outer surfaces of the inner pipes and the outer pipes are connected in a sealing mode, heat conducting medium inlets and heat conducting medium outlets are formed in the pipe walls of the outer pipes of the first pipe body and the second pipe body, and temperature detectors are arranged on the first pipe body and the second pipe body;
one end of the first pipe body is connected with the first metering pump, and the other end of the first pipe body is connected with the pipeline mixer; one end of the second pipe body is connected with the pipeline mixer, and the other end of the second pipe body is connected with the quenching kettle; the second metering pump is connected with the pipeline mixer.
Preferably, the bending part of the coiled pipe is arc-shaped or right-angle-shaped.
Preferably, the cross section of the coiled pipe is circular.
Preferably, the heat conducting medium inlet is respectively arranged at one end of the first pipe body connected with the pipeline mixer and one end of the second pipe body connected with the quenching kettle.
Preferably, the heat-conducting medium outlet is respectively arranged at one end of the first pipe body connected with the first metering pump and one end of the second pipe body connected with the pipeline mixer.
Preferably, the coiled pipe is made of stainless steel, and the inner diameter of the inner pipe is 0.01-0.1m.
Preferably, the total length of the first pipe body and the second pipe body is 50-100m.
Preferably, the top of the quenching kettle is provided with a rotary stirrer, a hydrochloric acid feeding pipe and an ultrapure water feeding pipe.
Preferably, the material of the quenching kettle is enamel.
Preferably, a valve is arranged at one end of the second pipe body connected with the quenching kettle.
The beneficial effects obtained by one or more of the technical schemes of the utility model are as follows:
the tubular reactor can realize the continuous production of the p-chlorophenylboronic acid, is easy to operate and implement, has low energy consumption and high safety, and is easy to recycle by using the quenching kettle material.
The tubular reactor can realize rapid heat exchange through the heat conducting medium, and meanwhile, the temperature detector is arranged to detect the reaction temperature, so that the reaction temperature is easier to control, and the occurrence of side reaction can be effectively controlled.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model.
FIG. 1 is a schematic structural view of a tubular reactor suitable for producing p-chlorophenylboronic acid according to example 1 of the present utility model;
fig. 2 is a sectional view of the first tube body 1 and the second tube body 2 in fig. 1.
The symbols in the above drawings represent respectively: 1-first pipe body, 2-second pipe body, 3-quenching cauldron, 4-first measuring pump, 5-second measuring pump, 6-pipe mixer, 7-heat conduction medium import, 8-heat conduction medium export, 9-thermoscope, 10-valve, 11-rotatory agitator, 12-hydrochloric acid inlet pipe, 13-ultrapure water inlet pipe, 14-inner tube, 15-outer tube, 16-cavity.
Detailed Description
In order to enable those skilled in the art to more clearly understand the technical scheme of the present utility model, the technical scheme of the present utility model will be described in detail below with reference to specific examples and comparative examples.
Example 1
As shown in fig. 1, a tubular reactor suitable for producing p-chlorophenylboronic acid, comprising: a first pipe body 1, a second pipe body 2, a quenching kettle 3, a first metering pump 4, a second metering pump 5 and a pipeline mixer 6. One end of the first pipe body 1 is connected with the first metering pump 4, and the other end of the first pipe body is connected with the pipeline mixer 6; one end of the second pipe body 2 is connected with the pipeline mixer 6, and the other end is connected with the quenching kettle 3 and is provided with a valve 10; the second metering pump 5 is connected to the pipe mixer 6. The first metering pump 4 and the second metering pump 5 can be respectively used for pumping boric acid ester and format reagent according to production requirements.
The first pipe body 1 and the second pipe body 2 are stainless steel coiled pipes. The first pipe body 1 is bent at a right angle closest to one end connected with the pipeline mixer 6, and the rest bent is arc-shaped. The second pipe body 2 is bent at right angles at the two ends closest to each other, and the rest of the second pipe body is bent into an arc shape. The total length of the first pipe body 1 and the second pipe body 2 is 100m.
As shown in fig. 2, the section of the coiled pipe is circular, and the coiled pipe is composed of an inner pipe 14 and an outer pipe 15 which are concentrically arranged, a cavity 16 is formed between the inner pipe 14 and the outer pipe 15, and the outer surfaces of the inner pipe 14 and the outer pipe 15 are connected in a sealing manner. The inner diameter of the inner tube 14 is 0.01m.
The pipe walls of the outer pipes 15 of the first pipe body 1 and the second pipe body 2 are respectively provided with a heat conducting medium inlet 7 and a heat conducting medium outlet 8, the heat conducting medium inlets 7 are respectively arranged at one end of the first pipe body 1 connected with the pipeline mixer 6 and one end of the second pipe body 2 connected with the quenching kettle 3, and the heat conducting medium outlets 8 are respectively arranged at one end of the first pipe body 1 connected with the first metering pump 4 and one end of the second pipe body 2 connected with the pipeline mixer 6. The first pipe body 1 is provided with a temperature detector 9, and the second pipe body 2 is provided with three temperature detectors 9. The heat conducting medium flows reversely relative to the materials, so that the heat transfer effect is enhanced. The temperature detector 9 is used for monitoring the temperature in the first pipe body 1 and the second pipe body 2, so that the heat conducting medium is convenient to adjust the reaction temperature, and side reactions are prevented.
The quenching kettle 3 is made of enamel, and a rotary stirrer 11, a hydrochloric acid feeding pipe 12 and an ultrapure water feeding pipe 13 are arranged at the top of the quenching kettle. Hydrochloric acid and ultrapure water can be introduced into the quenching vessel 3 as quenching substances through the hydrochloric acid feed pipe 12 and the ultrapure water feed pipe 13 to quench the reaction.
Example 2
A tubular reactor suitable for producing p-chlorophenylboronic acid comprising: a first pipe body 1, a second pipe body 2, a quenching kettle 3, a first metering pump 4, a second metering pump 5 and a pipeline mixer 6. One end of the first pipe body 1 is connected with the first metering pump 4, and the other end of the first pipe body is connected with the pipeline mixer 6; one end of the second pipe body 2 is connected with the pipeline mixer 6, and the other end is connected with the quenching kettle 3 and is provided with a valve 10; the second metering pump 5 is connected to the pipe mixer 6. The first metering pump 4 and the second metering pump 5 can be respectively used for pumping boric acid ester and format reagent according to production requirements.
The first pipe body 1 and the second pipe body 2 are stainless steel coiled pipes and are bent into circular arc shapes. The total length of the first pipe body 1 and the second pipe body 2 is 50m.
The section of the coiled pipe is circular, the coiled pipe consists of an inner pipe 14 and an outer pipe 15 which are concentrically arranged, a cavity 16 is formed between the inner pipe 14 and the outer pipe 15, and the outer surfaces of the inner pipe 14 and the outer pipe 15 are connected in a sealing mode. The inner diameter of the inner tube 14 is 0.01m.
The pipe walls of the outer pipes 15 of the first pipe body 1 and the second pipe body 2 are respectively provided with a heat conducting medium inlet 7 and a heat conducting medium outlet 8, the heat conducting medium inlets 7 are respectively arranged at one end of the first pipe body 1 connected with the pipeline mixer 6 and one end of the second pipe body 2 connected with the quenching kettle 3, and the heat conducting medium outlets 8 are respectively arranged at one end of the first pipe body 1 connected with the first metering pump 4 and one end of the second pipe body 2 connected with the pipeline mixer 6. The first pipe body 1 is provided with two temperature detectors 9, and the second pipe body 2 is provided with three temperature detectors 9. The heat conducting medium flows reversely relative to the materials, so that the heat transfer effect is enhanced. The temperature detector 9 is used for monitoring the temperature in the first pipe body 1 and the second pipe body 2, so that the heat conducting medium is convenient to adjust the reaction temperature, and side reactions are prevented.
The quenching kettle 3 is made of enamel, and a rotary stirrer 11, a hydrochloric acid feeding pipe 12 and an ultrapure water feeding pipe 13 are arranged at the top of the quenching kettle. Hydrochloric acid and ultrapure water can be introduced into the quenching vessel 3 as quenching substances through the hydrochloric acid feed pipe 12 and the ultrapure water feed pipe 13 to quench the reaction.
Example 3
A tubular reactor suitable for producing p-chlorophenylboronic acid comprising: a first pipe body 1, a second pipe body 2, a quenching kettle 3, a first metering pump 4, a second metering pump 5 and a pipeline mixer 6. One end of the first pipe body 1 is connected with the first metering pump 4, and the other end of the first pipe body is connected with the pipeline mixer 6; one end of the second pipe body 2 is connected with the pipeline mixer 6, and the other end is connected with the quenching kettle 3; the second metering pump 5 is connected to the pipe mixer 6. The first metering pump 4 and the second metering pump 5 can be respectively used for pumping boric acid ester and format reagent according to production requirements.
The first pipe body 1 and the second pipe body 2 are stainless steel coiled pipes and are bent into a right angle shape. The total length of the first pipe body 1 and the second pipe body 2 is 100m.
The section of the coiled pipe is circular, the coiled pipe consists of an inner pipe 14 and an outer pipe 15 which are concentrically arranged, a cavity 16 is formed between the inner pipe 14 and the outer pipe 15, and the outer surfaces of the inner pipe 14 and the outer pipe 15 are connected in a sealing mode. The inner diameter of the inner tube 14 is 0.01m.
The pipe walls of the outer pipes 15 of the first pipe body 1 and the second pipe body 2 are respectively provided with a heat conducting medium inlet 7 and a heat conducting medium outlet 8, the heat conducting medium inlets 7 are respectively arranged at one end of the first pipe body 1 connected with the pipeline mixer 6 and one end of the second pipe body 2 connected with the quenching kettle 3, and the heat conducting medium outlets 8 are respectively arranged at one end of the first pipe body 1 connected with the first metering pump 4 and one end of the second pipe body 2 connected with the pipeline mixer 6. The first pipe body 1 is provided with three temperature detectors 9, and the second pipe body 2 is provided with three temperature detectors 9. The heat conducting medium flows reversely relative to the materials, so that the heat transfer effect is enhanced. The temperature detector 9 is used for monitoring the temperature in the first pipe body 1 and the second pipe body 2, so that the heat conducting medium is convenient to adjust the reaction temperature, and side reactions are prevented.
The quenching kettle 3 is made of enamel, and a rotary stirrer 11, a hydrochloric acid feeding pipe 12 and an ultrapure water feeding pipe 13 are arranged at the top of the quenching kettle. Hydrochloric acid and ultrapure water can be introduced into the quenching vessel 3 as quenching substances through the hydrochloric acid feed pipe 12 and the ultrapure water feed pipe 13 to quench the reaction.
Example 4
A tubular reactor suitable for producing p-chlorophenylboronic acid comprising: a first pipe body 1, a second pipe body 2, a quenching kettle 3, a first metering pump 4, a second metering pump 5 and a pipeline mixer 6. One end of the first pipe body 1 is connected with the first metering pump 4, and the other end of the first pipe body is connected with the pipeline mixer 6; one end of the second pipe body 2 is connected with the pipeline mixer 6, and the other end is connected with the quenching kettle 3; the second metering pump 5 is connected to the pipe mixer 6. The first metering pump 4 and the second metering pump 5 can be respectively used for pumping boric acid ester and format reagent according to production requirements.
The first pipe body 1 and the second pipe body 2 are stainless steel coiled pipes and are bent into a right angle shape. The total length of the first pipe body 1 and the second pipe body 2 is 100m.
The section of the coiled pipe is circular, the coiled pipe consists of an inner pipe 14 and an outer pipe 15 which are concentrically arranged, a cavity 16 is formed between the inner pipe 14 and the outer pipe 15, and the outer surfaces of the inner pipe 14 and the outer pipe 15 are connected in a sealing mode. The inner diameter of the inner tube 14 is 0.1m.
The pipe walls of the outer pipes 15 of the first pipe body 1 and the second pipe body 2 are respectively provided with a heat conducting medium inlet 7 and a heat conducting medium outlet 8, the heat conducting medium inlets 7 are respectively arranged at one end of the first pipe body 1 connected with the pipeline mixer 6 and one end of the second pipe body 2 connected with the quenching kettle 3, and the heat conducting medium outlets 8 are respectively arranged at one end of the first pipe body 1 connected with the first metering pump 4 and one end of the second pipe body 2 connected with the pipeline mixer 6. The first pipe body 1 is provided with three temperature detectors 9, and the second pipe body 2 is provided with three temperature detectors 9. The heat conducting medium flows reversely relative to the materials, so that the heat transfer effect is enhanced. The temperature detector 9 is used for monitoring the temperature in the first pipe body 1 and the second pipe body 2, so that the heat conducting medium is convenient to adjust the reaction temperature, and side reactions are prevented.
The quenching kettle 3 is made of enamel, and a rotary stirrer 11, a hydrochloric acid feeding pipe 12 and an ultrapure water feeding pipe 13 are arranged at the top of the quenching kettle. Hydrochloric acid and ultrapure water can be introduced into the quenching vessel 3 as quenching substances through the hydrochloric acid feed pipe 12 and the ultrapure water feed pipe 13 to quench the reaction.
Example 5
A tubular reactor suitable for producing p-chlorophenylboronic acid comprising: a first pipe body 1, a second pipe body 2, a quenching kettle 3, a first metering pump 4, a second metering pump 5 and a pipeline mixer 6. One end of the first pipe body 1 is connected with the first metering pump 4, and the other end of the first pipe body is connected with the pipeline mixer 6; one end of the second pipe body 2 is connected with the pipeline mixer 6, and the other end is connected with the quenching kettle 3; the second metering pump 5 is connected to the pipe mixer 6. The first metering pump 4 and the second metering pump 5 can be respectively used for pumping boric acid ester and format reagent according to production requirements.
The first pipe body 1 and the second pipe body 2 are stainless steel coiled pipes and are bent into circular arc shapes. The total length of the first pipe body 1 and the second pipe body 2 is 50m.
The section of the coiled pipe is circular, the coiled pipe consists of an inner pipe 14 and an outer pipe 15 which are concentrically arranged, a cavity 16 is formed between the inner pipe 14 and the outer pipe 15, and the outer surfaces of the inner pipe 14 and the outer pipe 15 are connected in a sealing mode. The inner diameter of the inner tube 14 is 0.1m.
The pipe walls of the outer pipes 15 of the first pipe body 1 and the second pipe body 2 are respectively provided with a heat conducting medium inlet 7 and a heat conducting medium outlet 8, the heat conducting medium inlets 7 are respectively arranged at one end of the first pipe body 1 connected with the pipeline mixer 6 and one end of the second pipe body 2 connected with the quenching kettle 3, and the heat conducting medium outlets 8 are respectively arranged at one end of the first pipe body 1 connected with the first metering pump 4 and one end of the second pipe body 2 connected with the pipeline mixer 6. The first pipe body 1 is provided with three temperature detectors 9, and the second pipe body 2 is provided with two temperature detectors 9. The heat conducting medium flows reversely relative to the materials, so that the heat transfer effect is enhanced. The temperature detector 9 is used for monitoring the temperature in the first pipe body 1 and the second pipe body 2, so that the heat conducting medium is convenient to adjust the reaction temperature, and side reactions are prevented.
The quenching kettle 3 is made of enamel, and a rotary stirrer 11, a hydrochloric acid feeding pipe 12 and an ultrapure water feeding pipe 13 are arranged at the top of the quenching kettle. Hydrochloric acid and ultrapure water can be introduced into the quenching vessel 3 as quenching substances through the hydrochloric acid feed pipe 12 and the ultrapure water feed pipe 13 to quench the reaction.
The above description is only of the preferred embodiments of the present utility model and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.

Claims (10)

1. A tubular reactor suitable for use in the production of p-chlorophenylboronic acid comprising: the quenching device comprises a first pipe body (1), a second pipe body (2), a quenching kettle (3), a first metering pump (4), a second metering pump (5) and a pipeline mixer (6);
the heat-conducting pipe comprises a first pipe body (1) and a second pipe body (2), wherein the first pipe body and the second pipe body (2) are coiled pipes, each coiled pipe consists of an inner pipe (14) and an outer pipe (15) which are concentrically arranged, a cavity (16) is formed between the inner pipe (14) and the outer pipe (15), the inner pipe (14) is connected with the outer surface of the outer pipe (15) in a sealing way, the pipe walls of the outer pipes (15) of the first pipe body (1) and the second pipe body (2) are respectively provided with a heat-conducting medium inlet (7) and a heat-conducting medium outlet (8), and a temperature detector (9) is arranged on the first pipe body (1) and the second pipe body (2);
one end of the first pipe body (1) is connected with the first metering pump (4), and the other end of the first pipe body is connected with the pipeline mixer (6); one end of the second pipe body (2) is connected with the pipeline mixer (6), and the other end of the second pipe body is connected with the quenching kettle (3); the second metering pump (5) is connected with the pipeline mixer (6).
2. A tubular reactor as claimed in claim 1 wherein the serpentine tube is curved or square in shape at the bend.
3. A tubular reactor as claimed in claim 1 wherein the serpentine tube is circular in cross-section.
4. A tubular reactor according to claim 1, characterized in that the heat transfer medium inlet (7) is provided at the end of the first pipe body (1) connected to the pipe mixer (6) and at the end of the second pipe body (2) connected to the quenching vessel (3), respectively.
5. A tubular reactor according to claim 1, characterized in that the heat-conducting medium outlet (8) is provided at the end of the first pipe body (1) connected to the first metering pump (4) and at the end of the second pipe body (2) connected to the pipe mixer (6), respectively.
6. A tubular reactor according to claim 1, wherein the coiled tube is made of stainless steel, and the inner diameter of the inner tube (14) is 0.01-0.1m.
7. A tubular reactor according to claim 1, characterized in that the total length of the first tube body (1) and the second tube body (2) is 50-100m.
8. A tubular reactor according to claim 1, characterized in that the top of the quench tank (3) is provided with a rotary stirrer (11), a hydrochloric acid feed pipe (12) and an ultrapure water feed pipe (13).
9. A tubular reactor according to claim 1, characterized in that the quenching vessel (3) is enamel.
10. A tubular reactor according to claim 1, characterized in that the end of the second pipe body (2) connected to the quenching vessel (3) is provided with a valve (10).
CN202321387334.XU 2023-05-31 2023-05-31 Tubular reactor suitable for producing p-chlorophenylboronic acid Active CN219984674U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202321387334.XU CN219984674U (en) 2023-05-31 2023-05-31 Tubular reactor suitable for producing p-chlorophenylboronic acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321387334.XU CN219984674U (en) 2023-05-31 2023-05-31 Tubular reactor suitable for producing p-chlorophenylboronic acid

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CN219984674U true CN219984674U (en) 2023-11-10

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