CN213708197U - P-chlorophenylhydrazine hydrochloride reaction system - Google Patents

P-chlorophenylhydrazine hydrochloride reaction system Download PDF

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CN213708197U
CN213708197U CN202022586983.5U CN202022586983U CN213708197U CN 213708197 U CN213708197 U CN 213708197U CN 202022586983 U CN202022586983 U CN 202022586983U CN 213708197 U CN213708197 U CN 213708197U
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reaction
reduction
reduction reaction
liquid inlet
continuous flow
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马兵
穆文波
王函
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Shanghai Hybrid Chem Technologies Co ltd
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Shanghai Hybrid Chem Technologies Co ltd
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Abstract

The utility model discloses a p-chlorophenylhydrazine hydrochloride reaction system, which comprises a diazonium salt intermediate liquid inlet pipeline, a reducing agent liquid inlet pipeline, a hydrochloric acid liquid inlet pipeline, a reduction reaction area, a hydrolysis reaction area and a product liquid outlet; a diazonium salt intermediate liquid inlet pipeline and a reducing agent liquid inlet pipeline are respectively connected with the reduction reaction zone; the hydrochloric acid liquid inlet pipeline is connected with the hydrolysis reaction area; the product liquid outlet is connected with the hydrolysis reaction zone; the reduction reaction zone comprises n reduction reaction units, 2 continuous flow reactors, a plate heat exchanger and a reduction intermediate liquid storage tank which are connected in sequence; the hydrolysis reaction zone comprises 1 hydrolysis reaction kettle and 4 continuous flow reactors. The reaction system of the p-chlorophenylhydrazine hydrochloride in the utility model has short reaction time, can reduce energy consumption, save cost, and has no problems of wastewater treatment, environmental pollution and the like; the operation is simple, the stability is high, and the yield is high; high selectivity, less side reaction, no other impurity in the coarse product and high yield.

Description

P-chlorophenylhydrazine hydrochloride reaction system
Technical Field
The utility model relates to a p-chlorophenylhydrazine hydrochloride reaction system.
Background
The p-chlorophenylhydrazine hydrochloride is an important intermediate of medicines and pesticides, and the synthetic route mainly takes p-chlorophenylhydrazine, a diazotization reagent, a reducing agent and hydrochloric acid as raw materials to prepare the p-chlorophenylhydrazine hydrochloride through three steps of reactions of diazotization, reduction and hydrolysis.
In the prior art, the synthesis route mainly adopts an intermittent process, after raw materials are added into a reactor, the reaction time, the cooling time, the heating time, the heat preservation time, the interval time of each operation and the like of each step need to be waited, after the reaction meets the requirement, the product is discharged at one time, the production mode of intermittent process products is divided into batches, and the quantity of the products produced in each batch is limited by the volume of the reactor. In addition, in the operation process of the batch process, the state parameters of the composition, the temperature and the like of materials such as intermediate products, final products and the like in the reactor can change along with time, so that the batch process is an unstable process. Therefore, both the production process and the product quality have large uncertainty and are difficult to control.
CN106316879A discloses a method for preparing phenylhydrazine hydrochloride by a continuous reaction kettle type operation method, which can be used in industrial production, wherein the diazotization stage is a continuous operation, and partially solves the safety risk faced by the diazotization reaction, but the reduction reaction stage and the acidolysis reaction stage still use reaction kettles, the two reactions are still batch processes, and the whole process flow for synthesizing phenylhydrazine hydrochloride is still a batch process in essence. The two reactions of reduction and acidolysis take several hours in total, resulting in a long total reaction time in the process; furthermore, after the acid precipitation, purification steps such as neutralization and distillation are required. Therefore, the process is still a batch reaction process in essence, and the problems of long reaction time, low production efficiency, low product purity, high production energy consumption and high cost of the batch process cannot be fundamentally solved.
Therefore, it is highly desirable to provide a reaction system for p-chlorophenylhydrazine hydrochloride.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to have reaction time long in order to overcome among the prior art parachlorophenylhydrazine hydrochloride reaction system, and production efficiency is low, and the result purity is low, and the production energy consumption is big, and is with high costs, and has increased the industrialization degree of difficulty, can't realize defects such as extensive continuous production, provides a parachlorophenylhydrazine hydrochloride reaction system.
The utility model discloses an above-mentioned technical problem is solved through following technical scheme:
the utility model provides a p-chlorophenylhydrazine hydrochloride reaction system, which comprises a diazonium salt intermediate liquid inlet pipeline, a reducing agent liquid inlet pipeline, a hydrochloric acid liquid inlet pipeline, a reduction reaction area, a hydrolysis reaction area and a product liquid outlet;
the diazonium salt intermediate liquid inlet pipeline and the reducing agent liquid inlet pipeline are respectively connected with the reduction reaction zone; the hydrochloric acid liquid inlet pipeline is connected with the hydrolysis reaction area; the product liquid outlet is connected with the hydrolysis reaction zone;
the reduction reaction zone comprises n reduction reaction units, 2 continuous flow reactors, a plate heat exchanger and a reduction intermediate liquid storage tank which are connected in sequence;
each of the n reduction reaction units comprises 1 reduction reaction kettle and 2 continuous flow reactors which are sequentially connected in series;
wherein n is more than or equal to 3;
the hydrolysis reaction zone comprises 1 hydrolysis reaction kettle and 4 continuous flow reactors;
wherein, the reduction intermediate liquid storage tank is connected with the hydrolysis reaction kettle and the 4 continuous flow reactors in series.
In the utility model, the reduction reaction can be carried out in the reduction reaction zone. The reduction reaction can be a reduction reaction in a p-chlorophenylhydrazine hydrochloride synthesis process which is conventional in the field. Preferably, the reduction reaction is carried out in the n reduction reaction units and the 2 continuous flow reactors.
In the reduction reaction zone, n reduction reaction kettles in the n reduction reaction units are respectively provided with a diazonium salt intermediate liquid inlet. Preferably, the diazonium salt intermediate liquid inlet pipeline comprises n diazonium salt intermediate liquid inlet pipelines connected in parallel and respectively used for inputting diazonium salt intermediate solutions into the n reduction reaction kettles.
The first reduction reaction kettle in the first reduction reaction unit can be also provided with a reducing agent liquid inlet for inputting a reducing agent into the first reduction reaction kettle; and a first reaction liquid outlet for inputting the reaction liquid into the first continuous flow reactor in the first reduction reaction unit.
Preferably, the second continuous flow reactor in the first reduction reaction unit is connected with the second reduction reaction kettle in the second reduction reaction unit through the first reduction reaction liquid inlet.
Preferably, the nth reduction reaction unit is connected with the 2 continuous flow reactors through a reduction reaction liquid outlet.
The 2 continuous flow reactors are preferably connected with the plate heat exchanger and the reduction intermediate liquid storage tank in sequence through a reduction intermediate solution inlet.
Wherein, the reduction intermediate liquid storage tank is provided with a liquid storage inlet and a liquid storage outlet. The liquid storage inlet can be connected with the plate heat exchanger. The liquid storage outlet can be connected with the hydrolysis reaction kettle.
The utility model discloses in, the hydrolysis reaction district can carry out the hydrolysis reaction. The hydrolysis reaction can be a hydrolysis reaction in a p-chlorophenylhydrazine hydrochloride synthesis process which is conventional in the field. Preferably, the hydrolysis reaction is carried out in the 1 hydrolysis reaction kettle and the 4 continuous flow reactors.
In the hydrolysis reaction zone, a reducing intermediate liquid inlet can be formed in the hydrolysis reaction kettle and is used for being connected with a liquid storage outlet in the reducing intermediate liquid storage tank and inputting a reducing intermediate solution into the hydrolysis reaction kettle; a hydrochloric acid liquid inlet for inputting a hydrochloric acid solution into the hydrolysis reaction kettle; and a hydrolysis reaction liquid outlet for inputting hydrolysis reaction liquid into the first continuous flow reactor in the 4 continuous flow reactors.
And a product liquid outlet can be arranged on the fourth continuous flow reactor in the 4 continuous flow reactors and is used for outputting the p-chlorophenylhydrazine hydrochloride.
In the present invention, the continuous flow reactor may be any one or more reactors capable of realizing continuous flow reaction, such as one or more of a micro-reactor, a tubular reactor, a cascade mixer and a static mixer; preferably a microreactor.
The utility model discloses in, p chlorobenzene hydrazine hydrochloride reaction system still can include thick liquids delivery pump and diaphragm metering pump.
Preferably, the diazonium salt intermediate liquid inlet pipeline, the reducing agent liquid inlet pipeline and the hydrochloric acid liquid inlet pipeline are sequentially provided with the slurry conveying pump and the diaphragm metering pump. The diaphragm metering pump can be two diaphragm metering pumps which are arranged in parallel. When one of the diaphragm metering pumps fails, the other diaphragm metering pump may be used.
The utility model discloses in, p chlorobenzene hydrazine hydrochloride reaction system still can include conduction oil heating device. The heat-conducting oil heating device can be respectively connected with the reduction reaction area and the hydrolysis reaction area through a heat-conducting oil liquid inlet pipeline and a heat-conducting oil liquid outlet pipeline and is used for heating the n reduction reaction kettles and the hydrolysis reaction kettle through heat-conducting oil. Wherein the heat transfer oil can be recycled.
The utility model discloses in, the application method of p chlorobenzene hydrochloride reaction system includes following step: respectively inputting the heat conduction oil into the reduction reaction zone and the hydrolysis reaction zone through the heat conduction oil liquid inlet pipeline, and continuously inputting a diazonium salt intermediate solution and a reducing agent into the reduction reaction zone through the diazonium salt intermediate liquid inlet pipeline and the reducing agent liquid inlet pipeline respectively to perform reduction reaction so as to obtain a reduction intermediate solution; and continuously inputting a hydrochloric acid solution into the hydrolysis reaction zone through the hydrochloric acid liquid inlet pipeline for hydrolysis reaction to obtain the p-chlorophenylhydrazine hydrochloride.
Preferably, a diazonium salt intermediate solution and a reducing agent are continuously input into the first reduction reaction unit through a diazonium salt intermediate liquid inlet pipeline and a reducing agent liquid inlet pipeline respectively for reaction, after the reaction is finished, the first reduction reaction solution enters the second reduction reaction unit to the nth reduction reaction unit which are sequentially connected in series for reaction, after the reaction is finished, the nth reduction reaction solution enters the 2 continuous flow reactors which are sequentially connected in series for reaction, after the reaction is finished, the reduction intermediate solution enters the plate heat exchanger, then enters the reduction intermediate liquid storage tank, and is input into the hydrolysis reaction kettle through the liquid storage outlet; and continuously inputting a hydrochloric acid solution into the hydrolysis reaction kettle through the hydrochloric acid liquid inlet pipeline, and performing hydrolysis reaction on the hydrochloric acid solution and the reduction intermediate solution to obtain p-chlorophenylhydrazine hydrochloride, and outputting the p-chlorophenylhydrazine hydrochloride through a product liquid outlet.
In the present invention, the reducing agent may be a reducing agent conventional in the art, such as a sodium sulfite solution.
On the basis of the common knowledge in the field, the above preferred conditions can be combined at will to obtain the preferred embodiments of the present invention.
The reagent and the raw material used in the utility model are available on the market.
The utility model discloses an actively advance the effect and lie in:
(1) the utility model discloses a p chlorobenzene hydrazine hydrochloride reaction system has overcome intermittent type formula technology reaction time long, and the productivity is not high, and the industrialization degree of difficulty is big, can't realize the defect of extensive continuous production, can even running, and reaction time shortens greatly, reduces the energy consumption, practices thrift the cost, and does not have waste water treatment and environmental pollution scheduling problem.
(2) The utility model discloses well p-chlorophenylhydrazine hydrochloride reaction system's operating procedure is few, simple process, and stability is high.
(3) The utility model discloses a p chlorobenzene hydrazine hydrochloride reaction system conversion rate is high, and selectivity is high, and the side reaction is few, and the coarse product does not have other impurity, and the yield is high, and the aftertreatment is simple, easily separates.
Drawings
FIG. 1 is a schematic diagram of a reaction system for p-chlorophenylhydrazine hydrochloride in example 1.
Description of the reference numerals
Diazonium salt intermediate liquid inlet pipeline 1
First diazonium salt intermediate liquid inlet pipeline 11
Second diazonium salt intermediate liquid inlet pipeline 12
Third diazonium salt intermediate liquid inlet pipeline 13
First diazonium salt intermediate inlet 111
Second diazonium salt intermediate liquid inlet 121
Third diazonium salt intermediate liquid inlet 131
Reducing agent inlet pipe 2
Liquid inlet 21 for reducing agent
Hydrochloric acid inlet pipe 3
Hydrochloric acid inlet 31
Reduction reaction zone 4
First reduction reaction vessel 41
First continuous flow reactor 411
Second continuous flow reactor 412
First reaction liquid outlet 413
Second reduction reaction vessel 42
Third continuous flow reactor 421
Fourth continuous flow reactor 422
First reduction reaction liquid inlet 423
Third reduction reaction kettle 43
Fifth continuous flow reactor 431
Sixth continuous flow reactor 432
Seventh continuous flow reactor 46
Eighth continuous flow reactor 47
Second reduction reaction liquid inlet 435
Reduction reaction liquid outlet 437
Reducing intermediate solution inlet 471
Plate heat exchanger 44
Reducing intermediate liquid storage tank 45
Liquid storage inlet 451
Reservoir outlet 452
Hydrolysis reaction zone 5
Hydrolysis reaction kettle 51
Ninth continuous flow reactor 511
Tenth continuous flow reactor 512
Eleventh continuous flow reactor 513
Twelfth continuous flow reactor 514
Reduction intermediate liquid inlet 515
Hydrolysis reaction liquid outlet 516
Product outlet 6
Detailed Description
The present invention is further illustrated by way of the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1
The reaction system of p-chlorophenylhydrazine hydrochloride in embodiment 1 comprises a diazonium salt intermediate liquid inlet pipeline 1, a reducing agent liquid inlet pipeline 2, a hydrochloric acid liquid inlet pipeline 3, a reduction reaction zone 4, a hydrolysis reaction zone 5 and a product liquid outlet 6.
A diazonium salt intermediate liquid inlet pipeline 1 and a reducing agent liquid inlet pipeline 2 are respectively connected with a reduction reaction zone 4; the hydrochloric acid liquid inlet pipeline 3 is connected with the hydrolysis reaction area 5; the product liquid outlet 6 is connected with the hydrolysis reaction zone 5.
The reduction reaction zone 4 comprises 3 reduction reaction units, 2 continuous flow reactors, a plate heat exchanger 44 and a reduction intermediate storage tank 45.
Each reduction reaction unit comprises 1 reduction reaction kettle and 2 continuous flow reactors which are connected in series in sequence.
The hydrolysis reaction zone 5 comprises a hydrolysis reaction kettle 51 and 4 continuous flow reactors;
wherein the reducing intermediate storage tank 45 is connected in series with the hydrolysis reaction kettle 51, the ninth continuous flow reactor 511, the tenth continuous flow reactor 512, the eleventh continuous flow reactor 513 and the twelfth continuous flow reactor 514 in sequence.
In the reaction system of p-chlorophenylhydrazine hydrochloride of example 1, the reduction reaction is a reduction reaction in the synthesis process of p-chlorophenylhydrazine hydrochloride which is conventional in the art. The reduction reaction is carried out in a reduction reaction zone 4, preferably in 3 reduction reaction units and 2 continuous flow reactors.
In the reduction reaction zone 4, a first diazonium salt intermediate liquid inlet 111 is arranged on a first reduction reaction kettle 41 in a first reduction reaction unit; a second diazonium salt intermediate liquid inlet 121 is formed in a second reduction reaction kettle 42 in the second reduction reaction unit; a third reducing reaction kettle 43 in the third reducing reaction unit is provided with a third diazonium salt intermediate liquid inlet 131.
The diazonium salt intermediate liquid inlet pipeline 1 comprises 3 first diazonium salt intermediate liquid inlet pipelines 11, second diazonium salt intermediate liquid inlet pipelines 12 and third diazonium salt intermediate liquid inlet pipelines 13 which are connected in parallel and are respectively used for inputting diazonium salt intermediate solutions into 3 reduction reaction kettles.
A reducing agent liquid inlet 21 is arranged on a first reduction reaction kettle 41 in the first reduction reaction unit and is used for inputting a reducing agent into the first reduction reaction kettle 41; and a first reaction liquid outlet 413 for inputting a reaction liquid into the first continuous flow reactor 411.
The second continuous flow reactor 412 in the first reduction reaction unit is connected to the second reduction reaction tank 42 in the second reduction reaction unit through the first reduction reaction liquid inlet 423.
The fourth continuous flow reactor 422 in the second reduction reaction unit is connected with the third reduction reaction kettle 43 in the third reduction reaction unit through a second reduction reaction liquid inlet 435.
The sixth continuous flow reactor 432 in the third reduction reaction unit is connected to the seventh continuous flow reactor 46 and the eighth continuous flow reactor 47 in series in this order through a reduction reaction liquid outlet 437.
The eighth continuous flow reactor 47 is provided with a reducing intermediate solution inlet 471. The eighth continuous flow reactor 47 is connected in sequence to the plate heat exchanger 44 and the reducing intermediate reservoir tank 45 through a reducing intermediate solution inlet 471.
The reducing intermediate storage tank 45 is provided with a storage inlet 451 and a storage outlet 452. The reservoir inlet 451 is connected to the plate heat exchanger 44. The outlet 452 of the liquid storage is connected to the hydrolysis reactor 51.
In the reaction system of p-chlorophenylhydrazine hydrochloride of example 1, the hydrolysis reaction is a hydrolysis reaction in a synthesis process of p-chlorophenylhydrazine hydrochloride which is conventional in the art. The hydrolysis reaction is carried out in the hydrolysis reaction zone 5. Preferably in hydrolysis reactor 51 and 4 continuous flow reactors.
In the hydrolysis reaction zone 5, a reducing intermediate liquid inlet 515 is arranged on the hydrolysis reaction kettle 51 and is used for connecting with a liquid storage outlet 452 on the reducing intermediate liquid storage tank 45 and inputting a reducing intermediate solution into the hydrolysis reaction kettle 51; a hydrochloric acid inlet 31 for inputting a hydrochloric acid solution into the hydrolysis reaction kettle 51; and a hydrolysis reaction liquid outlet 516 for inputting hydrolysis reaction liquid into the ninth continuous flow reactor 511.
A product liquid outlet 6 is arranged on the twelfth continuous flow reactor 514 and is used for outputting the p-chlorophenylhydrazine hydrochloride.
The continuous flow reactor in example 1 is a microreactor.
The p-chlorophenylhydrazine hydrochloride reaction system of example 1 further comprises a slurry transfer pump and a diaphragm metering pump. In order to more clearly show the p-chlorophenylhydrazine hydrochloride reaction system, the delivery pump and the diaphragm metering pump are not shown in FIG. 1.
A slurry delivery pump and a diaphragm metering pump are sequentially arranged on the diazonium salt intermediate liquid inlet pipeline 1, the reducing agent liquid inlet pipeline 2 and the hydrochloric acid liquid inlet pipeline 3. Wherein, the diaphragm metering pump is two diaphragm metering pumps that are connected in parallel. When one of the diaphragm metering pumps fails, the other diaphragm metering pump may be used.
The p-chlorophenylhydrazine hydrochloride reaction system of embodiment 1 further comprises a heat transfer oil heating device. In order to more clearly show the reaction system of p-chlorophenylhydrazine hydrochloride, a heat conducting oil heating device is not shown in fig. 1.
The heat-conducting oil heating device is respectively connected with the reduction reaction zone 4 and the hydrolysis reaction zone 5 through a heat-conducting oil liquid inlet pipeline and a heat-conducting oil liquid outlet pipeline, and is used for heating the first reduction reaction kettle 41, the second reduction reaction kettle 42, the third reduction reaction kettle 43 and the hydrolysis reaction kettle 51 through heat-conducting oil. Wherein, the heat conducting oil can be recycled.
The method for using the reaction system of p-chlorophenylhydrazine hydrochloride in the example 1 comprises the following steps: respectively inputting heat conducting oil into a reduction reaction zone 4 and a hydrolysis reaction zone 5 through a heat conducting oil liquid inlet pipeline, and continuously inputting a diazonium salt intermediate solution and a reducing agent into the reduction reaction zone 4 through a diazonium salt intermediate liquid inlet pipeline 1 and a reducing agent liquid inlet pipeline 2 to carry out reduction reaction to obtain a reduction intermediate solution; and continuously inputting the hydrochloric acid solution into a hydrolysis reaction zone 5 through a hydrochloric acid liquid inlet pipeline 3 for hydrolysis reaction to obtain the p-chlorophenylhydrazine hydrochloride.
Specifically, a diazonium salt intermediate solution and a reducing agent are continuously input into the first reduction reaction kettle 41 through a diazonium salt intermediate liquid inlet pipeline 1 and a reducing agent liquid inlet pipeline 2 respectively for reaction, and after the reaction is completed, the reaction solution enters the first continuous flow reactor 411 and the second continuous flow reactor 412 which are connected in series in sequence for continuous reaction; after the reaction is finished, the reaction solution enters a second reduction reaction kettle 42 for reaction, and after the reaction is finished, the reaction solution enters a third continuous flow reactor 421 and a fourth continuous flow reactor 422 which are connected in series in sequence for continuous reaction; after the reaction, the reaction solution enters the third reduction reaction kettle 43 for reaction, after the reaction is completed, the reaction solution enters the fifth continuous flow reactor 431 and the sixth continuous flow reactor 432 which are connected in series in sequence, and after the reaction is completed, the reaction solution enters the seventh continuous flow reactor 46 and the eighth continuous flow reactor 47 which are connected in series in sequence for continuous reaction; the reducing intermediate solution enters the plate heat exchanger 44 through the reducing intermediate solution inlet 471, then enters the reducing intermediate liquid storage tank 45, and is input into the hydrolysis reaction kettle 51 through the liquid storage outlet 452; and continuously inputting the hydrochloric acid solution into the hydrolysis reaction kettle 51 through a hydrochloric acid liquid inlet pipeline 3, and performing hydrolysis reaction on the hydrochloric acid solution and the reduction intermediate solution to obtain the p-chlorophenylhydrazine hydrochloride, and outputting the p-chlorophenylhydrazine hydrochloride through a product liquid outlet 6. Wherein the reducing agent is sodium sulfite solution.
The p-chlorophenylhydrazine hydrochloride reaction system in the embodiment 1 overcomes the defects of long reaction time, low yield, high industrialization difficulty and incapability of realizing large-scale continuous production of an intermittent process, can stably run, greatly shortens the reaction time, reduces the energy consumption, saves the cost, and has no problems of wastewater treatment, environmental pollution and the like. In addition, the reaction system of p-chlorophenylhydrazine hydrochloride in the embodiment 1 has the advantages of few operation steps, simple process and high stability. Further, the reaction system of p-chlorophenylhydrazine hydrochloride in the embodiment 1 has the advantages of high conversion rate, high selectivity, less side reaction, no other impurities in the crude product, high yield, simple post-treatment and easy separation.

Claims (10)

1. A p-chlorophenylhydrazine hydrochloride reaction system is characterized by comprising a diazonium salt intermediate liquid inlet pipeline, a reducing agent liquid inlet pipeline, a hydrochloric acid liquid inlet pipeline, a reduction reaction zone, a hydrolysis reaction zone and a product liquid outlet;
the diazonium salt intermediate liquid inlet pipeline and the reducing agent liquid inlet pipeline are respectively connected with the reduction reaction zone; the hydrochloric acid liquid inlet pipeline is connected with the hydrolysis reaction area; the product liquid outlet is connected with the hydrolysis reaction zone;
the reduction reaction zone comprises n reduction reaction units, 2 continuous flow reactors, a plate heat exchanger and a reduction intermediate liquid storage tank which are connected in sequence;
each of the n reduction reaction units comprises 1 reduction reaction kettle and 2 continuous flow reactors which are sequentially connected in series;
wherein n is more than or equal to 3;
the hydrolysis reaction zone comprises 1 hydrolysis reaction kettle and 4 continuous flow reactors;
wherein, the reduction intermediate liquid storage tank is connected with the hydrolysis reaction kettle and the 4 continuous flow reactors in series.
2. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein the diazonium salt intermediate feed line comprises n diazonium salt intermediate feed lines connected in parallel, and the n diazonium salt intermediate feed lines are respectively used for feeding diazonium salt intermediate solutions into the n reduction reaction kettles.
3. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein in the reduction reaction zone, n reduction reaction kettles in the n reduction reaction units are respectively provided with a diazonium salt intermediate liquid inlet.
4. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein a reducing agent inlet is arranged on the first reduction reaction kettle in the first reduction reaction unit, and is used for inputting a reducing agent into the first reduction reaction kettle; and a first reaction liquid outlet for inputting a reaction liquid into the first continuous flow reactor in the first reduction reaction unit.
5. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein the second continuous flow reactor in the first reduction reaction unit is connected with the second reduction reaction kettle in the second reduction reaction unit through the first reduction reaction liquid inlet;
the nth reduction reaction unit is connected with the 2 continuous flow reactors through a reduction reaction liquid outlet;
the 2 continuous flow reactors are sequentially connected with the plate heat exchanger and the reduction intermediate liquid storage tank through a reduction intermediate solution inlet.
6. The chlorophenylhydrazine hydrochloride reaction system as claimed in claim 5, wherein the reducing intermediate storage tank is provided with a storage inlet and a storage outlet;
the liquid storage inlet is connected with the plate heat exchanger; and the liquid storage outlet is connected with the hydrolysis reaction kettle.
7. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein in the hydrolysis reaction zone, the hydrolysis reaction kettle is provided with a reducing intermediate liquid inlet for connecting with a liquid storage outlet on the reducing intermediate liquid storage tank and inputting a reducing intermediate solution into the hydrolysis reaction kettle; a hydrochloric acid liquid inlet for inputting a hydrochloric acid solution into the hydrolysis reaction kettle; and a hydrolysis reaction liquid outlet for inputting hydrolysis reaction liquid into the first continuous flow reactor of the 4 continuous flow reactors;
and a product liquid outlet is formed in the fourth continuous flow reactor of the 4 continuous flow reactors and is used for outputting the p-chlorophenylhydrazine hydrochloride.
8. The p-chlorophenylhydrazine hydrochloride reaction system according to claim 1, wherein the continuous flow reactor is one or more of a microreactor, a tubular reactor, a cascade mixer, a static mixer.
9. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein the p-chlorophenylhydrazine hydrochloride reaction system comprises a slurry delivery pump and a diaphragm metering pump;
the diazonium salt intermediate liquid inlet pipeline, the reducing agent liquid inlet pipeline and the hydrochloric acid liquid inlet pipeline are sequentially provided with the slurry conveying pump and the diaphragm metering pump;
the diaphragm metering pump is two diaphragm metering pumps which are arranged in parallel.
10. The p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein the p-chlorophenylhydrazine hydrochloride reaction system comprises a heat conducting oil heating device;
the heat-conducting oil heating device is respectively connected with the reduction reaction area and the hydrolysis reaction area through a heat-conducting oil liquid inlet pipeline and a heat-conducting oil liquid outlet pipeline and is used for heating the n reduction reaction kettles and the hydrolysis reaction kettle through heat-conducting oil.
CN202022586983.5U 2020-11-10 2020-11-10 P-chlorophenylhydrazine hydrochloride reaction system Active CN213708197U (en)

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