CN112225677B - P-chlorophenylhydrazine hydrochloride reaction system and method - Google Patents
P-chlorophenylhydrazine hydrochloride reaction system and method Download PDFInfo
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Abstract
The invention discloses a p-chlorophenylhydrazine hydrochloride reaction system and a method, wherein the p-chlorophenylhydrazine hydrochloride reaction system comprises 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 zone; 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 included 1 hydrolysis reactor and 4 continuous flow reactors. The p-chlorophenylhydrazine hydrochloride reaction system has short reaction time, can reduce energy consumption, saves 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 impurities in the crude product and high yield.
Description
Technical Field
The invention relates to a system and a method for reacting parachlorophenyl hydrazine hydrochloride.
Background
The p-chlorophenylhydrazine hydrochloride is an important intermediate of medicines and pesticides, and the synthetic route is mainly to take p-chloroaniline, diazotizing reagent, reducing agent and hydrochloric acid as raw materials, and the p-chlorophenylhydrazine hydrochloride is prepared by three steps of reactions of diazotization, reduction and hydrolysis in sequence.
In the prior art, the above synthetic route mainly adopts an intermittent process, after raw materials are added into a reactor, the time for each step of reaction, the time for cooling, the time for heating, the time for heat preservation, the time for each operation interval and the like need to be waited, and after the reaction reaches the requirement, the products are discharged at one time. In addition, during the operation of the batch process, the composition of materials such as intermediate products and final products in the reactor, the temperature and other state parameters can change with time, and the batch process is an unsteady state process. It can be seen that there is a large uncertainty in both the production process and the product quality, which is difficult to control.
CN106316879a discloses a method for preparing phenylhydrazine hydrochloride by using a continuous reaction kettle type operation mode, which can be used for industrial production, although the diazotization stage is continuously operated, and the safety risk faced by the diazotization reaction is partially solved, reaction kettles are still used in the reduction reaction stage and the acidolysis reaction stage, the two steps of reactions are still batch processes, and the whole process flow for synthesizing phenylhydrazine hydrochloride is still substantially batch reaction processes. The two steps of reduction and acidolysis require several hours in total, resulting in longer total reaction time in the process; furthermore, the acid precipitation is followed by purification steps such as neutralization and distillation. Therefore, the process is still a batch reaction process, 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.
Accordingly, there is a need to provide a system and method for reacting p-chlorophenylhydrazine hydrochloride.
Disclosure of Invention
The invention aims to overcome the defects that a p-chlorophenylhydrazine hydrochloride reaction system in the prior art has long reaction time, low production efficiency, low product purity, high production energy consumption, high cost, increased industrialization difficulty, incapability of realizing large-scale continuous production and the like.
The invention solves the technical problems by the following technical scheme:
the invention 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 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 zone; 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 n reduction reaction units comprise 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 4 continuous flow reactors in series in sequence.
In the present invention, the reduction reaction may be performed in the reduction reaction zone. The reduction reaction may be a reduction reaction in a p-chlorophenylhydrazine hydrochloride synthesis process conventional in the art. Preferably, the reduction reaction is carried out in the n reduction reaction units and the 2 continuous flow reactors.
In the reduction reaction zone, diazonium salt intermediate liquid inlets are arranged on n reduction reaction kettles in the n reduction reaction units. Preferably, the diazonium salt intermediate liquid inlet pipeline comprises n diazonium salt intermediate liquid inlet pipelines which are connected in parallel and are 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 further 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 to 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 reducing intermediate liquid storage tank in sequence through a reducing 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.
In the present invention, the hydrolysis reaction zone may be subjected to hydrolysis reaction. The hydrolysis reaction may be that in the art conventional p-chlorophenylhydrazine hydrochloride synthesis process. 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 reduction intermediate liquid inlet is arranged on the hydrolysis reaction kettle and is used for being connected with a liquid storage outlet on the reduction intermediate liquid storage tank, and a reduction intermediate solution is input into the hydrolysis reaction kettle; the hydrochloric acid liquid inlet is used for inputting hydrochloric acid solution into the hydrolysis reaction kettle; and a hydrolysis reaction liquid outlet for inputting the hydrolysis reaction liquid into the first continuous flow reactor among the 4 continuous flow reactors.
And a product outlet for outputting p-chlorophenylhydrazine hydrochloride can be arranged on the fourth continuous flow reactor in the 4 continuous flow reactors.
In the present invention, the continuous flow reactor may be any one or more reactors that can realize continuous flow reaction, such as one or more of a microreactor, a tubular reactor, a cascade mixer, and a static mixer; preferably a microreactor.
In the invention, the p-chlorophenylhydrazine hydrochloride reaction system can also comprise a slurry delivery pump and a 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. Wherein, the diaphragm metering pump can be two diaphragm metering pumps that the parallel arrangement. When one of the diaphragm metering pumps fails, the other diaphragm metering pump may be used.
In the invention, the p-chlorophenylhydrazine hydrochloride reaction system can also comprise a heat conducting oil heating device. The heat conducting oil heating device can be connected with the reduction reaction zone and the hydrolysis reaction zone respectively 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 kettles through heat conducting oil. Wherein, the heat conduction oil can be recycled.
The invention also provides a using method of the p-chlorophenylhydrazine hydrochloride reaction system, which comprises the following steps: respectively inputting the heat conducting oil into the reduction reaction zone and the hydrolysis reaction zone through the heat conducting 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 for reduction reaction to obtain a reduction intermediate solution; and continuously inputting the hydrochloric acid solution into the hydrolysis reaction zone through the hydrochloric acid liquid inlet pipeline to carry out hydrolysis reaction to obtain the p-chlorophenylhydrazine hydrochloride.
Preferably, the diazonium salt intermediate solution and the reducing agent are respectively and continuously input into the first reduction reaction unit through the diazonium salt intermediate liquid inlet pipeline and the reducing agent liquid inlet pipeline for reaction, after the reaction is finished, the first reduction reaction liquid 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 liquid enters the 2 continuous flow reactors which are sequentially connected in series for reaction, after the reaction is finished, the reducing intermediate solution enters the plate heat exchanger, then enters the reducing intermediate liquid storage tank, and is input into the hydrolysis reaction kettle through the liquid storage outlet; and continuously inputting the hydrochloric acid solution into the hydrolysis reaction kettle through the hydrochloric acid liquid inlet pipeline, 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 sodium sulfite solution.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the invention.
The reagents and materials used in the present invention are commercially available.
The invention has the positive progress effects that:
(1) The p-chlorophenylhydrazine hydrochloride reaction system overcomes the defects of long reaction time, low yield, large industrialization difficulty, incapability of realizing large-scale continuous production of an intermittent process, stable operation, greatly shortened reaction time, reduced energy consumption, cost saving, no wastewater treatment, no environmental pollution and the like.
(2) The p-chlorophenylhydrazine hydrochloride reaction system has the advantages of few operation steps, simple process and high stability.
(3) The p-chlorophenylhydrazine hydrochloride reaction system 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.
Drawings
FIG. 1 is a schematic diagram of the reaction system of p-chlorophenylhydrazine hydrochloride in example 1.
Description of the reference numerals
Diazonium salt intermediate feed liquor pipeline 1
First diazonium salt intermediate feed liquor pipe 11
Second diazonium salt intermediate liquid inlet conduit 12
Third diazonium salt intermediate liquid inlet pipe 13
First diazonium salt intermediate liquid inlet 111
Second diazonium salt intermediate liquid inlet 121
Third diazonium salt intermediate liquid inlet 131
Reducing agent liquid inlet pipeline 2
Reducing agent inlet 21
Hydrochloric acid liquid inlet pipeline 3
Hydrochloric acid inlet 31
Reduction reaction zone 4
First reduction reactor 41
First continuous flow reactor 411
Second continuous flow reactor 412
First reaction liquid outlet 413
Second reduction reactor 42
Third continuous flow reactor 421
Fourth continuous flow reactor 422
First reduction reaction liquid inlet 423
Third reduction reactor 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 solution outlet 437
Reduction intermediate solution inlet 471
Plate heat exchanger 44
Reduction intermediate liquid storage tank 45
Liquid storage inlet 451
Liquid storage outlet 452
Hydrolysis reaction zone 5
Hydrolysis reactor 51
Ninth continuous flow reactor 511
Tenth continuous flow reactor 512
Eleventh continuous flow reactor 513
Twelfth continuous flow reactor 514
Reduction intermediate feed 515
Hydrolysis reaction liquid outlet 516
Product outlet 6
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
Example 1
The p-chlorophenylhydrazine hydrochloride reaction system in example 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.
The diazonium salt intermediate liquid inlet pipeline 1 and the reducing agent liquid inlet pipeline 2 are respectively connected with the reduction reaction zone 4; the hydrochloric acid liquid inlet pipeline 3 is connected with the hydrolysis reaction zone 5; the product 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 reducing intermediate liquid reservoir 45.
Each reduction reaction unit comprises 1 reduction reaction kettle and 2 continuous flow reactors which are sequentially connected in series.
Hydrolysis reaction zone 5 comprises hydrolysis reaction kettle 51 and 4 continuous flow reactors;
wherein the reduction intermediate liquid storage tank 45 is connected in series with the hydrolysis reaction vessel 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 this order.
In the p-chlorophenylhydrazine hydrochloride reaction system of example 1, the reduction reaction was that of the conventional art p-chlorophenylhydrazine hydrochloride synthesis process. 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 arranged on a second reduction reaction kettle 42 in the second reduction reaction unit; a third diazonium salt intermediate liquid inlet 131 is provided on the third reduction reactor 43 in the third reduction reaction unit.
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 reducing agent into the first reduction reaction kettle 41; and a first reaction liquid outlet 413 for inputting the 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 to the third reduction reaction tank 43 in the third reduction reaction unit through the 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 the reduction reaction liquid outlet 437.
The eighth continuous flow reactor 47 is provided with a reduction intermediate solution inlet 471. The eighth continuous flow reactor 47 is connected in turn to the plate heat exchanger 44 and the reducing intermediate reservoir 45 via a reducing intermediate solution inlet 471.
The reducing intermediate liquid tank 45 is provided with a liquid storage inlet 451 and a liquid storage outlet 452. The liquid storage inlet 451 is connected to the plate heat exchanger 44. The liquid storage outlet 452 is connected with the hydrolysis reaction kettle 51.
In the p-chlorophenylhydrazine hydrochloride reaction system of example 1, the hydrolysis reaction was that in the art conventional p-chlorophenylhydrazine hydrochloride synthesis process. The hydrolysis reaction is carried out in hydrolysis reaction zone 5. Preferably in hydrolysis reactor 51 and 4 continuous flow reactors.
In the hydrolysis reaction zone 5, a reduction intermediate liquid inlet 515 is arranged on the hydrolysis reaction kettle 51 and is used for being connected with a liquid storage outlet 452 on the reduction intermediate liquid storage tank 45, and a reduction intermediate solution is input 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 a hydrolysis reaction liquid into the ninth continuous flow reactor 511.
A product outlet 6 is provided in the twelfth continuous flow reactor 514 for outputting p-chlorophenylhydrazine hydrochloride.
The continuous flow reactor in example 1 is a microreactor.
The p-chlorophenylhydrazine hydrochloride reaction system of example 1 also included a slurry transfer pump and a diaphragm metering pump. In order to more clearly present the p-chlorophenylhydrazine hydrochloride reaction system, the delivery pump and diaphragm metering pump are not shown in fig. 1.
And 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 the parallel arrangement. When one of the diaphragm metering pumps fails, the other diaphragm metering pump may be used.
The p-chlorophenylhydrazine hydrochloride reaction system of example 1 also includes a conduction oil heating device. In order to more clearly present the p-chlorophenylhydrazine hydrochloride reaction system, the conduction oil heating apparatus is not shown in fig. 1.
The conduction oil heating device is respectively connected with the reduction reaction zone 4 and the hydrolysis reaction zone 5 through a conduction oil liquid inlet pipeline and a conduction 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 conduction oil. Wherein, the heat conduction oil can be recycled.
The method for using the parachlorophenylhydrazine hydrochloride reaction system in the embodiment 1 comprises the following steps: the method comprises the steps of respectively inputting heat conduction oil into a reduction reaction zone 4 and a hydrolysis reaction zone 5 through heat conduction oil liquid inlet pipelines, and continuously inputting 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 respectively for reduction reaction to obtain a reduction intermediate solution; the hydrochloric acid solution is continuously input into a hydrolysis reaction zone 5 through a hydrochloric acid liquid inlet pipeline 3 for hydrolysis reaction, and p-chlorophenylhydrazine hydrochloride is obtained.
Specifically, the diazonium salt intermediate solution and the reducing agent are continuously input into a first reduction reaction kettle 41 for reaction through a diazonium salt intermediate liquid inlet pipeline 1 and a reducing agent liquid inlet pipeline 2 respectively, and after the reaction is finished, the reaction liquid enters a first continuous flow reactor 411 and a second continuous flow reactor 412 which are sequentially connected in series 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 sequentially connected in series for continuous reaction; after the reaction is finished, the reaction solution enters a third reduction reaction kettle 43 for reaction, after the reaction is finished, the reaction solution enters a fifth continuous flow reactor 431 and a sixth continuous flow reactor 432 which are sequentially connected in series, and after the reaction is finished, the reaction solution enters a seventh continuous flow reactor 46 and an eighth continuous flow reactor 47 which are sequentially connected in series 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; hydrochloric acid solution is continuously input into a hydrolysis reaction kettle 51 through a hydrochloric acid liquid inlet pipeline 3, hydrolysis reaction is carried out on the hydrochloric acid solution and the reduction intermediate solution, p-chlorophenylhydrazine hydrochloride is obtained, and the p-chlorophenylhydrazine hydrochloride is output through a product liquid outlet 6. Wherein the reducing agent is sodium sulfite solution.
The parachlorophenylhydrazine hydrochloride reaction system in the embodiment 1 overcomes the defects of long reaction time, low yield, large industrialization difficulty and incapability of realizing large-scale continuous production of a batch process, can stably operate, 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 p-chlorophenylhydrazine hydrochloride reaction system in the embodiment 1 has the advantages of few operation steps, simple process and high stability. Further, the p-chlorophenylhydrazine hydrochloride reaction system 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 (12)
1. The 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 zone; 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 n reduction reaction units comprise 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 n reduction reaction kettles in the n reduction reaction units are respectively provided with a diazonium salt intermediate liquid inlet;
a reducing agent liquid inlet is arranged on a 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 a first continuous flow reactor in the first reduction reaction unit;
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 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 4 continuous flow reactors in series in sequence.
2. The p-chlorophenylhydrazine hydrochloride reaction system of claim 1, wherein the diazonium salt intermediate liquid inlet conduit in the reduction reaction zone comprises n parallel diazonium salt intermediate liquid inlet conduits for feeding diazonium salt intermediate solutions to the n reduction reaction vessels, respectively.
3. The p-chlorophenylhydrazine hydrochloride reaction system of claim 1, wherein an nth reduction reaction unit is connected to 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 the reduction intermediate solution inlet.
4. The p-chlorophenylhydrazine hydrochloride reaction system of claim 1, wherein the reducing intermediate reservoir is provided with a reservoir inlet and a reservoir outlet; the liquid storage inlet is connected with the plate heat exchanger; the liquid storage outlet is connected with the hydrolysis reaction kettle.
5. The p-chlorophenylhydrazine hydrochloride reaction system according to claim 1, wherein in the hydrolysis reaction zone, a reducing intermediate liquid inlet is arranged on the hydrolysis reaction kettle and is used for being connected with a liquid storage outlet on the reducing intermediate liquid storage tank, and reducing intermediate solution is input into the hydrolysis reaction kettle; the hydrochloric acid liquid inlet is used for inputting hydrochloric acid solution into the hydrolysis reaction kettle; and a hydrolysis reaction liquid outlet for inputting a hydrolysis reaction liquid into a first continuous flow reactor among the 4 continuous flow reactors;
and/or a product outlet is arranged on the fourth continuous flow reactor in the 4 continuous flow reactors and is used for outputting the parachlorophenyl hydrazine hydrochloride.
6. The p-chlorophenylhydrazine hydrochloride reaction system of claim 1, wherein the continuous flow reactor is one or more of a microreactor, a tubular reactor, a cascade mixer, a static mixer.
7. The p-chlorophenylhydrazine hydrochloride reaction system of claim 6, wherein the continuous flow reactor is a microreactor.
8. The p-chlorophenylhydrazine hydrochloride reaction system of claim 1, wherein the p-chlorophenylhydrazine hydrochloride reaction system comprises a slurry transfer pump and a diaphragm metering pump;
and/or the p-chlorophenylhydrazine hydrochloride reaction system comprises a heat conducting oil heating device.
9. The p-chlorophenylhydrazine hydrochloride reaction system of claim 8, wherein the diazonium salt intermediate liquid inlet pipe, the reducing agent liquid inlet pipe and the hydrochloric acid liquid inlet pipe are provided with the slurry delivery pump and the diaphragm metering pump in sequence; wherein, the diaphragm metering pump is two diaphragm metering pumps that the parallel arrangement was put.
10. The p-chlorophenylhydrazine hydrochloride reaction system of claim 8, wherein the heat transfer oil heating means is connected to the reduction reaction zone and the hydrolysis reaction zone respectively by a heat transfer oil feed line and a heat transfer oil discharge line for heating the n reduction reaction vessels and the hydrolysis reaction vessels by heat transfer oil.
11. A method of using the p-chlorophenylhydrazine hydrochloride reaction system according to any one of claims 1 to 10, comprising the steps of: the method comprises the steps of respectively inputting heat conduction oil into a reduction reaction zone and a hydrolysis reaction zone through heat conduction oil liquid inlet pipelines, and continuously inputting diazonium salt intermediate solution and reducing agent into the reduction reaction zone through diazonium salt intermediate liquid inlet pipelines and reducing agent liquid inlet pipelines respectively for reduction reaction to obtain a reduction intermediate solution; and continuously inputting the hydrochloric acid solution into the hydrolysis reaction zone through the hydrochloric acid liquid inlet pipeline to carry out hydrolysis reaction to obtain the p-chlorophenylhydrazine hydrochloride.
12. The method for using a p-chlorophenylhydrazine hydrochloride reaction system according to claim 11, wherein a diazonium salt intermediate solution and a reducing agent are continuously input into a 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, a first reduction reaction liquid enters a second reduction reaction unit to an nth reduction reaction unit which are sequentially connected in series for reaction, after the reaction is finished, an nth reduction reaction liquid enters 2 continuous flow reactors which are sequentially connected in series for reaction, after the reaction is finished, a reduction intermediate solution enters a plate heat exchanger, then enters a reduction intermediate liquid storage tank and is input into the hydrolysis reaction kettle through a liquid storage outlet; and continuously inputting the hydrochloric acid solution into the hydrolysis reaction kettle through the hydrochloric acid liquid inlet pipeline, 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.
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| CN106316879A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Method for preparing hydrazinobenzene in continuous micro-channel reactor |
| CN107663160B (en) * | 2016-07-27 | 2019-03-01 | 上海惠和化德生物科技有限公司 | A kind of continuous flow synthesis technology of 4- chlorobenzene hydrazonium salt |
| CN107573256B (en) * | 2017-09-26 | 2020-02-21 | 安徽国星生物化学有限公司 | Continuous production method and device for p-chlorophenylhydrazine hydrochloride |
| CN107739313B (en) * | 2017-11-29 | 2020-04-17 | 黑龙江鑫创生物科技开发有限公司 | Method for synthesizing 4-amino-3-chlorophenol by multi-temperature-zone continuous flow microchannel reactor |
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