CN112225677A - Reaction system and method for p-chlorophenylhydrazine hydrochloride - Google Patents
Reaction system and method for p-chlorophenylhydrazine hydrochloride Download PDFInfo
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Abstract
The invention discloses a reaction system and a method for p-chlorophenylhydrazine hydrochloride, wherein the reaction system for p-chlorophenylhydrazine hydrochloride 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; 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 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
Technical Field
The invention relates to a reaction system and a reaction method for p-chlorophenylhydrazine hydrochloride.
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 desirable to provide a system and a method for reacting p-chlorophenylhydrazine hydrochloride.
Disclosure of Invention
The invention aims to overcome the defects that in the prior art, a p-chlorophenylhydrazine hydrochloride reaction system has long reaction time, low production efficiency, low product purity, high production energy consumption and high cost, increases the industrialization difficulty, cannot realize large-scale continuous production and the like, and provides a p-chlorophenylhydrazine hydrochloride reaction system and a method.
The invention solves the technical problems through 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 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 present invention, a reduction reaction may be performed 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.
In the present invention, the hydrolysis reaction zone may perform a 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 microreactor, a tubular reactor, a cascade mixer, and a static mixer; preferably a microreactor.
In the invention, the reaction system for p-chlorophenylhydrazine hydrochloride can also comprise a slurry conveying 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. 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.
In the invention, the reaction system of the p-chlorophenylhydrazine hydrochloride can also comprise a heat-conducting 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 invention also provides a using method of the p-chlorophenylhydrazine hydrochloride reaction system, which comprises the following steps: 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, for example, a sodium sulfite solution.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
(1) the reaction system of p-chlorophenylhydrazine hydrochloride 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 energy consumption, saves cost, and has no problems of wastewater treatment, environmental pollution and the like.
(2) The reaction system of p-chlorophenylhydrazine hydrochloride 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, few side reactions, no other impurities in the crude product, high yield, simple post-treatment and easy separation.
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
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
Reducing intermediate liquid storage tank 45
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
Detailed Description
The invention is further illustrated by 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 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;
and/or the diazonium salt intermediate liquid inlet pipeline comprises n diazonium salt intermediate liquid inlet pipelines connected in parallel and is respectively used for inputting diazonium salt intermediate solutions into the n reduction reaction kettles.
3. 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.
4. 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;
and/or 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.
5. The chlorophenylhydrazine hydrochloride reaction system as claimed in claim 1, wherein the reducing intermediate storage tank is provided with a storage inlet and a storage outlet; the liquid storage inlet is preferably connected with the plate heat exchanger; the liquid storage outlet is preferably connected with the hydrolysis reaction kettle.
6. 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/or a product liquid outlet is arranged on the fourth continuous flow reactor in the 4 continuous flow reactors and is used for outputting the p-chlorophenylhydrazine hydrochloride.
7. 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; preferably a microreactor.
8. 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;
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 is preferably two diaphragm metering pumps which are arranged in parallel;
and/or the p-chlorophenylhydrazine hydrochloride reaction system comprises a heat conduction oil heating device;
preferably, the heat-conducting oil heating device is respectively connected with the reduction reaction zone and the hydrolysis reaction zone through a heat-conducting oil inlet pipeline and a heat-conducting oil outlet pipeline, and is used for heating the n reduction reaction kettles and the hydrolysis reaction kettle through heat-conducting oil.
9. A method for using the p-chlorophenylhydrazine hydrochloride reaction system as defined in any one of claims 1 to 8, comprising the steps of: respectively inputting heat conducting oil into the reduction reaction zone and the hydrolysis reaction zone 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 through the diazonium salt intermediate liquid inlet pipeline and the reducing agent liquid inlet pipeline respectively to carry out 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.
10. The use method of the p-chlorophenylhydrazine hydrochloride reaction system as claimed in claim 9, wherein the diazonium salt intermediate solution and the reducing agent are continuously fed into the first reduction reaction unit for reaction through the diazonium salt intermediate liquid inlet pipeline and the reducing agent liquid inlet pipeline, after the reaction is completed, the first reduction reaction solution enters the second reduction reaction unit to the nth reduction reaction unit which are connected in series in sequence for reaction, after the reaction is completed, the nth reduction reaction solution enters the 2 continuous flow reactors which are connected in series in sequence for reaction, after the reaction is completed, the reduction intermediate solution enters the plate heat exchanger, then enters the reduction intermediate liquid storage tank, and is fed 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.
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| CN107739313A (en) * | 2017-11-29 | 2018-02-27 | 黑龙江鑫创生物科技开发有限公司 | A kind of method of the multi-temperature zone continuous stream micro passage reaction synthesis chlorophenol of 4 amino 3 |
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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 |
| CN107663161A (en) * | 2016-07-27 | 2018-02-06 | 上海惠和化德生物科技有限公司 | A kind of continuous stream synthesis technique of phenylhydrazine salt and substituted benzene hydrazonium salt |
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