CN113477183A - Reaction kettle for p-chlorobenzyl chloride production and production process of p-chlorobenzyl chloride - Google Patents
Reaction kettle for p-chlorobenzyl chloride production and production process of p-chlorobenzyl chloride Download PDFInfo
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- CN113477183A CN113477183A CN202110756127.6A CN202110756127A CN113477183A CN 113477183 A CN113477183 A CN 113477183A CN 202110756127 A CN202110756127 A CN 202110756127A CN 113477183 A CN113477183 A CN 113477183A
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- reaction kettle
- kettle body
- gas inlet
- barometer
- reation kettle
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 84
- JQZAEUFPPSRDOP-UHFFFAOYSA-N 1-chloro-4-(chloromethyl)benzene Chemical compound ClCC1=CC=C(Cl)C=C1 JQZAEUFPPSRDOP-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 12
- 230000007613 environmental effect Effects 0.000 claims abstract description 8
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 28
- 238000002347 injection Methods 0.000 claims description 13
- 239000007924 injection Substances 0.000 claims description 13
- NPDACUSDTOMAMK-UHFFFAOYSA-N 4-Chlorotoluene Chemical compound CC1=CC=C(Cl)C=C1 NPDACUSDTOMAMK-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 125000006283 4-chlorobenzyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1Cl)C([H])([H])* 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 3
- 238000012824 chemical production Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- PTHGDVCPCZKZKR-UHFFFAOYSA-N (4-chlorophenyl)methanol Chemical compound OCC1=CC=C(Cl)C=C1 PTHGDVCPCZKZKR-UHFFFAOYSA-N 0.000 description 1
- PVNUPDOGDDNZBB-UHFFFAOYSA-N 3-(4-chlorophenyl)propanenitrile Chemical compound ClC1=CC=C(CCC#N)C=C1 PVNUPDOGDDNZBB-UHFFFAOYSA-N 0.000 description 1
- AVPYQKSLYISFPO-UHFFFAOYSA-N 4-chlorobenzaldehyde Chemical compound ClC1=CC=C(C=O)C=C1 AVPYQKSLYISFPO-UHFFFAOYSA-N 0.000 description 1
- XRHGYUZYPHTUJZ-UHFFFAOYSA-N 4-chlorobenzoic acid Chemical compound OC(=O)C1=CC=C(Cl)C=C1 XRHGYUZYPHTUJZ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- WKSAUQYGYAYLPV-UHFFFAOYSA-N pyrimethamine Chemical compound CCC1=NC(N)=NC(N)=C1C1=CC=C(Cl)C=C1 WKSAUQYGYAYLPV-UHFFFAOYSA-N 0.000 description 1
- 229960000611 pyrimethamine Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/14—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the side-chain of aromatic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a reaction kettle for producing p-chlorobenzyl chloride and a production process of the p-chlorobenzyl chloride, and relates to the technical field of chemical production. This reation kettle is used in production of parachlorobenzyl chloride, including the reation kettle body, the bottom of reation kettle body is provided with the bottom through the connecting piece, the left side of reation kettle body is provided with gas inlet and pan feeding mouth. This reation kettle and production technology of parachlorobenzyl chloride are used in parachlorobenzyl chloride production becomes two relatively independent spaces through keeping apart reation kettle inside to the atmospheric pressure of the environment of reaction is changed through the mode of magnetic field atmospheric pressure, thereby increases reaction degree, and whole improvement can not make reation kettle appear the position of revealing easily simultaneously, fine assurance reation kettle's atmospheric pressure safe value, thereby reduced material cost and environmental maintenance cost.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a reaction kettle for producing p-chlorobenzyl chloride and a production process of the p-chlorobenzyl chloride.
Background
The p-chlorobenzyl chloride is needle crystal with melting point of 29 deg.c and boiling point of 222 deg.c, and is decomposed at 214 deg.c. Flash point 97 ℃. Can be sublimed, dissolved in diethyl ether, acetic acid, carbon disulfide and benzene, and still dissolved in cold ethanol. The freezing point is 31 ℃, and the relative density is 1.270-1.280. Can be dissolved in ethanol, ether and acetone, is insoluble in water, is an organic synthetic raw material, and can be used for preparing p-chlorobenzyl alcohol, p-chlorobenzaldehyde, p-chlorobenzyl acetonitrile, p-chlorobenzoic acid, etc. The pharmaceutical industry is used for preparing pyrimethamine and the like, and in addition, the application is also applied to the dye industry.
In the prior art, p-chlorobenzyl chloride is obtained after p-chlorotoluene and liquid chlorine react by taking catalyst azo as a catalyst, the existing reaction kettle is difficult to well realize higher reaction degree on the premise of ensuring the safety value of air pressure, and the p-chlorotoluene and the liquid chlorine do not react sufficiently to cause the waste of materials, so that the material cost and the environmental maintenance cost are increased.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a reaction kettle for producing p-chlorobenzyl chloride and a production process of the p-chlorobenzyl chloride, and solves the problems that in the prior art, the p-chlorobenzyl chloride is obtained by reacting p-chlorotoluene and liquid chlorine with a catalyst azo as a catalyst, the existing reaction kettle is difficult to realize high reaction degree on the premise of ensuring the safety value of air pressure, the p-chlorotoluene and the liquid chlorine do not react sufficiently to cause material waste, and the material cost and the environmental maintenance cost are increased.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a reaction kettle for producing p-chlorobenzyl chloride comprises a reaction kettle body, wherein the bottom of the reaction kettle body is provided with a bottom cover through a connecting piece, the left side of the reaction kettle body is provided with a gas inlet and a feeding port, the right side of the reaction kettle body is provided with a gas outlet, the right side of the reaction kettle body is provided with a first air pressure gauge, two sides of an inner cavity of the reaction kettle body are provided with limiting blocks, the horizontal positions of the gas inlet, the feeding port and the gas outlet are all positioned below the limiting blocks, a piston body is arranged in the inner cavity of the reaction kettle body and positioned above the limiting blocks, the inner cavity of the reaction kettle body is divided into two relatively sealed spaces by the piston body, a permanent magnet is fixedly arranged on the piston body, the top of the reaction kettle body is embedded with a coil block which is matched with the permanent magnet, and the direction of a magnetic field generated after the coil block is electrified is opposite to the direction of the magnetic field of the permanent magnet, and the top of the reaction kettle body is respectively provided with a pressurized gas inlet and a second barometer.
Preferably, the piston body is provided with a guide rod in a penetrating mode, the top end of the guide rod is fixedly arranged at the top of the inner cavity of the reaction kettle body, the bottom end of the guide rod is fixedly provided with a guide block, and the guide block is fixed on the inner wall of the reaction kettle body.
Preferably, a one-way valve is arranged on the gas inlet.
A production process of p-chlorobenzyl chloride comprises the reaction kettle for producing the p-chlorobenzyl chloride, and comprises the following specific operations:
s1, determining and obtaining quantitative p-chlorotoluene, catalyst azo and liquid chlorine according to production requirements;
s2, raising the environmental temperature of the reaction kettle for producing p-chlorobenzyl chloride to 93-97 ℃;
s3, opening an air outlet, and then adding the p-chlorotoluene obtained in the step S1 into the reaction kettle body through a feeding port;
s4, adding the catalyst azo obtained in the step S1 into the reaction kettle body through a feeding port, and then closing a gas outlet;
s5, simultaneously injecting the liquid chlorine obtained in the step S1 into the inner cavity of the reaction kettle body through the pressurized gas inlet and the gas inlet, monitoring the pressure condition of the inner cavity of the reaction kettle body in real time through the first barometer and the second barometer, and carrying out different operations according to the pressure condition displayed by the corresponding barometers, wherein the specific operations are as follows:
1. stopping injecting the liquid chlorine at the pressurized gas inlet when the pressure value displayed by the second barometer reaches the maximum safety value, and stopping injecting the liquid chlorine at the gas inlet when the pressure value displayed by the first barometer reaches the maximum safety value, wherein the maximum safety value is determined according to the material and the inner wall thickness of the reaction kettle body and is the maximum pressure value which can be borne by the reaction kettle body;
2. injection rate of pressurized gas inlet liquid chlorine: the injection speed of liquid chlorine at the gas inlet is 1:3 to 2: 7;
3. when the pressure value displayed by the first barometer and the pressure value displayed by the second barometer are larger than the maximum safety value of the piston body, stopping the injection of the liquid chlorine at the pressurized gas inlet and the gas inlet, and then entering the step S6;
4. after the liquid chlorine obtained in the step S1 is completely injected, closing the pressurized gas inlet and the gas inlet, and determining whether the pressure value displayed by the current first barometer reaches the maximum safe value, if not, switching on the power supply of the coil block to generate a mutually repulsive magnetic field between the coil block and the permanent magnet, and moving the piston body downwards relative to the reaction kettle body to possibly increase the value displayed by the first barometer, and then entering the step S6;
s6, after waiting for 3 hours, stopping heating the environment, opening the gas outlet to recover the redundant gas, and opening the bottom cover after the gas pressure is stable to take out the substances in the reaction kettle body;
and S7, stirring the substance obtained in the step S6 for 30 minutes, pumping the substance into a distillation kettle for distillation, pumping the parachlorobenzyl into a parachlorobenzyl elevated tank for the next step, and thus finishing the production of the parachlorobenzyl chloride.
(III) advantageous effects
The invention provides a reaction kettle for producing p-chlorobenzyl chloride and a production process of the p-chlorobenzyl chloride. The method has the following beneficial effects: this reation kettle and production technology of parachlorobenzyl chloride are used in parachlorobenzyl chloride production becomes two relatively independent spaces through keeping apart reation kettle inside to the atmospheric pressure of the environment of reaction is changed through the mode of magnetic field atmospheric pressure, thereby increases reaction degree, and whole improvement can not make reation kettle appear the position of revealing easily simultaneously, fine assurance reation kettle's atmospheric pressure safe value, thereby reduced material cost and environmental maintenance cost.
Drawings
FIG. 1 is a schematic view of the structure of the present invention.
In the figure: 1. a reaction kettle body; 2. a bottom cover; 3. a gas inlet; 4. a feeding port; 5. an air outlet; 6. a first barometer; 7. a limiting block; 8. a piston body; 9. a guide bar; 10. a guide block; 11. a permanent magnet; 12. a coil block; 13. a pressurized gas inlet; 14. and a second barometer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: a reaction kettle for producing p-chlorobenzyl chloride comprises a reaction kettle body 1, the bottom of the reaction kettle body 1 is provided with a bottom cover 2 through a connecting piece, the left side of the reaction kettle body 1 is provided with a gas inlet 3 and a material inlet 4, the gas inlet 3 is provided with a one-way valve 15, the right side of the reaction kettle body 1 is provided with a gas outlet 5, the right side of the reaction kettle body 1 is provided with a first air pressure meter 6, two sides of the inner cavity of the reaction kettle body 1 are provided with limit blocks 7, the horizontal positions of the gas inlet 3, the material inlet 4 and the gas outlet 5 are all positioned below the limit blocks 7, the inner cavity of the reaction kettle body 1 and positioned above the limit blocks 7 are provided with a piston body 8, a guide rod 9 penetrates through the piston body 8, the top end of the guide rod 9 is fixedly arranged at the top of the inner cavity of the reaction kettle body 1, the bottom end of the guide rod 9 is fixedly provided with a guide block 10, the guide block 10 is fixed on the inner wall of the reaction kettle body 1, the inner cavity of the reaction kettle body 1 is divided into two relatively sealed spaces by the piston body 8, the permanent magnet 11 is fixedly arranged on the piston body 8, the coil block 12 which is matched with the permanent magnet 11 is embedded in the top of the reaction kettle body 1, the direction of a magnetic field generated after the coil block 12 is electrified is opposite to the direction of the magnetic field of the permanent magnet 11, and the top of the reaction kettle body 1 is respectively provided with a pressurized gas inlet 13 and a second barometer 14.
A production process of p-chlorobenzyl chloride comprises the reaction kettle for producing p-chlorobenzyl chloride, and comprises the following specific operations:
s1, determining and obtaining quantitative p-chlorotoluene, catalyst azo and liquid chlorine according to production requirements;
s2, raising the environmental temperature of the reaction kettle for producing p-chlorobenzyl chloride to 93-97 ℃;
s3, opening the air outlet 5, and then adding the p-chlorotoluene obtained in the step S1 into the reaction kettle body 1 through the feeding port 4;
s4, adding the catalyst azo obtained in the step S1 into the reaction kettle body 1 through a feeding port 4, and then closing a gas outlet 5;
s5, simultaneously injecting the liquid chlorine obtained in the step S1 into the inner cavity of the reaction kettle body 1 through the pressurized gas inlet 13 and the gas inlet 3, monitoring the pressure condition of the inner cavity of the reaction kettle body 1 in real time through the first barometer 6 and the second barometer 14, and carrying out different operations according to the pressure condition displayed by the corresponding barometers, wherein the specific operations are as follows:
1. stopping the injection of the liquid chlorine at the pressurized gas inlet 13 when the pressure value displayed by the second barometer 14 reaches the maximum safety value, and stopping the injection of the liquid chlorine at the gas inlet 3 when the pressure value displayed by the first barometer 6 reaches the maximum safety value, wherein the maximum safety value is determined according to the material and the inner wall thickness of the reaction kettle body 1 and is the maximum pressure value which can be borne by the reaction kettle body 1;
2. injection rate of liquid chlorine at the pressurized gas inlet 13: the injection speed of the liquid chlorine at the gas inlet 3 is 1:3 to 2: 7;
3. when the pressure value displayed by the first barometer 6 and the pressure value displayed by the second barometer 14 are larger than the maximum safety value of the piston body 8, stopping the injection of the liquid chlorine at the pressurized gas inlet 13 and the gas inlet 3, and then entering the step S6;
4. after the liquid chlorine obtained in step S1 is completely injected, the pressurized gas inlet 13 and the gas inlet 3 are closed, and it is determined whether the pressure value currently displayed by the first barometer 6 reaches the maximum safe value, if not, the power supply of the coil block 12 is turned on, so that a mutually repulsive magnetic field is generated between the coil block 12 and the permanent magnet 11, and the piston body 8 is moved downward relative to the reaction vessel body 1, thereby possibly increasing the value displayed by the first barometer 6, and then the process proceeds to step S6;
s6, after waiting for 3 hours, stopping heating the environment, opening the gas outlet 5 to recycle the redundant gas, and opening the bottom cover 2 after the gas pressure is stable to take out the substances in the reaction kettle body 1;
and S7, stirring the substance obtained in the step S6 for 30 minutes, pumping the substance into a distillation kettle for distillation, pumping the parachlorobenzyl into a parachlorobenzyl elevated tank for the next step, and thus finishing the production of the parachlorobenzyl chloride.
In conclusion, this reation kettle for p-chlorobenzyl chloride production and production technology of p-chlorobenzyl chloride become two relatively independent spaces through keeping apart reation kettle inside to the atmospheric pressure of the environment of reaction is changed through the mode of magnetic field atmospheric pressure, thereby increases the reaction degree, and whole improvement can not make reation kettle appear the position of revealing easily simultaneously, and the fine atmospheric pressure safe value of having guaranteed reation kettle has thus reduced material cost and environmental maintenance cost.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The utility model provides a reation kettle is used in production of parachlorobenzyl chloride, includes reation kettle body (1), the bottom of reation kettle body (1) is provided with bottom (2) through the connecting piece, the left side of reation kettle body (1) is provided with gas inlet (3) and pan feeding mouth (4), the right side of reation kettle body (1) is provided with gas outlet (5), the right side of reation kettle body (1) is provided with first barometer (6), its characterized in that: the two sides of the inner cavity of the reaction kettle body (1) are provided with limit blocks (7), the horizontal positions of the gas inlet (3), the feeding port (4) and the gas outlet (5) are all positioned below the limit blocks (7), a piston body (8) is arranged in the inner cavity of the reaction kettle body (1) and above the limiting block (7), the piston body (8) divides the inner cavity of the reaction kettle body (1) into two relatively sealed spaces, a permanent magnet (11) is fixedly arranged on the piston body (8), a coil block (12) matched with the permanent magnet (11) is embedded at the top of the reaction kettle body (1), the direction of the magnetic field generated after the coil block (12) is electrified is opposite to the direction of the magnetic field of the permanent magnet (11), the top of the reaction kettle body (1) is respectively provided with a pressurized gas inlet (13) and a second barometer (14).
2. The reaction kettle for producing p-chlorobenzyl chloride according to claim 1, which is characterized in that: the reaction kettle is characterized in that a guide rod (9) penetrates through the piston body (8), the top end of the guide rod (9) is fixedly arranged at the top of the inner cavity of the reaction kettle body (1), a guide block (10) is fixedly arranged at the bottom end of the guide rod (9), and the guide block (10) is fixed on the inner wall of the reaction kettle body (1).
3. The reaction kettle for producing p-chlorobenzyl chloride according to claim 1, which is characterized in that: and a one-way valve (15) is arranged on the gas inlet (3).
4. The production process of p-chlorobenzyl chloride is characterized by comprising the following steps: the reaction kettle for producing p-chlorobenzyl chloride comprises the reaction kettle for producing p-chlorobenzyl chloride as claimed in claim 1, and is specifically operated as follows:
s1, determining and obtaining quantitative p-chlorotoluene, catalyst azo and liquid chlorine according to production requirements;
s2, raising the environmental temperature of the reaction kettle for producing p-chlorobenzyl chloride to 93-97 ℃;
s3, opening the air outlet (5), and then adding the p-chlorotoluene obtained in the step S1 into the reaction kettle body (1) through the feeding port (4);
s4, adding the catalyst azo obtained in the step S1 into the reaction kettle body (1) through a feeding port (4), and then closing an air outlet (5);
s5, simultaneously injecting the liquid chlorine obtained in the step S1 into the inner cavity of the reaction kettle body (1) through the pressurized gas inlet (13) and the gas inlet (3), monitoring the pressure condition of the inner cavity of the reaction kettle body (1) in real time through the first barometer (6) and the second barometer (14), and performing different operations according to the pressure condition displayed by the corresponding barometers, wherein the specific operations are as follows:
1) stopping the injection of the liquid chlorine at the pressurized gas inlet (13) when the pressure value displayed by the second barometer (14) reaches the maximum safety value, and stopping the injection of the liquid chlorine at the gas inlet (3) when the pressure value displayed by the first barometer (6) reaches the maximum safety value, wherein the maximum safety value is determined according to the material and the inner wall thickness of the reaction kettle body (1) and is the maximum pressure value which can be borne by the reaction kettle body (1);
2) injection rate of liquid chlorine into the pressurized gas inlet (13): the injection speed of the liquid chlorine at the gas inlet (3) is 1:3 to 2: 7;
3) when the pressure value displayed by the first barometer (6) and the pressure value displayed by the second barometer (14) are larger than the maximum safety value of the piston body (8), stopping the injection of the liquid chlorine at the pressurized gas inlet (13) and the gas inlet (3), and then entering the step S6;
4) after the liquid chlorine obtained in the step S1 is completely injected, closing the pressurized gas inlet (13) and the gas inlet (3), judging whether the pressure value displayed by the first gas pressure gauge (6) reaches the maximum safe value or not, if not, switching on the power supply of the coil block (12), so that a mutually repulsive magnetic field is generated between the coil block (12) and the permanent magnet (11), and enabling the piston body (8) to move downwards relative to the reaction kettle body (1), so as to possibly increase the value displayed by the first gas pressure gauge (6), and then entering a step S6;
s6, after waiting for 3 hours, stopping heating the environment, opening the gas outlet (5) to recover the redundant gas, and opening the bottom cover (2) after the gas pressure is stable to take out the substances in the reaction kettle body (1);
and S7, stirring the substance obtained in the step S6 for 30 minutes, pumping the substance into a distillation kettle for distillation, pumping the parachlorobenzyl into a parachlorobenzyl elevated tank for the next step, and thus finishing the production of the parachlorobenzyl chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110756127.6A CN113477183A (en) | 2021-07-05 | 2021-07-05 | Reaction kettle for p-chlorobenzyl chloride production and production process of p-chlorobenzyl chloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110756127.6A CN113477183A (en) | 2021-07-05 | 2021-07-05 | Reaction kettle for p-chlorobenzyl chloride production and production process of p-chlorobenzyl chloride |
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| CN113477183A true CN113477183A (en) | 2021-10-08 |
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| CN202110756127.6A Pending CN113477183A (en) | 2021-07-05 | 2021-07-05 | Reaction kettle for p-chlorobenzyl chloride production and production process of p-chlorobenzyl chloride |
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Application publication date: 20211008 |