CN116440846A

CN116440846A - Chlorination separation equipment for improving yield of 6-chloro-2-nitrotoluene and preparation method

Info

Publication number: CN116440846A
Application number: CN202310698820.1A
Authority: CN
Inventors: 田兆勇; 郭春鹏; 巩鹏飞
Original assignee: Shandong Green Tai New Materials Co ltd
Current assignee: Shandong Green Tai New Materials Co ltd
Priority date: 2023-06-14
Filing date: 2023-06-14
Publication date: 2023-07-18
Anticipated expiration: 2043-06-14
Also published as: CN116440846B

Abstract

The invention relates to the technical field of 6-chloro-2-nitrotoluene production, and particularly discloses chlorination separation equipment and a preparation method for improving the yield of 6-chloro-2-nitrotoluene.

Description

Chlorination separation equipment for improving yield of 6-chloro-2-nitrotoluene and preparation method

Technical Field

The invention relates to the technical field of 6-chloro-2-nitrotoluene production, in particular to chlorination separation equipment for improving the yield of 6-chloro-2-nitrotoluene and a preparation method thereof.

Background

The 6-chloro-2-nitrotoluene is an organic synthesis intermediate for chloridizing o-nitrotoluene, and is mainly used for synthesizing 3-chloro-2-methylaniline, 2, 6-dichlorobenzaldehyde and the like, wherein in the prior art, the 6-chloro-2-nitrotoluene is prepared by filling the o-nitrotoluene with chlorine gas to carry out specific chloridizing reaction, and then carrying out steps of acid washing, water washing, alkali washing, fractionation and the like, and parts such as a reaction kettle in 6-chloro-2-nitrotoluene production equipment in the prior art are common equipment.

The invention patent application No. 201010278858.6 discloses a method for preparing 6-chloro-2-nitrotoluene, which comprises the following steps: putting ortho-nitrotoluene into a reaction kettle, starting stirring, putting a catalyst, heating, keeping the temperature within the range of 25-85 ℃, introducing chlorine, detecting, finishing the reaction when the ortho-nitrotoluene content is 8-12%, cooling, discharging, and entering a rectification working section, wherein the chlorination reaction kettle used in the actual production is a common reaction kettle, and the synchronous reaction point and the reaction contact surface of the chlorine and the ortho-nitrotoluene are less, so that the chlorination reaction efficiency is required to be further improved.

In addition, the added solid raw materials and the liquid raw materials are easy to agglomerate when being mixed, so that partial parts are easy to be blocked, the reaction efficiency is affected because the partial parts cannot be fully reacted, and in addition, the partial products are more remained in the previous working procedure in the process of transferring and conveying among the working procedures, so that the final yield of the products is affected.

Disclosure of Invention

The invention aims to provide a chlorination separation device and a preparation method for improving the yield of 6-chloro-2-nitrotoluene, which can effectively improve the synchronous reaction point and the reaction contact surface of chlorine and o-nitrotoluene, effectively prevent caking of solid raw materials and blockage of part of parts, fully react the raw materials, effectively reduce the residue of a product in the last process in the process of transferring and conveying among the processes, and prevent influencing the final yield of the product so as to solve the problems in the prior art.

In order to achieve the above purpose, the present invention provides the following technical solutions: the utility model provides an improve chlorination splitter of 6-chloro-2-nitrotoluene yield, includes reation kettle subassembly, the stirring subassembly and the inflation subassembly that establish in the middle of the reation kettle subassembly, one side of reation kettle subassembly is equipped with first separation kettle subassembly, be equipped with the adsorption module in the first separation kettle subassembly, one side of first separation kettle subassembly is equipped with the second separation kettle subassembly, the top of second separation kettle subassembly is equipped with the decompression subassembly, be equipped with first conveying subassembly between reation kettle subassembly and the first separation kettle subassembly, be equipped with the second conveying subassembly between first separation kettle subassembly and the second separation kettle subassembly;

The reaction kettle assembly comprises a reaction bin, a reaction bin cover is arranged at the top of the reaction bin, first air inlet pipe joints are arranged on two sides of the reaction bin cover, the air charging assembly comprises an upper air guide pipe, and the upper air guide pipe is communicated with the bottom end of the first air inlet pipe joint through a corrugated pipe arranged at the top;

the first separation kettle assembly comprises a first separation bin, the adsorption assembly comprises a cylindrical molecular sieve which is in sliding fit with the inner wall of the first separation bin, and the top surface of the cylindrical molecular sieve is elastically connected with the inner wall of the first separation bin through an elastic sheet;

the second separation kettle component comprises a second separation bin, a first electric valve is arranged on one side of the top of the second separation bin, a hose is arranged on one side of the top surface of the second separation bin, the pressure reducing component comprises an electric push rod arranged at the top of the second separation bin, and a piston plate which is in sliding fit with the inner wall of the second separation bin is arranged at the lower end of a piston rod of the electric push rod.

Preferably, the outside fixed cover of reaction storehouse is equipped with first heating storehouse, and is fixed in the outside of the bottom of reaction storehouse and be equipped with first supporting seat, the centre of reaction storehouse bottom is fixed downwards and is linked together there is first flowing back coupling, and the lower port department fixed mounting of first flowing back coupling has first solenoid valve, the right side of first air inlet coupling is equipped with the first sensor mount pad that is linked together with reaction storehouse lid inner wall, and has first pressure sensor in the last port department fixed mounting of first sensor mount pad, the right side fixed mounting of reaction storehouse lid upper end has level sensor.

Preferably, the lower end of the inner wall of the reaction bin is fixedly provided with a positioning ring, the left side and the right side of the positioning ring are symmetrically provided with limiting holes, the left side and the right side of the upper air guide pipe are fixedly communicated with side air guide pipes which are inserted and matched with the limiting holes downwards, the inner side of the side air guide pipe is fixedly communicated with radial air guide pipes from top to bottom, the side of the radial air guide pipe is fixedly communicated with annular air guide pipes which are annularly and uniformly distributed, and the lower end of the annular air guide pipe is provided with air outlet holes which are annularly and uniformly distributed.

Preferably, the stirring assembly comprises a stirring motor fixedly mounted at the upper end of the reaction bin cover, a first connecting plate is fixedly connected to the lower end of a main shaft of the stirring motor, a second connecting plate is fixedly connected to the lower end of the first connecting plate, a rotating shaft is vertically and fixedly connected to the lower end of the second connecting plate, stirring rods are annularly and fixedly connected to the side face of the rotating shaft, and the stirring rods are staggered with the annular air guide pipe in the vertical direction.

Preferably, the inside bottom surface of first separation storehouse is equipped with the heating rod, the upper end of first separation storehouse is detained and is equipped with first separation storehouse lid, the outside fixed cover of first separation storehouse is equipped with the second heating storehouse, and has the flowing back storehouse in the bottom of first separation storehouse fixed connection downwards, the outside fixedly connected with supporting baseplate of flowing back storehouse bottom, and is fixed to be equipped with the second supporting seat in the outside of supporting baseplate's lower extreme, the centre of flowing back storehouse bottom is fixed downwards and is linked together there is the second flowing back coupling, and has the third solenoid valve at the downward fixed mounting of second flowing back coupling.

Preferably, the middle of the upper end of the first separation bin cover is fixedly communicated with a second sensor mounting seat, a second pressure sensor is fixedly arranged at the upper port of the second sensor mounting seat, a first liquid inlet pipe joint communicated with the lower end of the first separation bin cover is arranged on the left side of the second sensor mounting seat, and a first air outlet pipe joint communicated with the lower end of the first separation bin cover is arranged on the right side of the second sensor mounting seat.

Preferably, the first conveying component comprises a conveying pump and a second electromagnetic valve, a first conveying pipe is fixedly communicated between the left end of the conveying pump and the lower end of the first electromagnetic valve, a second conveying pipe is fixedly communicated between the conveying pump and the second electromagnetic valve, and a third conveying pipe is fixedly communicated between the second electromagnetic valve and the first liquid inlet pipe joint.

Preferably, the outside fixed cover in second separation storehouse is equipped with the third heating storehouse, the lower extreme in second separation storehouse is fixed with the third supporting seat, the bottom in second separation storehouse is fixed downwards and is linked together there is the third fluid-discharge tube connector, and at the lower extreme fixed mounting of third fluid-discharge tube connector there is the fifth solenoid valve, the inner wall in second separation storehouse is fixed to the outside in third heating storehouse and is linked together there is the second coupling that admits air, be equipped with the second motorised valve on the hose, the tip of hose is linked together with the top of the first coupling that admits air of both sides respectively through the tee bend.

Preferably, the second conveying assembly comprises a flowmeter, a fourth conveying pipe is fixedly communicated between the flowmeter and the first air outlet pipe joint, and a fourth electromagnetic valve is fixedly communicated between the flowmeter and the second air inlet pipe joint.

The preparation method for improving the yield of 6-chloro-2-nitrotoluene adopts the chloridizing separation equipment for improving the yield of 6-chloro-2-nitrotoluene to realize the improvement of the yield of 6-chloro-2-nitrotoluene, and comprises the following steps:

firstly, preparing materials, namely weighing solid-liquid raw materials for preparing 6-chloro-2-nitrotoluene according to corresponding components, putting the weighed raw materials into a reaction bin, and covering the reaction bin at the upper end of the reaction bin to be fixedly buckled, wherein the raw materials for preparing 6-chloro-2-nitrotoluene comprise o-nitrotoluene, ferric trichloride and chlorine;

heating and stirring, namely filling hot water into the reaction kettle assembly, enabling the temperature in the reaction bin to be within 60-70 ℃, starting the stirring assembly to stir the materials in the reaction bin, and controlling the stirring rotating speed to be 160-200 r/min;

step three, ventilation reaction, namely discharging chlorine into the reaction bin by utilizing the inflation assembly, and reacting the chlorine discharged into the reaction bin with materials in the reaction bin, wherein the reaction time is controlled to be 15-20 hours;

Step four, primary transfer, namely conveying the chlorinated products in the reaction bin into the first separation bin by utilizing the first conveying component to finish primary transfer action of materials;

fifthly, heating, adsorbing and separating, namely filling hot water into the first separation kettle assembly, controlling the temperature in the first separation bin to be 50-60 ℃, then filling a certain amount of nitrogen into the first separation bin, controlling the pressure in the first separation bin to be 1.2-1.4 standard atmospheric pressures, enabling benzene products in the first separation bin to be adsorbed in a cylindrical molecular sieve, discharging other liquid from the bottom of the first separation bin, and controlling the adsorption time to be 30-35 min;

step six, heating and vaporizing, namely firstly filling high-temperature gas into the first separation bin to control the temperature in the second separation bin to be 150-160 ℃, then heating the cylindrical molecular sieve to control the heating temperature to be 240-260 ℃ to vaporize benzene products adsorbed in the cylindrical molecular sieve, and controlling the heating time to be 15-20 min;

step seven, secondary transfer, namely conveying the vaporized benzene products in the first separation bin into a second separation bin by utilizing the second conveying assembly, so as to finish secondary transfer of materials;

Step eight, depressurization and separation, namely starting the electric push rod to drive the piston plate to move upwards along the inner wall of the second separation bin, further completing depressurization control on the internal pressure of the second separation bin, and sequentially separating the reacted benzene substances under different pressure conditions, wherein the separated benzene substances comprise o-nitrotoluene, 6-chloro-2-nitrotoluene and 4-chloro-2-nitrotoluene.

Compared with the prior art, the invention has the following beneficial effects:

1. according to the invention, chlorine can be filled into the upper air guide pipe through the first air inlet pipe joint, and the chlorine is sprayed into the reaction bin from the lower port of the air outlet hole along the side air guide pipe, the radial air guide pipe and the annular air guide pipe in the upper air guide pipe to react with the o-nitrotoluene, wherein the annular air guide pipe is arranged in a multi-layer way from top to bottom and from inside to outside, so that the synchronous reaction point and the reaction contact surface of the chlorine and the o-nitrotoluene are improved, and the chlorination reaction efficiency is improved.

2. According to the invention, in the process that chlorine on the upper side of the piston plate is filled into the reaction bin, the fifth electromagnetic valve is in an open state, the fourth electromagnetic valve is in a closed state, the electric push rod is made to stretch back and forth, the shrinkage is larger than the elongation, the up-and-down reciprocating motion of the annular gas guide pipe is realized, the blocking of the gas outlet hole caused by the attachment of a solid-liquid mixture on the gas outlet hole is effectively prevented, and meanwhile, the further scattering of the solid raw material can be realized by utilizing the cooperation of the up-and-down motion of the annular gas guide pipe and the horizontal rotary motion of the stirring rod, and the caking of the solid raw material is effectively prevented.

3. When the top of the cylindrical molecular sieve is covered by residues and impurities, the electric push rod can stretch back and forth, and the cylindrical molecular sieve is elastically connected with the inner wall of the first separation bin through the elastic sheet, so that the high-frequency up-and-down vibration of the cylindrical molecular sieve is realized, the residues and impurities attached to the top of the cylindrical molecular sieve can vibrate, benzene products on the cylindrical molecular sieve are further fully vaporized by starting the heating rod in the vibration process, and the yield of the products is improved.

Drawings

FIG. 1 is an isometric view of the overall structure of the present invention;

FIG. 2 is an axial side half sectional view of the overall structure of the present invention;

FIG. 3 is an enlarged schematic view of the partial structure at A in FIG. 2;

FIG. 4 is an enlarged schematic view of a partial structure at B in FIG. 2;

FIG. 5 is an enlarged schematic view of the partial structure at F in FIG. 2;

FIG. 6 is an enlarged schematic view of a part of the structure at G in FIG. 2;

FIG. 7 is a front view of the overall structure of the present invention;

FIG. 8 is an isometric view of the cross-sectional structure of FIG. 7 at C-C;

FIG. 9 is an isometric view of the cross-sectional structure of FIG. 7 at D-D;

fig. 10 is an isometric view of the cross-sectional structure of fig. 7 at E-E.

In the figure: 1. a reaction kettle assembly; 2. a stirring assembly; 3. an inflation assembly; 4. a first transport assembly; 5. a first separation tank assembly; 6. an adsorption assembly; 7. a second transport assembly; 8. a second separation tank assembly; 9. a pressure relief assembly; 101. a reaction bin; 102. a reaction bin cover; 103. a first support base; 104. a first heating bin; 105. a positioning ring; 106. a limiting hole; 107. a first air inlet pipe joint; 108. a first sensor mount; 109. a first pressure sensor; 110. a liquid level sensor; 111. a first drain pipe joint; 112. a first electromagnetic valve; 201. a stirring motor; 202. a first connection plate; 203. a second connecting plate; 204. a rotating shaft; 205. a stirring rod; 301. an upper airway; 302. a side airway; 303. a radial air duct; 304. an annular air guide pipe; 305. an air outlet hole; 306. a bellows; 401. a transfer pump; 402. a first delivery tube; 403. a second delivery tube; 404. a second electromagnetic valve; 405. a third delivery tube; 501. a first separation bin; 502. a first separation bin cover; 503. a second support base; 504. a second heating bin; 505. a liquid discharge bin; 506. a support base plate; 507. a second drain pipe joint; 508. a third electromagnetic valve; 509. the first liquid inlet pipe joint; 510. a second sensor mount; 511. a second pressure sensor; 512. a first outlet pipe joint; 601. cylindrical molecular sieves; 602. a heating rod; 603. an elastic sheet; 701. a fourth conveying pipe; 702. a flow meter; 703. a fourth electromagnetic valve; 801. a second separation bin; 802. a third support base; 803. a third heating bin; 804. a third drain pipe joint; 805. a fifth electromagnetic valve; 806. a second air inlet pipe joint; 807. a first electrically operated valve; 808. a hose; 901. an electric push rod; 902. a piston plate.

Detailed Description

The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

First embodiment

Referring to fig. 1-10, the present invention provides a technical solution: the utility model provides an improve chlorination splitter of 6-chloro-2-nitrotoluene yield, including reation kettle subassembly 1, stirring subassembly 2 and the subassembly 3 of aerifing that establish in the middle of reation kettle subassembly 1, one side of reation kettle subassembly 1 is equipped with first separation cauldron subassembly 5, be equipped with adsorption component 6 in the first separation cauldron subassembly 5, one side of first separation cauldron subassembly 5 is equipped with second separation cauldron subassembly 8, the top of second separation cauldron subassembly 8 is equipped with decompression subassembly 9, be equipped with first conveying component 4 between reation kettle subassembly 1 and the first separation cauldron subassembly 5, be equipped with second conveying component 7 between first separation cauldron subassembly 5 and the second separation cauldron subassembly 8.

The reaction kettle assembly 1 comprises a reaction bin 101, a reaction bin cover 102 is arranged at the top of the reaction bin 101, first air inlet pipe joints 107 are arranged on two sides of the reaction bin cover 102, a first heating bin 104 is fixedly sleeved on the outer side of the reaction bin 101, a first supporting seat 103 is fixedly arranged on the outer side of the bottom of the reaction bin 101, a first liquid outlet pipe joint 111 is fixedly communicated downwards in the middle of the bottom of the reaction bin 101, a first electromagnetic valve 112 is fixedly arranged at the lower port of the first liquid outlet pipe joint 111, a first sensor mounting seat 108 which is communicated with the inner wall of the reaction bin cover 102 is arranged on the right side of the first air inlet pipe joint 107, a first pressure sensor 109 is fixedly arranged at the upper port of the first sensor mounting seat 108, a liquid level sensor 110 is fixedly arranged on the right side of the upper end of the reaction bin cover 102, a positioning ring 105 is fixedly arranged on the lower end of the inner wall of the reaction bin 101, limiting holes 106 are symmetrically arranged on the left side and the right side of the positioning ring 105, the first heating bin 104 controls the temperature in the reaction bin 101 in a certain range, a chlorination reaction bin 101 is provided with a first electromagnetic valve 112, the right side of the first liquid outlet pipe joint is provided with a first sensor mounting seat 108 which is communicated with the inner wall of the first liquid outlet pipe joint, the first pressure sensor 109 can be communicated with the first air inlet pipe joint 101, the first pressure sensor is communicated with the first air inlet pipe joint is formed by the first pressure sensor 101, the chlorine sensor is communicated with the first liquid inlet pipe joint 101, the chlorine sensor is communicated with the first pressure sensor 101, the chlorine bin is formed in the reaction bin 101, the reaction bin is communicated with the air chamber, the air inlet pipe joint is communicated with the air chamber and can be communicated with the air chamber, and can be monitored, and the air chamber and can be communicated with the air chamber and has a real-time, and can be communicated with the air chamber and has the air inlet cavity and has the air inlet flow chamber and has the air chamber 1.

Further, chlorine is conveyed into the upper air guide pipe 301 through the first air inlet pipe joint 107, is continuously conveyed into the annular air guide pipe 304 along the side air guide pipe 302 and the radial air guide pipe 303, and is continuously discharged into the reaction liquid in the reaction bin 101 through the air outlet hole 305 at the lower end of the annular air guide pipe 304, so that the conveyed chlorine can perform multi-point synchronous contact reaction in the o-nitrotoluene liquid, the contact area of the reaction is increased, the absorption rate of the chlorine is increased, and the whole chlorination reaction efficiency is improved.

The stirring assembly 2 comprises a stirring motor 201 fixedly mounted at the upper end of the reaction bin cover 102, a first connecting plate 202 is fixedly connected to the lower end of a main shaft of the stirring motor 201, a second connecting plate 203 is fixedly connected to the lower end of the first connecting plate 202, a rotating shaft 204 is vertically and fixedly connected to the lower end of the second connecting plate 203, stirring rods 205 are annularly and fixedly connected to the side surfaces of the rotating shaft 204, the stirring rods 205 are staggered with an annular air guide pipe 304 in the vertical direction, and specifically, the main shaft of the stirring motor 201 drives the first connecting plate 202 to rotate, so that the first connecting plate 202 rotates synchronously with the second connecting plate 203, the rotating shaft 204 and the stirring rods 205.

The inflating assembly 3 comprises an upper air guide pipe 301, the upper air guide pipe 301 is communicated with the bottom end of the first air inlet pipe joint 107, the left side and the right side of the upper air guide pipe 301 are fixedly communicated with side air guide pipes 302 which are inserted and matched with the limiting holes 106, the inner sides of the side air guide pipes 302 are fixedly communicated with radial air guide pipes 303 from top to bottom, annular air guide pipes 304 which are annularly and uniformly distributed are fixedly communicated with the side surfaces of the radial air guide pipes 303, air outlet holes 305 which are annularly and uniformly distributed are formed in the lower ends of the annular air guide pipes 304, and particularly, when the stirring rod 205 stirs and rotates the o-nitrotoluene in the reaction bin 101, chlorine gas discharged from the air outlet holes 305 at the lower ends of the annular air guide pipes 304 can be in contact reaction with the o-nitrotoluene at different points, so that the synchronous contact point and the whole reaction area of the chlorine gas are improved, and the whole chlorination reaction efficiency is improved.

The first separation kettle assembly 5 comprises a first separation bin 501, a heating rod 602 is arranged on the inner bottom surface of the first separation bin 501, a first separation bin cover 502 is buckled at the upper end of the first separation bin 501, a second heating bin 504 is fixedly sleeved at the outer side of the first separation bin 501, a liquid draining bin 505 is fixedly communicated with the bottom of the first separation bin 501 downwards, a supporting bottom plate 506 is fixedly connected to the outer side of the bottom of the liquid draining bin 505, a second supporting seat 503 is fixedly arranged at the outer side of the lower end of the supporting bottom plate 506, a second liquid draining pipe joint 507 is fixedly communicated with the middle of the bottom of the liquid draining bin 505 downwards, a third electromagnetic valve 508 is fixedly communicated with the middle of the upper end of the second liquid draining pipe joint 507, a second sensor mounting seat 510 is fixedly communicated with the middle of the upper end of the first separation bin cover 502, a second pressure sensor 511 is fixedly arranged at the upper end of the second sensor mounting seat 510, a first liquid inlet pipe joint is arranged at the left side of the second sensor mounting seat 510 and is communicated with the lower end of the first separation bin 502, a second liquid draining pipe joint is arranged at the right side of the second sensor mounting seat 509, the second liquid draining bin is communicated with the second liquid draining bin 502, a liquid is completely filtered by the second liquid is drained into the second liquid draining bin 502, and is completely communicated with the second liquid draining bin 502, and is completely filtered by the liquid is completely drained into the second liquid draining bin 501, and is completely communicated with the second liquid draining pipe joint is connected to the second liquid draining cabin through the second electromagnetic valve, and is completely separated by the second liquid draining pipe joint, and is completely connected to the second liquid draining pipe pipeline.

The adsorption component 6 comprises a cylindrical molecular sieve 601 in sliding fit with the inner wall of the first separation bin 501, specifically, when the liquid in the reaction bin 101 is conveyed into the first separation bin 501 through the first conveying component 4, benzene liquid in the liquid is adsorbed into the cylindrical molecular sieve 601 through the cylindrical molecular sieve 601, other waste materials are filtered into a liquid discharge bin 505 at the lower end of the first separation bin 501, after the adsorption is completed, the waste materials are discharged, and then a heating rod 602 is started to heat the benzene liquid in the cylindrical molecular sieve 601 at a high temperature, so that the benzene liquid is separated from the cylindrical molecular sieve 601 after vaporization.

The second separation kettle component 8 comprises a second separation bin 801, a first electric valve 807 is arranged on one side of the top of the second separation bin 801, a hose 808 is arranged on one side of the top surface of the second separation bin 801, a third heating bin 803 is fixedly sleeved on the outer side of the second separation bin 801, a third supporting seat 802 is fixedly arranged at the lower end of the second separation bin 801, a third liquid discharging pipe joint 804 is fixedly communicated with the bottom of the second separation bin 801 downwards, a fifth electromagnetic valve 805 is fixedly arranged at the lower end of the third liquid discharging pipe joint 804, a second air inlet pipe joint 806 is fixedly communicated with the inner wall of the second separation bin 801 towards the outer side of the third heating bin 803, a second electric valve is arranged on the hose 808, the end part of the hose 808 is respectively communicated with the top ends of the first air inlet pipe joints 107 on two sides through a tee joint, specifically, the third heating bin 803 can control the temperature in the second separation bin 801, the third heating bin 803 is used for heating the second separation bin 801 to control the temperature to be 150-160 ℃, the gas conveyed into the second separation bin 801 is condensed and separated one by one along with the pressure change in the second separation bin 801, o-nitrotoluene, 6-chloro-2-nitrotoluene and 4-chloro-2-nitrotoluene are separated in different pressure ranges, the o-nitrotoluene, 6-chloro-2-nitrotoluene and 4-chloro-2-nitrotoluene are communicated with different recovery pipelines through the fifth electromagnetic valve 805, when each substance is singly separated, the fifth electromagnetic valve 805 is opened, and the separated product is conveyed into the corresponding recovery pipeline.

Further, in the initial state, the second separation chamber 801 is located at the upper side of the piston plate 902 to quantitatively store chlorine to be added into the reaction chamber 101.

The decompression assembly 9 comprises an electric push rod 901 arranged at the top of a second separation bin 801, a piston plate 902 which is in sliding fit with the inner wall of the second separation bin 801 is arranged at the lower end of a piston rod of the electric push rod 901, and specifically, the electric push rod 901 is started to drive the piston plate 902 to lift up in the second separation bin 801, so that the pressure in the second separation bin 801 is subjected to corresponding decompression treatment, and after the pressure in the second separation bin 801 is reduced to different degrees, the corresponding benzene gas is liquefied and separated.

The first conveying assembly 4 comprises a conveying pump 401 and a second electromagnetic valve 404, a first conveying pipe 402 is fixedly communicated between the left end of the conveying pump 401 and the lower end of the first electromagnetic valve 112, a second conveying pipe 403 is fixedly communicated between the conveying pump 401 and the second electromagnetic valve 404, a third conveying pipe 405 is fixedly communicated between the second electromagnetic valve 404 and a first liquid inlet pipe joint 509, specifically, the second electromagnetic valve 404 is an electric control three-way valve, the second electromagnetic valve 404 is opened, the second conveying pipe 403 is communicated with the third conveying pipe 405, the conveying pump 401 is started to convey liquid in the reaction bin 101 to the first separation bin 501 through the first liquid outlet pipe joint 111, the conveying pump 401, the second conveying pipe 403 and the third conveying pipe 405, the conveying pump 401 is stopped after conveying is finished, the second electromagnetic valve 404 is communicated with an external nitrogen pipeline, a certain amount of nitrogen is filled into the first separation bin 501 through the nitrogen pipeline, the pressure in the first separation bin 501 is increased, and the adsorption and filtration of benzene liquid in the first separation bin is accelerated through the cylindrical molecular sieve 501.

The second conveying assembly 7 comprises a flow meter 702, a fourth conveying pipe 701 is fixedly communicated between the flow meter 702 and the first air outlet pipe joint 512, a fourth electromagnetic valve 703 is fixedly communicated between the flow meter 702 and the second air inlet pipe joint 806, specifically, the fourth electromagnetic valve 703 is an electric control three-way valve, the fourth electromagnetic valve 703 is opened to communicate the fourth conveying pipe 701 with the second air inlet pipe joint 806, the flow meter 702 is started to convey the gas in the first separation bin 501 into the second separation bin 801 through the first air outlet pipe joint 512, the fourth conveying pipe 701 and the second air inlet pipe joint 806, after conveying is finished, the flow meter 702 is stopped, the fourth electromagnetic valve 703 is communicated with a nitrogen pipeline, and nitrogen is filled into the second separation bin 801 through the nitrogen pipeline, so that the second separation bin 801 obtains certain initial pressure, and subsequent decompression separation treatment is facilitated.

When the device of the embodiment is used, firstly, solid-liquid raw materials for preparing 6-chloro-2-nitrotoluene are respectively weighed according to corresponding components and then put into a reaction chamber 101, a reaction chamber cover 102 is fixedly buckled at the upper end of the reaction chamber 101, hot water is filled into a first heating chamber 104 to keep the temperature in the reaction chamber 101 constant, then a stirring motor 201 is started to drive a main shaft of the stirring motor to drive a first connecting plate 202 to rotate, further a second connecting plate 203, a rotating shaft 204 and a stirring rod 205 are synchronously rotated, the stirring rod 205 performs stirring action relative to materials in the reaction chamber 101, meanwhile, a first air inlet pipe joint 107 is communicated with a hose 808 and a second electric valve is opened, the first electric valve 807 is kept in a closed state, a fifth electromagnetic valve 805 is in an open state, a fourth electromagnetic valve 703 is in a closed state, and an electric push rod 901 is started to drive a piston plate 902 to slide upwards, the quantitative chlorine gas stored at the top of the second separation bin 801 is all conveyed into the upper air guide pipe 301 through a hose 808 and a first air inlet pipe joint 107, the chlorine gas is conveyed into the radial air guide pipe 303 through the side air guide pipes 302 at two sides of the upper air guide pipe 301, and is discharged into the reaction bin 101 from the air outlet holes 305 through the annular air guide pipe 304 to react with the materials in the reaction bin 101, after the chlorine gas in the second separation bin 801 is all output, the third electric valve is closed, after the materials in the reaction bin 101 are reacted, the first electromagnetic valve 112 and the second electromagnetic valve 404 are opened, the conveying pump 401 is started to convey the chlorinated products in the reaction bin 101 into the first separation bin 501 through the first liquid discharge pipe joint 111, the first conveying pipe 402, the second conveying pipe 403, the third conveying pipe 405 and the first liquid inlet pipe joint 509, the transfer of the materials is completed, after the transfer is completed, the conveying pump 401 is stopped, while closing the first solenoid 112.

Then, hot water is filled into the second heating bin 504 to keep the temperature in the first separation bin 501 constant, then the second electromagnetic valve 404 is communicated with an external nitrogen pipeline, a certain amount of nitrogen is filled into the first separation bin 501, the pressure display of the second pressure sensor 511 is observed to control the pressure within 1.2-1.4 standard atmospheric pressure ranges, benzene products in the first separation bin 501 are adsorbed in the cylindrical molecular sieve 601, other liquids such as water are conveyed into the liquid discharge bin 505, after adsorption separation is finished, the third electromagnetic valve 508 is communicated with an external waste liquid recovery pipeline, the third electromagnetic valve 508 is opened, waste liquid in the liquid discharge bin 505 is conveyed downwards into the recovery pipeline, and the third electromagnetic valve 508 is closed after the conveying is finished.

Then, the first electric valve 807 is opened, the piston plate 902 is driven by the electric push rod 901 to move downwards to a position close to the second air inlet pipe joint 806, high-temperature gas is filled into the third heating bin 803, the temperature in the second separation bin 801 is controlled to be 150-160 ℃, the heating rod 602 is started to heat the cylindrical molecular sieve 601 at high temperature, the heating temperature is controlled to be 240-260 ℃, benzene products adsorbed in the cylindrical molecular sieve 601 are vaporized, the fourth electromagnetic valve 703 is started, the flowmeter 702 is started, meanwhile, the piston plate 902 is driven by the electric push rod 901 to move upwards to perform air suction, and the vaporized benzene products in the first separation bin 501 can be conveyed into the second separation bin 801 through the first air outlet pipe joint 512, the fourth conveying pipe 701 and the second air inlet pipe joint 806, so that material transfer is completed.

Finally, the piston plate 902 is driven to move upwards along the inner wall of the second separation bin 801 by starting the electric push rod 901, so that the pressure reduction control on the internal pressure of the second separation bin 801 is completed, the benzene substances after reaction are separated in sequence under different pressure conditions and discharged through the third liquid discharge pipe joint 804, and the separated benzene substances comprise o-nitrotoluene, 6-chloro-2-nitrotoluene and 4-chloro-2-nitrotoluene.

Second embodiment

Referring to fig. 1-10, in a chlorination separation device for improving the yield of 6-chloro-2-nitrotoluene according to the first embodiment, in the actual use process, since the raw materials added into the reaction bin 101 contain solids, the solid raw materials are easy to adhere to the gas outlet holes 305 after contacting with the liquid raw materials, which can then cause blocking of the gas outlet holes 305, and the solid raw materials are easy to agglomerate after contacting with the liquid raw materials, and since the stirring rods 205 are staggered with the annular gas guide tube 304, rotation of the stirring rods 205 can only proceed to the mixing frame plate in the horizontal direction, but a larger gap exists between two stirring rods 205 adjacent to each other, which can not break up the agglomerated materials and sufficiently and uniformly mix with the liquid materials, which affects the reaction efficiency, and in addition, when evaporating the benzene products on the cylindrical molecular sieve 601, residues with partial incomplete reaction and other impurities can adhere to the cylindrical molecular sieve 601, which can not sufficiently evaporate the benzene products on the cylindrical molecular sieve 601, which can not fully vaporize, thereby affecting the yield of the products, in order to solve the above problems:

The upper air duct 301 is communicated with the bottom end of the first air inlet pipe joint 107 through a corrugated pipe 306 arranged at the top, and specifically, the corrugated pipe 306 can realize the up-and-down movement of the side air duct 302.

The top surface of the cylindrical molecular sieve 601 is elastically connected with the inner wall of the first separation bin 501 through an elastic sheet 603.

When the device is used, the extension of the electric push rod 901 is utilized to drive the piston plate 902 to move downwards to charge chlorine on the upper side of the piston plate 902 into the reaction bin 101, the fifth electromagnetic valve 805 is in an open state, the fourth electromagnetic valve 703 is in a closed state, the electric push rod 901 is enabled to reciprocate and stretch out and draw back, intermittent air supply to the reaction bin 101 can be achieved, in the reciprocating and stretching process of the electric push rod 901, when the electric push rod 901 stretches out and draws back, air is pumped through the hose 808, part of liquid in the reaction bin 101 is sucked into the annular air guide pipe 304, when the electric push rod 901 contracts, air is exhausted through the hose 808, the process can discharge chlorine into the reaction bin 101 through the air outlet holes 305, and as the contraction amount of the electric push rod 901 is larger than the extension amount, chlorine can be gradually discharged into the reaction bin 101 until the chlorine on the upper side of the piston plate 902 is completely discharged, and the chlorine can generate an upward reversing force when the air outlet holes 305 are discharged into the inside of the liquid raw material in the reaction bin 101, upward sliding of the side air guide pipe 302 can be achieved under the action of the corrugated pipe, further, the reciprocating air guide pipe 302 and the side air guide pipe 302 can be utilized to reciprocate and the annular air guide pipe 302 can be sucked into the annular air guide pipe 304 through the hose 808, the air outlet holes can be effectively moved upwards and downwards through the air guide pipe 304, and can be effectively prevented from being matched with the air outlet holes to move downwards, and can be prevented from being horizontally and horizontally matched with the raw material, and the stirring rod is prevented from being adhered to the upper and lower to the solid and lower, and the raw material is prevented from being adhered to the upper and lower, and easier, and lower, and easier, and the raw material,.

In addition, after the benzene products in the first separation bin 501 are gasified, in the process of driving the piston plate 902 to move upwards by utilizing the first electric push rod 901 to pump the benzene vapors into the second separation bin 801, when the flow meter 702 detects that the flow rate of the flowing vapors is smaller than the threshold value set by the flow meter 702, the surface of the cylindrical molecular sieve 601 is actively judged to be attached with more residues and impurities to influence the evaporation and gasification of the benzene products, because the chlorine gas on the upper side of the piston plate 902 is completely discharged into the reaction bin 101, the second electric valve on the hose 808 is closed at the moment, the first electric valve 807 is opened, the fifth electromagnetic valve 805 is closed, the electric push rod 901 is made to reciprocate and expand, during the extension process of the electric push rod 901, the piston plate 902 moves downwards, the second air inlet pipe joint 806 and the fourth conveying pipe 701 are reversely exhausted into the first separation bin 501, so that the air pressure in the first separation bin 501 is increased, because the cylindrical molecular sieve 601 is elastically connected with the inner wall of the first separation bin 501 through the elastic sheet 603, the downward movement of the cylindrical molecular sieve 601 can be realized, in the contraction process of the electric push rod 901, the air is pumped from the first separation bin 501 through the second air inlet pipe joint 806 and the fourth conveying pipe 701, the position of the first separation bin 501 on the upper side of the cylindrical molecular sieve 601 is in a negative pressure state, the cylindrical molecular sieve 601 moves upwards, thereby realizing the high-frequency up-and-down vibration of the cylindrical molecular sieve 601 by utilizing the high-frequency reciprocating micro-expansion of the electric push rod 901, the residues and impurities attached to the top of the cylindrical molecular sieve 601 can vibrate, in the vibration process, benzene products on the cylindrical molecular sieve 601 are further fully evaporated and vaporized by starting the heating rod 602, in the evaporation process, the air pressure on the upper side of the cylindrical molecular sieve 601 is gradually increased, under the action of the elastic sheet 603, the cylindrical molecular sieve 601 gradually slides downwards to realize buffering, after evaporation is carried out for a designated time, the electric push rod 901 stops reciprocating expansion and drives the piston plate 902 to move upwards continuously, and the evaporated benzene products can be pumped into the second separation bin 801 more fully, so that the yield of the products is improved.

Therefore, in the process of filling chlorine gas on the upper side of the piston plate 902 into the reaction bin 101, the fifth electromagnetic valve 805 is in an open state, the fourth electromagnetic valve 703 is in a closed state, the electric push rod 901 is made to reciprocate and stretch, the contraction amount is larger than the elongation amount, the up-and-down reciprocating motion of the annular gas guide pipe 304 is realized, the blocking of the gas outlet 305 caused by the attachment of a solid-liquid mixture on the gas outlet 305 is effectively prevented, and meanwhile, the further scattering of the solid raw material can be realized by utilizing the up-and-down motion of the annular gas guide pipe 304 and the horizontal rotary motion of the stirring rod 205 in cooperation, and the caking of the solid raw material is effectively prevented; in addition, when the top of the cylindrical molecular sieve 601 is covered by residues and impurities, the electric push rod 901 is made to stretch back and forth, and as the cylindrical molecular sieve 601 is elastically connected with the inner wall of the first separation bin 501 through the elastic piece 603, high-frequency up-and-down vibration of the cylindrical molecular sieve 601 is realized, so that the residues and impurities attached to the top of the cylindrical molecular sieve 601 can vibrate, and benzene products on the cylindrical molecular sieve 601 are further fully vaporized by starting the heating rod 602 in the vibration process.

Third embodiment

The invention also provides a preparation method for improving the yield of 6-chloro-2-nitrotoluene, which is realized by a chlorination separation device for improving the yield of 6-chloro-2-nitrotoluene and comprises the following steps:

Firstly, preparing materials, namely weighing solid-liquid raw materials for preparing 6-chloro-2-nitrotoluene according to corresponding components, putting the solid-liquid raw materials into a reaction bin 101, and fixedly buckling a reaction bin cover 102 at the upper end of the reaction bin 101, wherein the raw materials for preparing 6-chloro-2-nitrotoluene comprise o-nitrotoluene, ferric trichloride and chlorine;

step two, heating and stirring, namely filling hot water into the first heating bin 104 to maintain the temperature in the reaction bin 101 within 60-70 ℃, then starting the stirring motor 201 to drive the first connecting plate 202 to rotate by the main shaft of the stirring motor, and further synchronously rotating the stirring rod 205 and the second connecting plate 203 together with the rotating shaft 204 by the stirring rod 205 to stir the materials in the reaction bin 101, wherein the rotating speed of the stirring motor 201 is controlled to be 160-200 r/min;

step three, ventilation reaction, namely communicating the first air inlet pipe joint 107 with a hose 808, opening a second electric valve, keeping the first electric valve 807 in a closed state, keeping the fifth electromagnetic valve 805 in an open state, starting an electric push rod 901 to drive a piston plate 902 to slide upwards at the same time, conveying all quantitative chlorine stored at the top of a second separation bin 801 into an upper air guide pipe 301 through the hose 808 and the first air inlet pipe joint 107, conveying the chlorine into a radial air guide pipe 303 through side air guide pipes 302 at two sides of the upper air guide pipe 301, and reacting the chlorine discharged from an air outlet hole 305 into a reaction bin 101 through an annular air guide pipe 304 with materials in the reaction bin 101, wherein the reaction time is controlled to be 15-20 hours;

In the process of filling chlorine gas on the upper side of the piston plate 902 into the reaction bin 101, the fifth electromagnetic valve 805 is in an open state, the fourth electromagnetic valve 703 is in a closed state, the electric push rod 901 is made to reciprocate and stretch, the contraction amount is larger than the elongation amount, the up-and-down reciprocating motion of the annular gas guide pipe 304 is realized, the blocking of the gas outlet hole 305 caused by the attachment of a solid-liquid mixture on the gas outlet hole 305 is effectively prevented, and meanwhile, the further scattering of solid raw materials can be realized by utilizing the up-and-down motion of the annular gas guide pipe 304 and the horizontal rotary motion of the stirring rod 205 in a matching manner, and the caking of the solid raw materials is effectively prevented;

step four, transferring once, after the material in the reaction bin 101 is reacted, opening a first electromagnetic valve 112 and a second electromagnetic valve 404, starting a conveying pump 401 to convey chlorinated products in the reaction bin 101 into a first separation bin 501 through a first liquid discharge pipe joint 111, a first conveying pipe 402, a second conveying pipe 403, a third conveying pipe 405 and a first liquid inlet pipe joint 509, completing the material transfer, closing the conveying pump 401 after the material transfer is completed, and simultaneously closing the first electromagnetic valve 112;

step five, heating, adsorbing and separating, namely filling hot water into a second heating bin 504, controlling the temperature in a first separation bin 501 to be 50-60 ℃, then communicating a second electromagnetic valve 404 with an external nitrogen pipeline, filling a certain amount of nitrogen into the first separation bin 501, observing the pressure display of a second pressure sensor 511, controlling the pressure display within a pressure range of 1.2-1.4 standard atmospheres, adsorbing benzene products in the first separation bin 501 in a cylindrical molecular sieve 601, conveying other liquid into a liquid discharge bin 505, communicating a third electromagnetic valve 508 with an external waste liquid recovery pipeline after the adsorption and separation are finished, opening the third electromagnetic valve 508, conveying waste liquid in the liquid discharge bin 505 downwards into a recovery pipeline, and closing the third electromagnetic valve 508 after the conveying is finished;

Step six, heating and vaporizing, namely opening a first electric valve 807, driving a piston plate 902 to move downwards to a position close to a second air inlet pipe joint 806 by utilizing an electric push rod 901, filling high-temperature gas into a third heating bin 803, controlling the temperature in the second separation bin 801 to be 150-160 ℃, starting a heating rod 602 to heat a cylindrical molecular sieve 601, controlling the heating temperature to be 240-260 ℃, and vaporizing benzene products adsorbed in the cylindrical molecular sieve 601, wherein the heating time is controlled to be 15-20 min;

step seven, secondary transfer, namely opening a fourth electromagnetic valve 703, starting a flowmeter 702, and simultaneously driving a piston plate 902 to move upwards by utilizing an electric push rod 901 to perform air extraction action, wherein benzene products vaporized in a first separation bin 501 can be conveyed into a second separation bin 801 through a first air outlet pipe joint 512, a fourth conveying pipe 701 and a second air inlet pipe joint 806, so that material transfer is completed;

when the top of the cylindrical molecular sieve 601 is covered by residues and impurities, the electric push rod 901 is made to stretch back and forth, and as the cylindrical molecular sieve 601 is elastically connected with the inner wall of the first separation bin 501 through the elastic piece 603, high-frequency up-down vibration of the cylindrical molecular sieve 601 is realized, so that the residues and impurities attached to the top of the cylindrical molecular sieve 601 can vibrate, and benzene products on the cylindrical molecular sieve 601 are further fully evaporated and vaporized by starting the heating rod 602 in the vibration process;

Step eight, depressurization and separation, namely, starting the electric push rod 901 to drive the piston plate 902 to continuously move upwards along the inner wall of the second separation bin 801, so as to complete depressurization control on the internal pressure of the second separation bin 801, sequentially separating the reacted benzene substances under different pressure conditions and discharging the benzene substances through the third liquid discharge pipe joint 804, wherein the separated benzene substances comprise o-nitrotoluene, 6-chloro-2-nitrotoluene and 4-chloro-2-nitrotoluene.

Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The utility model provides an improve chlorination separation device of 6-chloro-2-nitrotoluene yield which characterized in that: the reaction kettle comprises a reaction kettle assembly, a stirring assembly and an inflating assembly which are arranged in the middle of the reaction kettle assembly, wherein a first separation kettle assembly is arranged on one side of the reaction kettle assembly, an adsorption assembly is arranged in the first separation kettle assembly, a second separation kettle assembly is arranged on one side of the first separation kettle assembly, a decompression assembly is arranged at the top of the second separation kettle assembly, a first conveying assembly is arranged between the reaction kettle assembly and the first separation kettle assembly, and a second conveying assembly is arranged between the first separation kettle assembly and the second separation kettle assembly;

2. The chlorination separation device for improving the yield of 6-chloro-2-nitrotoluene according to claim 1, wherein: the outside fixed cover of reaction storehouse is equipped with first heating storehouse, and is fixed in the outside of the bottom of reaction storehouse to be equipped with first supporting seat, the centre of reaction storehouse bottom is fixed downwards and is linked together there is first flowing back coupling, and the lower port department fixed mounting of first flowing back coupling has first solenoid valve, the right side of first air inlet coupling is equipped with the first sensor mount pad that is linked together with reaction storehouse lid inner wall, and has first pressure sensor in the last port department fixed mounting of first sensor mount pad, the right side fixed mounting of reaction storehouse lid upper end has level sensor.

3. The chlorination separation device for improving the yield of 6-chloro-2-nitrotoluene according to claim 1, wherein: the lower end of the inner wall of the reaction bin is fixedly provided with a positioning ring in an annular manner, the left side and the right side of the positioning ring are symmetrically provided with limiting holes, the left side and the right side of the upper air guide pipe are fixedly communicated with side air guide pipes which are inserted and matched with the limiting holes in a downward manner, the inner side of the side air guide pipe is fixedly communicated with a radial air guide pipe from top to bottom in a bilateral manner, the side face of the radial air guide pipe is fixedly communicated with an annular air guide pipe which is uniformly distributed in an annular manner, and the lower end of the annular air guide pipe is provided with air outlet holes which are uniformly distributed in an annular manner.

4. The chlorination separation device for improving the yield of 6-chloro-2-nitrotoluene according to claim 1, wherein: the stirring assembly comprises a stirring motor fixedly mounted at the upper end of the reaction bin cover, a first connecting plate is fixedly connected to the lower end of a main shaft of the stirring motor, a second connecting plate is fixedly connected to the lower end of the first connecting plate, a rotating shaft is vertically and fixedly connected to the lower end of the second connecting plate, stirring rods are fixedly connected to the side faces of the rotating shaft in a circumferential direction, and the stirring rods are staggered with the circumferential air guide pipe in the vertical direction.

5. The chlorination separation device for improving the yield of 6-chloro-2-nitrotoluene according to claim 1, wherein: the inside bottom surface of first separation storehouse is equipped with the heating rod, the upper end of first separation storehouse is detained and is equipped with first separation storehouse lid, the outside fixed cover of first separation storehouse is equipped with the second heating storehouse, and has the flowing back storehouse in the bottom of first separation storehouse fixed connection downwards, the outside fixedly connected with supporting baseplate of flowing back storehouse bottom, and is fixed to be equipped with the second supporting seat in the outside of supporting baseplate's lower extreme, the centre of flowing back storehouse bottom is fixed downwards and is linked together there is the second flowing back coupling, and has the third solenoid valve at the downward fixed mounting of second flowing back coupling.

6. The chlorination separation device for increasing the yield of 6-chloro-2-nitrotoluene of claim 5, wherein: the middle of the upper end of the first separation bin cover is fixedly communicated with a second sensor mounting seat, a second pressure sensor is fixedly arranged at the upper port of the second sensor mounting seat, a first liquid inlet pipe joint communicated with the lower end of the first separation bin cover is arranged on the left side of the second sensor mounting seat, and a first air outlet pipe joint communicated with the lower end of the first separation bin cover is arranged on the right side of the second sensor mounting seat.

7. The chlorination separation device for increasing the yield of 6-chloro-2-nitrotoluene of claim 6, wherein: the first conveying assembly comprises a conveying pump and a second electromagnetic valve, a first conveying pipe is fixedly communicated between the left end of the conveying pump and the lower end of the first electromagnetic valve, a second conveying pipe is fixedly communicated between the conveying pump and the second electromagnetic valve, and a third conveying pipe is fixedly communicated between the second electromagnetic valve and the first liquid inlet pipe joint.

8. The chlorination separation device for increasing the yield of 6-chloro-2-nitrotoluene of claim 6, wherein: the outside fixed cover in second separation storehouse is equipped with the third heating storehouse, the lower extreme in second separation storehouse is fixed and is equipped with the third supporting seat, the bottom in second separation storehouse is fixed downwards and is linked together there is the third fluid-discharge tube connector, and at the lower extreme fixed mounting of third fluid-discharge tube connector there is the fifth solenoid valve, the inner wall in second separation storehouse is fixed to the outside in third heating storehouse and is linked together there is the second coupling that admits air, be equipped with the second motorised valve on the hose, the tip of hose is linked together with the top of the first coupling that admits air of both sides respectively through the tee bend.

9. The chlorination separation device for increasing the yield of 6-chloro-2-nitrotoluene of claim 8, wherein: the second conveying assembly comprises a flowmeter, a fourth conveying pipe is fixedly communicated between the flowmeter and the first air outlet pipe joint, and a fourth electromagnetic valve is fixedly communicated between the flowmeter and the second air inlet pipe joint.

10. A method for improving the yield of 6-chloro-2-nitrotoluene, which is realized by using the chlorination separation device according to claim 1, and is characterized by comprising the following steps: