CN115463632A - A kind of p-fluorobenzaldehyde chlorination device and processing method thereof - Google Patents

Abstract

The invention discloses a p-fluorobenzaldehyde chlorination device and a processing method thereof, comprising a reaction tank body, a motor is arranged on the reaction tank body, and a stirring shaft is connected to the lower end of the motor through a reduction box. The wall of the reaction tank is provided with a first stirring plate, the outer wall of the reaction tank is provided with a tail gas purification mechanism for chlorine gas treatment during the chlorination reaction, and the inner bottom of the reaction tank is provided with a second stirring plate for moving the reaction liquid up and down. Stirring mechanism; by setting the second purification shell, the liquid catheter, the first purification shell, the air guide pipe and the connecting pipe, it is convenient for p-fluorobenzaldehyde to purify the tail gas during the chlorination process, and the tail gas is directly sent to the External discharge will cause pollution to the environment. By setting the second stirring plate, fixed rod, rotating tube, first driving bevel gear and second driving bevel gear, the device can simultaneously stir the reaction solution in multiple directions to improve the mixing effect.

Description

A kind of p-fluorobenzaldehyde chlorination device and processing method thereof

technical field

The invention belongs to the technical field of p-fluorobenzaldehyde, and in particular relates to a p-fluorobenzaldehyde chlorination device and a processing method thereof.

Background technique

4-Fluorobenzaldehyde is an important fine chemical intermediate, which is used as the main raw material for the synthesis of various pesticides, medicines, surfactants, polymer monomers, and fungicides. For example, it is used in the synthesis of antihypertensive drugs, antipyretic, analgesic and anti-inflammatory drugs in medicine, in the synthesis of cyfluthrin and flufluthrin in pesticides, and in the synthesis of intermediates m-phenoxy-p-fluorobenzaldehyde, of which p- Fluorostyrene can be widely used in the manufacture of recording materials, thermoplastic resin coatings, liquid crystal materials, etc. During the production process of p-fluorobenzaldehyde, chlorination is carried out by passing p-fluorotoluene, benzoyl peroxide, and chlorine gas into the reactor reaction.

During the use of the existing reactor for the chlorination of p-fluorobenzaldehyde, the structure of the reactor is relatively simple, and the tail gas that pollutes the environment will be produced during the chlorination reaction, such as chlorine and hydrogen chloride, and it is necessary to purify these polluting gases in addition. emissions, and many processing steps, it is not convenient to directly purify the tail gas after the chlorination reaction. In addition, during the chlorination reaction process, the stirring of the reaction solution can only be directed in one direction, which is not conducive to the multi-directional flow of the reaction solution and improves the efficiency of the reaction solution. The mixing efficiency, for this reason we propose a kind of p-fluorobenzaldehyde chlorination device and processing method thereof.

Contents of the invention

The object of the present invention is to provide a kind of p-fluorobenzaldehyde chlorination device and processing method thereof, to solve the problem proposed in the above-mentioned background technology.

In order to achieve the above object, the present invention provides following technical scheme: a kind of p-Fluorobenzaldehyde chlorination device, comprises reaction tank body, described reaction tank body is provided with motor, and described motor lower end is connected with stirring shaft by reduction box, so The side wall of the stirring shaft is provided with a first stirring plate, the outer wall of the reaction tank is provided with a tail gas purification mechanism for chlorine gas treatment during the chlorination reaction, and the bottom end of the inner side of the reaction tank is provided with a device for making the reaction liquid go up and down. Movement of the second stirring mechanism;

The exhaust gas purification mechanism includes a second purification housing, a liquid catheter, a first purification housing, an air guide pipe and a communication pipe, and the first purification housing and the second purification housing are distributed around the circumference of the reaction tank, The top of the first purification shell is provided with an air duct for leading out the exhaust gas inside the reaction tank, the air duct runs through the first purification shell and extends to the inside of the first purification shell, and the side wall of the air duct passes The branch pipe is connected with an air outlet, and the inner top of the first purification shell is fixed with a catheter, and the lower surface of the catheter is provided with at least one liquid injection port, and the purification solution is sprayed through the liquid injection port to meet the air outlet. The outflowing tail gas is purified, one end of the guide tube penetrates the side wall of the first purification housing to form a liquid inlet, the other end of the guide tube penetrates the second purification housing and communicates with the inside of the second purification housing, The communication pipe is fixed between the first purification housing and the second purification housing.

Preferably, the second stirring mechanism includes a second stirring plate, a fixed rod, a rotating tube, a first transmission bevel and a second transmission bevel, the fixed rod is fixed on the inside of the reaction tank, and the outside of the fixed rod rotates A rotating tube is provided, one end of the rotating tube is fixed with a second transmission bevel, the lower end of the stirring shaft is fixed with a first transmission bevel, and the first transmission bevel is meshed with the second transmission bevel to drive the rotation The tube rotates, and a second stirring plate for stirring the reaction solution is fixed on the outer wall of the rotating tube.

Preferably, the second stirring plate is in an "L" shape, and a groove is opened on a side wall of the second stirring plate.

Preferably, two rotating tubes are arranged symmetrically along the center of the long side of the fixed rod, and four second stirring plates are arranged.

Preferably, a control valve is sheathed on the outside of the airway.

Preferably, the side wall of the second purification housing is provided with a sewage outlet, and the top of the second purification housing is provided with an exhaust pipe, and the exhaust pipe communicates with the inside of the second purification housing.

Preferably, the number of the liquid injection ports is greater than that of the air outlets, and the height of the communication pipe is lower than the liquid injection ports.

Preferably, the first stirring plate is an inclined structure, and a plurality of the first stirring plates are equidistantly arranged along the height direction of the stirring shaft.

Preferably, the lower surface of the reaction tank is provided with a liquid outlet, and the top of the reaction tank is provided with a feed port.

A kind of processing method of p-fluorobenzaldehyde chlorination device, comprises the steps:

a. Make p-fluorotoluene enter the inner side of the reaction tank through the feed port, then add benzoyl peroxide to the inner side of the reaction tank, feed chlorine gas to carry out the chlorination reaction, and the motor drives the first stirring plate to move through the stirring shaft , stirring the reaction solution;

b. The movement of the stirring shaft drives the two rotating tubes to rotate through the cooperation of the first transmission bevel gear and the second transmission bevel gear. The rotation tube drives the second stirring plate to move, and the second stirring plate moves to drive the reaction liquid at the inner bottom of the reaction tank upward. sports;

c. The movement of the second stirring plate drives more reaction liquid through the groove, the rotation of the two rotating tubes is opposite, and the rotation of the stirring shaft and the two rotating tubes is different, so that the reaction liquid moves in different directions to fully stir and mix;

d. Open the control valve after the reaction, and the tail gas after the reaction inside the reaction tank flows into the inside of the first purification shell through the air guide pipe, and flows out to the inside of the first purification shell through multiple gas outlets;

e. The catheter is connected to the lye pipeline through the liquid inlet, so that the lye flows into the first purification shell and the inside of the second purification shell respectively through the catheter, and the lye is dispersed through the liquid spray port, and the lye moves downward , the tail gas moves upward, and the two fully contact and react;

f. Excessive lye absorbs and purifies the tail gas, and the purified lye is discharged to the outside through the sewage outlet.

Compared with prior art, the beneficial effect of the present invention is:

(1) By setting up the second purification shell, the liquid catheter, the first purification shell, the air guide pipe and the connecting pipe, it is convenient to purify the tail gas during the chlorination reaction of p-fluorobenzaldehyde, and the tail gas is directly sent to the External discharge will cause pollution to the environment, and the additional purification process is cumbersome to operate. The device can conveniently purify the tail gas immediately after the reaction, which reduces the inconvenience of additional purification, is easy to operate, and improves the use effect of the device.

(2) By setting the second stirring plate, the fixed rod, the rotating tube, the first transmission bevel and the second transmission bevel, it is avoided that p-fluorobenzaldehyde can only face one direction when stirring the reaction solution during the chlorination reaction , the device can stir the reaction liquid in multiple directions at the same time to improve the mixing effect. The device is conducive to moving the reaction liquid at the inner bottom of the reaction tank upwards, reducing the situation of high-density materials sinking to the bottom, and increasing the practicability of the device.

Description of drawings

Fig. 1 is a structural representation of the present invention;

Fig. 2 is a schematic view of the sewage outlet structure of the present invention;

Fig. 3 is the front view structure schematic diagram of the present invention;

Fig. 4 is the schematic diagram of the sectional structure of the reaction tank body of the present invention;

Fig. 5 is a schematic cross-sectional structure diagram at A of Fig. 3 of the present invention;

Fig. 6 is the schematic diagram of enlarged structure at B place of Fig. 4 of the present invention;

Fig. 7 is the structural representation of the second stirring plate of the present invention;

In the figure: 1. Reaction tank body; 2. Second purification shell; 3. Liquid catheter; 4. Feed port; 5. Motor; 6. Air guide tube; 7. Control valve; 8. First purification shell 9, exhaust pipe; 10, sewage outlet; 11, liquid outlet; 12, connecting pipe; 13, stirring shaft; 14, second stirring plate; 15, fixed rod; 16, rotating pipe; 17, air outlet; 18. Liquid spray port; 19. First transmission bevel gear; 20. Second transmission bevel gear; 21. Groove; 22. First stirring plate.

detailed description

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

Please refer to Fig. 1-Fig. 7, the present invention provides a kind of technical scheme: a kind of p-fluorobenzaldehyde chlorination device, comprises reaction tank body 1, is provided with motor 5 on reaction tank body 1, and motor 5 lower end is connected with Stirring shaft 13, the side wall of stirring shaft 13 is provided with a first stirring plate 22, the outer wall of reaction tank body 1 is provided with a tail gas purification mechanism for chlorine gas treatment during chlorination reaction, and the inner bottom end of reaction tank body 1 is provided with a device for making the reaction The second stirring mechanism for the liquid to move up and down;

The exhaust gas purification mechanism includes a second purification housing 2, a liquid guide tube 3, a first purification housing 8, an air guide tube 6, and a communication pipe 12. Distributed to the surrounding area to facilitate better purification area, the top of the first purification shell 8 is provided with an air guide pipe 6 for leading out the exhaust gas inside the reaction tank 1, the air guide pipe 6 runs through the first purification shell 8 and leads to the first purification shell The inner side of the body 8 extends to facilitate the exhaust gas inside the reaction tank body 1 to flow to the inner side of the first purification shell 8, and the side wall of the air guide pipe 6 is connected with an air outlet 17 through a branch pipe to facilitate dispersion of the exhaust gas. The first purification shell 8 The inner top is fixed with a catheter 3, and the lower surface of the catheter 3 is provided with at least one liquid jet 18, and the purification solution is sprayed out through the liquid jet 18 to purify the tail gas flowing out of the air outlet 17, so as to facilitate better Disperse the purification solution, make the purification solution contact with the exhaust gas, and purify it. One end of the catheter 3 runs through the side wall of the first purification shell 8 to form a liquid inlet, and the other end of the catheter 3 runs through the second purification shell. body 2 and communicates with the inside of the second purification housing 2, and the communication pipe 12 is fixed between the first purification housing 8 and the second purification housing 2, so as to facilitate the connection between the first purification housing 8 and the second purification housing 2 The exhaust gas and the purification solution are circulated between them.

Preferably, the second stirring mechanism includes a second stirring plate 14, a fixed rod 15, a rotating tube 16, a first transmission bevel gear 19 and a second transmission bevel gear 20, the fixed rod 15 is fixed on the inner side of the reaction tank body 1, and the fixed rod 15 A rotating pipe 16 is arranged on the outer side, and the second driving bevel gear 20 is fixed on one end of the rotating pipe 16, and the first driving bevel gear 19 is fixed on the lower end of the stirring shaft 13, and the first driving bevel gear 19 is engaged with the second driving bevel gear 20 To drive the rotating tube 16 to rotate, the outer wall of the rotating tube 16 is fixed with a second stirring plate 14 for stirring the reaction solution, so as to better stir the reaction solution, make the reaction solution move in different directions, and improve the mixing effect.

Preferably, the second stirring plate 14 has an "L" shape, and a groove 21 is formed on a side wall of the second stirring plate 14, so as to drive more reaction liquid.

Preferably, two rotating tubes 16 are arranged symmetrically along the center of the long side of the fixed rod 15 , and four second stirring plates 14 are arranged.

Preferably, a control valve 7 is sheathed on the outside of the air duct 6 to facilitate the control of the flow of exhaust gas.

Preferably, the side wall of the second purification housing 2 is provided with a sewage outlet 10, which is convenient to discharge the purification solution absorbing tail gas, and the top of the second purification housing 2 is provided with an exhaust pipe 9, which is connected with the second purification The shell 2 communicates internally.

Preferably, the number of liquid injection ports 18 is greater than the number of gas outlets 17, and the connecting pipe 12 is lower than the height of the liquid injection ports 18, so as to reduce the contact between the purification solution absorbing exhaust gas and the liquid injection ports 18.

Preferably, the first stirring plate 22 has an inclined structure, and multiple first stirring plates 22 are equidistantly arranged along the height direction of the stirring shaft 13 for better stirring effect.

Preferably, the lower surface of the reaction tank body 1 is provided with a lower liquid port 11 to facilitate the discharge of the reacted reaction liquid, and the top of the reaction tank body 1 is provided with a feed port 4 .

A kind of processing method of p-fluorobenzaldehyde chlorination device, comprises the steps:

a. Make p-fluorotoluene enter the inner side of the reaction tank body 1 through the feed port 4, then add benzoyl peroxide to the inner side of the reaction tank body 1, feed chlorine gas, and carry out the chlorination reaction, and the motor 5 is driven by the stirring shaft 13 The first stirring plate 22 moves to stir the reaction solution;

b. The movement of the stirring shaft 13 drives the two rotating tubes 16 to rotate through the cooperation of the first transmission bevel gear 19 and the second transmission bevel gear 20, and the rotation tube 16 drives the second stirring plate 14 to move, and the second stirring plate 14 moves to drive the reaction tank The reaction liquid at the inner bottom of body 1 moves upward;

c, the movement of the second stirring plate 14 drives more reaction solution through the groove 21, the turning of the two rotating tubes 16 is opposite, the turning of the stirring shaft 13 and the turning of the two rotating tubes 16 is different, so that the reaction solution moves towards different directions, and the Mix thoroughly;

d, open the control valve 7 after the reaction, the tail gas after the reaction inside the reaction tank body 1 flows into the inside of the first purification housing 8 through the air guide pipe 6, and flows out to the inside of the first purification housing 8 through a plurality of gas outlets 17;

e, catheter 3 is externally connected to the lye pipeline through the liquid inlet, so that lye flows into the inside of the first purification housing 8 and the second purification housing 2 through the catheter 3, and the lye is dispersed through the liquid injection port 18, The lye moves downward, the tail gas moves upward, and the two fully contact and react;

f. Excessive lye absorbs and purifies the tail gas, and the purified lye is discharged to the outside through the sewage outlet 10 .

Although the embodiments of the present invention have been shown and described, those skilled in the art can understand that various changes, modifications and substitutions can be made to these embodiments without departing from the principle and spirit of the present invention. and modifications, the scope of the invention is defined by the appended claims and their equivalents.

Claims (10)

1. The utility model provides a p-fluorobenzaldehyde chlorination device, includes the retort body (1), be provided with motor (5) on the retort body (1), motor (5) lower extreme is connected with (mixing) shaft (13) through the reducing gear box, (mixing) shaft (13) lateral wall is provided with first stirring board (22), its characterized in that: the outer wall of the reaction tank body (1) is provided with a tail gas purification mechanism for treating chlorine during chlorination reaction, and the bottom end of the inner side of the reaction tank body (1) is provided with a second stirring mechanism for enabling reaction liquid to move up and down;

the tail gas purification mechanism comprises a second purification shell (2), a liquid guide pipe (3), a first purification shell (8), a gas guide pipe (6) and a communicating pipe (12), wherein the first purification shell (8) and the second purification shell (2) are distributed in a circumferential surrounding mode along a reaction tank body (1), the top end of the first purification shell (8) is provided with the gas guide pipe (6) used for guiding tail gas out of the inner side of the reaction tank body (1), the gas guide pipe (6) penetrates through the first purification shell (8) and extends towards the inner side of the first purification shell (8), one side wall of the gas guide pipe (6) is connected with a gas outlet (17) through a branch pipe, the liquid guide pipe (3) is fixed at the top end of the inner side of the first purification shell (8), the lower surface of the liquid guide pipe (3) is provided with at least one liquid spraying port (18), purification solution is sprayed out through the liquid spraying port (18) so as to purify tail gas flowing out of the gas outlet (17), one end of the first purification shell (3) penetrates through one side wall of the first purification shell (8) to form a liquid guide pipe (3), the other end of the second purification shell (2) and is communicated with the second purification shell (12).

2. The p-fluorobenzaldehyde chlorinating device according to claim 1, wherein: second rabbling mechanism includes second stirring board (14), dead lever (15), rotating tube (16), first transmission awl tooth (19) and second transmission awl tooth (20), dead lever (15) are fixed in the retort body (1) inboard, dead lever (15) outside is rotated and is provided with rotating tube (16), rotating tube (16) one end is fixed with second transmission awl tooth (20), (mixing) shaft (13) lower extreme is fixed with first transmission awl tooth (19), just first transmission awl tooth (19) are connected in order to drive rotating tube (16) to rotate with second transmission awl tooth (20) meshing, rotating tube (16) outer wall is fixed with second stirring board (14) that are used for the reaction liquid stirring.

3. The p-fluorobenzaldehyde chlorinating device according to claim 2, wherein: the second stirring plate (14) is L-shaped, and a groove (21) is formed in one side wall of the second stirring plate (14).

4. The p-fluorobenzaldehyde chlorinating device according to claim 2, wherein: the rotating pipe (16) is symmetrically provided with two positions along the center of the long side of the fixing rod (15), and the number of the second stirring plates (14) is four.

5. The p-fluorobenzaldehyde chlorinating device according to claim 1, wherein: the outer side of the air duct (6) is sleeved with a control valve (7).

6. The p-fluorobenzaldehyde chlorinating device according to claim 1, wherein: a sewage draining outlet (10) is formed in one side wall of the second purifying shell (2), an exhaust pipe (9) is arranged at the top end of the second purifying shell (2), and the exhaust pipe (9) is communicated with the interior of the second purifying shell (2).

7. The p-fluorobenzaldehyde chlorinating device according to claim 1, wherein: the number of the liquid spraying openings (18) is larger than that of the air outlets (17), and the communicating pipe (12) is lower than the height of the liquid spraying openings (18).

8. The p-fluorobenzaldehyde chlorinating device according to claim 1, wherein: first stirring board (22) are the inclined structure, first stirring board (22) are provided with a plurality ofly along (mixing) shaft (13) direction of height equidistance.

9. The p-fluorobenzaldehyde chlorinating device according to claim 1, wherein: the lower surface of the reaction tank body (1) is provided with a liquid outlet (11), and the top end of the reaction tank body (1) is provided with a feeding hole (4).

10. The processing method of a p-fluorobenzaldehyde chlorination plant according to any one of claims 1 to 9, wherein the processing method comprises the following steps: the method comprises the following steps:

a. allowing the p-fluorotoluene to enter the inner side of the reaction tank body (1) through the feed inlet (4), then adding benzoyl peroxide into the inner side of the reaction tank body (1), introducing chlorine, carrying out chlorination reaction, and driving a first stirring plate (22) to move by a motor (5) through a stirring shaft (13) to stir reaction liquid;

b. the stirring shaft (13) moves to drive the two rotating pipes (16) to rotate through the matching of the first transmission bevel gear (19) and the second transmission bevel gear (20), the rotating pipes (16) drive the second stirring plate (14) to move, and the second stirring plate (14) moves to drive the reaction liquid at the bottom end of the inner side of the reaction tank body (1) to move upwards;

c. the second stirring plate (14) moves to drive more reaction liquid through the groove (21), the rotation directions of the two rotating pipes (16) are opposite, and the rotation directions of the stirring shaft (13) and the two rotating pipes (16) are different, so that the reaction liquid moves towards different directions to be fully stirred and uniformly mixed;

d. after the reaction, the control valve (7) is opened, tail gas after the reaction at the inner side of the reaction tank body (1) flows into the inner side of the first purification shell (8) through the gas guide pipe (6) and flows out of the inner side of the first purification shell (8) through the plurality of gas outlets (17);

e. the liquid guide pipe (3) is externally connected with an alkali liquor pipeline through the liquid inlet, so that the alkali liquor flows into the inner sides of the first purifying shell (8) and the second purifying shell (2) through the liquid guide pipe (3) respectively, the alkali liquor is dispersed through the liquid spraying port (18), the alkali liquor moves downwards, the tail gas moves upwards, and the alkali liquor and the tail gas are in full contact reaction;

f. excessive alkali liquor absorbs and purifies the tail gas, and the purified alkali liquor is discharged outwards through a sewage outlet (10).

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