Chlorinated benzene production process

Abstract

The invention belongs to the technical field of chlorobenzene production. The invention discloses a chlorobenzene production process which comprises the following steps: treating benzene and chlorine, respectively conveying the benzene and the chlorine into a chlorinator, carrying out chlorination reaction under the action of a catalyst, cooling the chlorinator in the reaction process, and separating the product by adopting a separator, and carrying out dehydration treatment on the separated chlorobenzene to obtain the chlorobenzene. In the reaction process, mixed materials at the lower part and the middle upper part of the chlorinator are pumped out to the outside for forced cooling, and then the cooled mixed materials are returned into the chlorinator, so that the heat removal speed of the chlorination reaction can be greatly increased, and black materials can be avoided; and the specific separator is adopted to separate chlorobenzene, so that by-products separated during separation and rectification can be rapidly cooled and discharged from the discharge pipe, the separation efficiency of the by-products in the rectification process can be improved, and the production efficiency of chlorobenzene can be improved.

Description

Technical Field

[0001] The invention belongs to the technical field of chlorobenzene production, and in particular relates to a chlorobenzene production process. Background Art

[0002] Chlorobenzene is an organic compound with the chemical formula C6H5Cl. It is a colorless, transparent liquid with a bitter almond flavor. It is insoluble in water but soluble in most organic solvents such as ethanol, ether, chloroform, carbon disulfide, and benzene. It is mainly used as an intermediate in dyes, medicines, pesticides, and organic synthesis. It can also be used as a solvent and a reference for gas chromatography.

[0003] The chlorination of pure benzene to produce monochlorobenzene is an exothermic reaction. The heat released by the reaction will cause the material temperature to rise continuously and the reaction speed to accelerate. The more reaction heat released per unit time, the faster the material temperature will rise. Therefore, in order to keep the material constant at a certain reaction temperature, the reaction heat must be removed in time during the chlorination of pure benzene. The speed of removing the reaction heat determines the production capacity of the chlorination reaction equipment.

[0004] The method of removing the reaction heat in the existing process is: during the reaction, the generated hydrogen chloride gas and part of the benzene vapor vaporized by the reaction heat are discharged from the top of the chlorinator, cooled by the tail gas system, and the cooled benzene is returned to the chlorinator to continue to participate in the reaction. The cooled hydrogen chloride is sent to the hydrochloric acid absorption system, and the heat is removed by the vaporization of the raw benzene, so that the reaction temperature in the chlorinator is maintained at about 80°C (the vaporization temperature of pure benzene).

[0005] The existing method of removing the reaction heat has the following disadvantages: since the chlorination reaction heat is taken away by the gasification of the raw materials, it is controlled by the gas phase rising cross section of the chlorinator equipment, and the natural flow is used to push the materials up, so the rising and removal speed of the raw materials and the materials after the reaction is slow, and the speed of removing the reaction heat is also slow. The method is passive, which easily causes the local reaction heat in the chlorinator to be released untimely, the local temperature is prone to rise sharply, and the black material phenomenon often occurs, so that the amount of chlorine consumed by the reaction is limited, and the production capacity of the equipment is greatly limited; the reaction heat is balanced by adding a large excess of raw material benzene through gasification, and a large amount of cold energy is consumed to condense the gas phase benzene. At the same time, the raw material benzene cooled by the tail gas system needs to flow back to the chlorinator naturally to continue to participate in the reaction. The condenser must be arranged at a high position, thereby increasing the transmission pressure and cold energy of the circulating water and the refrigerated brine, and the energy consumption is large.

[0006] Moreover, the chlorobenzene obtained after preliminary separation may still contain a small amount of impurities and needs to be further refined. Generally, it can be refined by methods such as secondary distillation, crystallization, washing, etc. to improve the purity of chlorobenzene, but the separation equipment used is not good, resulting in poor purification effect, making the purity of the prepared chlorobenzene insufficient, affecting the quality. Summary of the invention

[0007] The purpose of the present invention is to overcome the problems existing in the prior art and provide a chlorobenzene production process.

[0008] The purpose of the present invention and the solution to the technical problem are achieved by adopting the following technical solutions.

[0009] One aspect of the present invention provides a chlorinated benzene production process, comprising the following steps:

[0010] S1: Raw material preparation: treating benzene and chlorine;

[0011] S2: Chlorination reaction: Benzene and chlorine are transported to the chlorinator respectively, and the chlorination reaction is carried out under the action of the catalyst, and the chlorinator is cooled during the reaction;

[0012] S3: separation of chlorinated products: separation of the products using a separator;

[0013] S4: Purification: Dehydrating the separated chlorobenzene to obtain chlorobenzene.

[0014] Preferably, in step S1, the mass fraction of water in the treated benzene is less than 0.04%.

[0015] In any of the above schemes, preferably, in step S1, the mass fraction of water in the treated chlorine gas is less than 0.04%.

[0016] In any of the above schemes, preferably, in step S2, the catalyst is ferric chloride, and the amount of ferric chloride dissolved in benzene is 0.007% to 0.009% (mass fraction).

[0017] Preferably in any of the above schemes, in step S2, the catalyst is an iron ring arranged in the chlorinator.

[0018] In any of the above schemes, preferably, in step S2, the benzene feed amount is 2.0-2.5m 3 / h, chlorine feed rate 200-250m 3 / h.

[0019] Preferably in any of the above schemes, in step S2, two circulating coolers are externally installed at the lower part of the chlorinator.

[0020] Preferably in any of the above schemes, in step S2, a condenser is provided on the top of the chlorinator.

[0021] In any of the above schemes, preferably, in step S4, chlorobenzene is filtered through a filter to remove impurities therein, and then the chlorobenzene is contacted with a desiccant to make it absorb water, and then a dehydration treatment is performed.

[0022] During the reaction process, the mixed materials in the lower and middle upper parts of the chlorinator are extracted to the outside for forced cooling, and then the cooled mixed materials are returned to the chlorinator, which can greatly improve the heat removal rate of the chlorination reaction. Under the premise of not changing the original chlorinator equipment, the chlorine consumption depth is increased, and the production capacity of the equipment for producing monochlorobenzene is improved while maximizing the control of dichlorobenzene formation. In addition, the circulating cooler equipment can be arranged at a low position, which reduces the conveying pressure of circulating water and chilled brine and reduces energy consumption. At the same time, due to the large circulation volume, the materials are mixed evenly and the discharge is rapid. There will be no untimely release of local reaction heat in the chlorinator, which can avoid black materials.

[0023] In step S3, the separator includes: a separation kettle body, a heating chamber and a cooling chamber are arranged in the separation kettle body, three heating pipes are arranged in the heating chamber, a feed pipe connected to one end of each of the three heating pipes is arranged on the side wall of the separation kettle body, a connecting ring is arranged at the other ends of the three heating pipes, the top end of the connecting ring extends to the cooling chamber and is connected to a condensing pipe, and a discharge pipe connected to the bottom end of the condensing pipe is also arranged on the side wall of the separation kettle body;

[0024] The heating chamber is filled with heat transfer liquid, the cooling chamber is filled with condensate, a mixing component is arranged in the separation kettle body, and the mixing component comprises a transmission shaft rotatably mounted in the cooling chamber, the transmission shaft, a cylindrical disk is sleeved on the top end of the transmission shaft, stirring blades are symmetrically fixedly mounted on the side wall of the cylindrical disk, a plurality of paddles are evenly fixedly mounted on the inner side of the stirring blade, the bottom end of the transmission shaft extends into the heating chamber and is fixedly connected to a reciprocating screw rod, a movable ring is sleeved on the outer side of the reciprocating screw rod, a connecting frame is fixedly connected to the outer side of the movable ring, and a plurality of connecting plates are evenly fixedly mounted on the connecting frame.

[0025] Preferably, a heater is provided at the bottom end of the separation kettle body, a motor is fixedly installed at the top end of the separation kettle body, and an output end of the motor is fixedly connected to a transmission shaft.

[0026] Preferably, a water inlet pipe and a water outlet pipe connected to the cooling chamber are arranged on the side wall of the separation kettle body, the water inlet pipe is located below the water outlet pipe, and a throttle valve is arranged on the water inlet pipe.

[0027] Preferably, slide grooves are symmetrically provided on the inner wall of the heating chamber, and sliding blocks adapted to the slide grooves are fixedly mounted on the connecting plate.

[0028] Preferably, a PLC controller is also provided on the separation kettle body, and the PLC controller is electrically connected to the motor, the throttle valve and the heater.

[0029] Preferably, a threaded hole adapted to the reciprocating screw is provided at the center of the movable ring, and the horizontal angle of the connecting plate is 45°.

[0030] Through the above scheme, when in use, the PLC controller can control the motor to power on and work, at this time the motor can drive the transmission shaft to rotate in the cooling cabin and the heating cabin, at this time the reciprocating screw at the bottom end of the transmission shaft can rotate in the heating cabin, at this time the threaded hole at the center of the movable ring cooperates with the reciprocating screw to enable the connecting frame to slide up and down along the slide groove in the heating cabin, at this time the connecting plate drives the heat transfer fluid heated by the heater in the heating cabin to surge up and down during the up and down movement, so that the reaction liquid in the heating tube can be heated evenly, the heating efficiency can be guaranteed, and the connecting plate set at a 45° angle can reduce the contact between it and the heat transfer fluid. The area can reduce the resistance encountered by the connecting plate during movement, reduce the load of the motor, make the temperature distribution of the heat transfer fluid uniform, improve the heating effect, and by changing the power of the heater, the temperature of the heat transfer fluid can be gradually increased, and the components with different boiling points in the by-product can be separated, which is beneficial to the separation of the by-products. In the process of rotation of the transmission shaft, the cylindrical disk can rotate at the same time. At this time, the paddle in the stirring blade can drive the cold water in the cooling cabin to quickly contact the condenser, so that the by-products separated during separation and distillation can be quickly cooled and discharged from the discharge pipe, which can improve the efficiency of by-product separation in the distillation process.

[0031] Preferably, a slide rail is fixedly installed on the top wall of the cooling chamber, and the cylindrical disk is slidably installed on the slide rail. The cylindrical disk is located above the water outlet pipe, and a limit assembly is also provided on the transmission shaft. The limit assembly includes a movable hole opened on the side wall of the transmission shaft, and a limit pin is slidably installed in the movable hole. An electromagnet electrically connected to the PLC controller is also fixedly installed on the side wall of the movable hole, and the limit pin is made of metal that matches the electromagnet.

[0032] Preferably, a limiting groove matched with the limiting pin is opened at the center of the cylindrical disk, and a spring is arranged between the limiting pin and the movable hole.

[0033] Through the above scheme, the power-on state of the electromagnet can be controlled by the PLC controller. When the electromagnet is energized, the electromagnet can push the limit pin to slide outward, and the limit pin can be embedded in the limit groove. At this time, the transmission shaft is fixedly connected to the cylindrical disk. At this time, the rotation of the transmission shaft can drive the cylindrical disk to rotate. At this time, the stirring blades and the paddles on the cylindrical disk can rotate synchronously, which can facilitate the stirring of the condensed water. Moreover, since the cylindrical disk is located above the water outlet pipe, the condensed water can be prevented from entering the movable hole, and the normal use of the electromagnet can be guaranteed. When the electromagnet is powered off, the spring can squeeze the limit pin, and the limit pin can be retracted into the movable hole, so that the transmission shaft and the cylindrical disk can be separated from each other, and the transmission shaft can rotate freely in the cylindrical disk. By controlling the power-on state of the electromagnet, it is possible to selectively adjust whether the transmission shaft and the cylindrical disk are fixed, and only the connecting plate can be driven to slide up and down during the initial heating process of separation, which can reduce the load on the output end of the motor and increase the service life of the motor.

[0034] By means of the above technical solution, the present invention has at least the following advantages:

[0035] 1. In the process of reaction, the present invention extracts the mixed material in the lower part and the middle and upper part of the chlorinator to the outside for forced cooling, and then returns the cooled mixed material to the chlorinator. Such operation can greatly improve the heat removal speed of the chlorination reaction, avoid the occurrence of black material, avoid the waste of raw materials, and make the raw materials react more fully, so that more products can be prepared from the same raw materials without waste, thereby improving the preparation yield and reducing the production cost. In addition, the circulating cooler can be arranged at a low position, reducing the conveying pressure of circulating water and refrigerated brine, and reducing energy consumption;

[0036] 2. The present invention generates chlorobenzene and reaction by-products after the reaction, so a separator is used to separate them, so that the purity of the chlorobenzene obtained is higher, and the motor in the separator can drive the transmission shaft to rotate in the cooling chamber and the heating chamber, and the reciprocating screw at the bottom end of the transmission shaft can rotate in the heating chamber. At this time, the threaded hole at the center of the movable ring cooperates with the reciprocating screw to enable the connecting frame to slide up and down along the slide groove in the heating chamber. At this time, the connecting plate drives the heat transfer liquid heated by the heater in the heating chamber to surge up and down during the up and down movement, so that the reaction liquid in the heating tube can be heated evenly, and the heating efficiency can be guaranteed. The connecting plate set at an angle of 45° can reduce the contact area between it and the heat transfer liquid, which can reduce the connection The resistance encountered by the plate during movement can reduce the load of the motor, make the temperature distribution of the heat transfer fluid uniform, and improve the heating effect. By changing the power of the heater, the temperature of the heat transfer fluid can be gradually increased, and components with different boiling points in the by-product can be separated, which is beneficial to the separation of the by-products. In the process of rotation of the transmission shaft, the cylindrical disk can rotate at the same time. At this time, the paddles in the stirring blades can drive the cold water in the cooling cabin to quickly contact the condenser tube, so that the by-products separated during separation and distillation can be quickly cooled and discharged from the discharge pipe. In this way, the by-products can be separated more thoroughly, and purer chlorobenzene can be obtained. The efficiency of by-product separation in the distillation process can be improved, and the production efficiency of chlorobenzene can be further improved.

[0037] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the preferred embodiments of the present invention are described in detail as follows. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 This is a schematic diagram of the overall structure of a separator for producing chlorinated benzene according to an embodiment of the present invention;

[0039] Figure 2 It is a schematic diagram of the front cross-sectional structure of the separation kettle body in an embodiment of the present invention;

[0040] Figure 3 This is a schematic diagram of the combined structure of the heating tube and the condensing tube in an embodiment of the present invention;

[0041] Figure 4 This is a schematic diagram of the structure of the output end of the motor in an embodiment of the present invention;

[0042] Figure 5 It is a schematic diagram of the structure on the connecting frame in an embodiment of the present invention;

[0043] Figure 6 for Figure 2 A is an enlarged view of the middle image.

[0044] In the figure: 1. separation kettle body; 2. motor; 3. water outlet pipe; 4. water inlet pipe; 5. throttle valve; 6. feed pipe; 7. electromagnet; 8. PLC controller; 9. discharge pipe; 10. cooling chamber; 11. slide; 12. heating pipe; 13. heater; 14. heating chamber; 15. condenser; 16. transmission shaft; 17. cylindrical plate; 18. slide rail; 19. connecting ring; 20. stirring blade; 21. paddle; 22. reciprocating screw rod; 23. connecting frame; 24. connecting plate; 25. movable ring; 26. threaded hole; 27. slider; 28. limit pin; 29. ​​limit groove; 30. spring; 31. movable hole; 32. through hole. DETAILED DESCRIPTION

[0045] In order to make the technical means, creative features, objectives and effects of the present invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0046] Embodiment 1:

[0047] A chlorinated benzene production process comprises the following steps:

[0048] S1: Raw material preparation: Benzene and chlorine are treated, and the water content in the treated benzene is less than 0.04%, and the water content in the chlorine is less than 0.04%. Ferric chloride is very soluble in water. When the water content in benzene is higher than 0.2%, the chlorination reaction cannot proceed normally. The ferric chloride dissolved in benzene is extracted by water (ferric chloride will not be hydrolyzed to form ferric hydroxide in acidic chlorination solution), which reduces the amount of ferric chloride dissolved in benzene, greatly reduces the chlorination reaction speed, and causes the chlorination reaction to not proceed normally. At the same time, the water content in benzene is an important factor leading to explosion during the chlorination reaction, so the water content in benzene and chlorine must be strictly controlled;

[0049] S2: Chlorination reaction: Benzene and chlorine are mixed with benzene at a rate of 2.0-2.5m 3 / h, chlorine feed rate 200-250m 3 / h are respectively transported to the chlorinator, and chlorination reaction is carried out under the action of a catalyst, the catalyst is ferric chloride, and the dissolution amount of ferric chloride in benzene is 0.007% to 0.009% (mass fraction). When the dissolution amount is lower than 0.006%, the chlorination reaction is difficult to carry out; when the dissolution amount reaches 0.01%, it is sufficient to meet the needs of the chlorination reaction. If it is higher than 0.01%, not only the yield of chlorobenzene cannot be increased, but also the content of by-products such as polychlorides in the chlorinated liquid will be greatly increased. Therefore, the amount of ferric chloride should be strictly controlled. At the same time, the catalyst can also be an iron ring, which is arranged in the chlorinator. The iron ring generates ferric chloride in the chlorination tower under the action of chlorine and trace water in benzene. The generated ferric chloride is dissolved in the chlorinated liquid as an activator for the reaction. Promote the reaction of benzene and chlorine, strengthen the full contact between chlorine and benzene, promote the mass transfer and reaction heat transfer of the production process, and cool the chlorinator during the reaction. Two external circulating coolers are installed at the bottom of the chlorinator. The two circulating coolers correspond to two circulating pumps. When the temperature in the middle of the chlorinator is greater than 70°C and other indicators are normal, open the inlet and outlet valves of the external first circulating pump and the second circulating pump. When the temperature in the middle of the chlorinator is lower than 70°C and the tail gas pressure is lower than 10kPa, start the first circulating pump, gradually increase its inverter frequency, open the circulating water valve of the first circulating cooler, keep the temperature in the chlorinator not lower than 50°C, and when the inverter of the first circulating pump is turned on to 30Hz, increase the chlorine feed rate by 10-20m each time. 3 / h, with a time interval of 10 to 20 minutes, while keeping the middle temperature of the chlorinator less than 70℃ and greater than 50℃, alternately increase the inverter frequency of the first circulation pump and the chlorine feed amount until the frequency of the first circulation pump reaches 50Hz; start the second circulation pump, gradually increase its inverter frequency, open the chilled brine valve of the second circulation cooler, and gradually open it to keep the temperature in the chlorinator not lower than 50℃. When the inverter of the second circulation pump is opened to 30Hz, gradually increase the chlorine feed amount, increasing it by 10 to 20m each time. 3 / h, with a time interval of 10 to 20 minutes, until the valve of the frozen brine of the second circulation cooler is opened to the maximum, and the frequency of the inverter of the second circulation pump and the chlorine feed amount are alternately increased while maintaining the temperature in the middle of the chlorinator less than 70°C and greater than 50°C, until the frequency of the second circulation pump is opened to 50Hz. Through the above operation process, the mixed materials in the upper and lower parts of the chlorinator can be extracted to the outside for forced cooling, and the cooled mixed materials are returned to the chlorinator to continue to participate in the reaction. During the reaction process, the forced cooling and return of the mixed materials are maintained to form a continuous cycle. Two condensers are set at the top of the chlorinator. The hydrogen chloride gas produced by the reaction of chlorine and benzene and part of the benzene vapor vaporized by the reaction heat are discharged from the top of the chlorinator, cooled by the first condenser and the second condenser, and the cooled benzene is returned to the chlorinator to continue to participate in the reaction;

[0050] S3: separation of chlorinated products: separation of the products using a separator;

[0051] S4: Purification: The separated chlorobenzene is filtered through a filter to remove impurities therein, and then the chlorobenzene is contacted with a desiccant to make it absorb water, and then dehydrated to obtain chlorobenzene.

[0052] Embodiment 2:

[0053] See also Figures 1 to 6 , a separator, comprising: a separation kettle body 1, a heating chamber 14 and a cooling chamber 10 are arranged in the separation kettle body 1, three heating tubes 12 are arranged in the heating chamber 14, a feed tube 6 connected to one end of each of the three heating tubes 12 is arranged on the side wall of the separation kettle body 1, a connecting ring 19 is arranged at the other end of the three heating tubes 12, a top end of the connecting ring 19 extends to the cooling chamber 10 and is connected to a condensing tube 15, and a discharge tube 9 connected to the bottom end of the condensing tube 15 is also arranged on the side wall of the separation kettle body 1;

[0054] The heating chamber 14 is filled with heat-conducting liquid, the cooling chamber 10 is filled with condensate, and a mixing component is arranged in the separation kettle body 1, which includes a transmission shaft 16 rotatably installed in the cooling chamber 10, the transmission shaft 16, the top end of the transmission shaft 16 is sleeved with a cylindrical disk 17, and stirring blades 20 are symmetrically fixedly installed on the side wall of the cylindrical disk 17, and a plurality of paddles 21 are evenly fixedly installed on the inner side of the stirring blade 20. The bottom end of the transmission shaft 16 extends into the heating chamber 14 and is fixedly connected to a reciprocating screw rod 22, and a movable ring 25 is sleeved on the outer side of the reciprocating screw rod 22, and a connecting frame 23 is fixedly connected to the outer side of the movable ring 25, and a plurality of connecting plates 24 are evenly fixedly installed on the connecting frame 23.

[0055] A heater 13 is provided at the bottom end of the separation kettle body 1 , and a motor 2 is fixedly installed at the top end of the separation kettle body 1 , and an output end of the motor 2 is fixedly connected to a transmission shaft 16 .

[0056] A water inlet pipe 4 and a water outlet pipe 3 connected to the cooling chamber 10 are arranged on the side wall of the separation kettle body 1. The water inlet pipe 4 is located below the water outlet pipe 3, and a throttle valve 5 is arranged on the water inlet pipe 4.

[0057] The inner wall of the heating chamber 14 is symmetrically provided with slide grooves 11 , and a sliding block 27 adapted to the slide grooves 11 is fixedly mounted on the connecting plate 24 .

[0058] The separation kettle body 1 is also provided with a PLC controller 8 , which is electrically connected to the motor 2 , the throttle valve 5 and the heater 13 .

[0059] A threaded hole 26 adapted to the reciprocating screw rod 22 is provided at the center of the movable ring 25, and the horizontal angle of the connecting plate 24 is 45°.

[0060] In this embodiment, the PLC controller 8 can control the motor 2 to be powered on, and the motor 2 can drive the transmission shaft 16 to rotate in the cooling chamber 10 and the heating chamber 14. At this time, the reciprocating screw 22 at the bottom end of the transmission shaft 16 can rotate in the heating chamber 14. At this time, the threaded hole 26 at the center of the movable ring 25 cooperates with the reciprocating screw 22 to enable the connecting frame 23 to slide up and down along the slide groove 11 in the heating chamber 14. At this time, the connecting plate 24 drives the heat transfer liquid heated by the heater 13 in the heating chamber 14 to surge up and down during the up and down movement, so that the reaction liquid in the heating tube 12 can be heated evenly, and the heating efficiency can be guaranteed. The connecting plate 24 set at a 45° angle can reduce its contact with the heat transfer liquid. The contact area between the liquids can reduce the resistance encountered by the connecting plate 24 during movement, reduce the load of the motor 2, make the temperature distribution of the heat transfer liquid uniform, improve the heating effect, and by changing the power of the heater 13, the temperature of the heat transfer liquid can be gradually increased, and the components with different boiling points in the by-products can be separated, which is beneficial to the separation of the by-products. In the process of rotation of the transmission shaft 16, the cylindrical disk 17 can rotate at the same time. At this time, the paddle 21 in the stirring blade 20 can drive the cold water in the cooling chamber 10 to quickly contact the condenser 15, so that the by-products separated during separation and distillation can be quickly cooled and discharged from the discharge pipe 9, which can improve the efficiency of by-product separation during the distillation process.

[0061] As an embodiment of the present invention, refer to Figure 2 , Figure 6 A separator for producing chlorobenzene, a slide rail 18 is fixedly installed on the top wall of the cooling chamber 10, a cylindrical disc 17 is slidably installed on the slide rail 18, the cylindrical disc 17 is located above the water outlet pipe 3, a limit assembly is also provided on the transmission shaft 16, the limit assembly includes a movable hole 31 opened on the side wall of the transmission shaft 16, a limit pin 28 is slidably installed in the movable hole 31, an electromagnet 7 electrically connected to a PLC controller 8 is also fixedly installed on the side wall of the movable hole 31, and the limit pin 28 is made of metal adapted to the electromagnet 7.

[0062] A through hole 32 is formed at the center of the cylindrical disk 17 . A limiting groove 29 matching the limiting pin 28 is formed on the inner wall of the through hole 32 . A spring 30 is provided between the limiting pin 28 and the movable hole 31 .

[0063] In this embodiment, during use, the power-on state of the electromagnet 7 can be controlled by the PLC controller 8. When the electromagnet 7 is powered on, the electromagnet 7 can push the limit pin 28 to slide outward, and the limit pin 28 can be embedded in the limit groove 29. At this time, the transmission shaft 16 is fixedly connected to the cylindrical disk 17. At this time, the rotation of the transmission shaft 16 can drive the cylindrical disk 17 to rotate. At this time, the stirring blade 20 and the paddle 21 on the cylindrical disk 17 can rotate synchronously, which can facilitate the stirring of the condensed water. In addition, since the cylindrical disk 17 is located above the water outlet pipe 3, the condensed water can be prevented from entering the movable hole. 31, which can ensure the normal use of the electromagnet 7. When the electromagnet 7 is powered off, the spring 30 can squeeze the limit pin 28, and the limit pin 28 can shrink into the movable hole 31, so that the transmission shaft 16 and the cylindrical disk 17 can be separated from each other, and the transmission shaft 16 can rotate freely in the cylindrical disk 17. By controlling the power-on state of the electromagnet 7, it is possible to selectively adjust whether the transmission shaft 16 and the cylindrical disk 17 are fixed, and only the connecting plate 24 can be driven to slide up and down during the initial heating process of separation, which can reduce the load on the output end of the motor 2 and increase the service life of the motor 2.

[0064] The separator is provided with a mixing component, and the motor can be controlled to work through the PLC controller. At this time, the motor can drive the transmission shaft to rotate in the cooling chamber and the heating chamber. At this time, the reciprocating screw at the bottom end of the transmission shaft can rotate in the heating chamber. At this time, the threaded hole at the center of the movable ring cooperates with the reciprocating screw to make the connecting frame slide up and down along the slide groove in the heating chamber. At this time, the connecting plate drives the heat transfer liquid heated by the heater in the heating chamber to surge up and down during the up and down movement, which can make the reaction liquid in the heating tube heated evenly and ensure the heating efficiency. The connecting plate set at a 45° angle can reduce the contact area between it and the heat transfer liquid, which can reduce The resistance encountered by the connecting plate during movement can reduce the load of the motor, make the temperature distribution of the heat transfer fluid uniform, and improve the heating effect. By changing the power of the heater, the temperature of the heat transfer fluid can be gradually increased, and components with different boiling points in the by-product can be separated, which is beneficial to the separation of the by-products. In the process of rotation of the transmission shaft, the cylindrical disk can rotate at the same time. At this time, the paddles in the stirring blades can drive the cold water in the cooling cabin to quickly contact the condenser tube, so that the by-products separated during separation and distillation can be quickly cooled and discharged from the discharge pipe, which can improve the efficiency of by-product separation in the distillation process and the production efficiency of chlorobenzene.

[0065] The separator is provided with a limit assembly, and the power-on state of the electromagnet can be controlled by a PLC controller. When the electromagnet is energized, the electromagnet can push the limit pin to slide outward, and the limit pin can be embedded in the limit groove. At this time, the transmission shaft is fixedly connected to the cylindrical disk, and the rotation of the transmission shaft can drive the cylindrical disk to rotate. At this time, the stirring blades and the paddles on the cylindrical disk can rotate synchronously, which can facilitate the stirring of the condensed water. Moreover, since the cylindrical disk is located above the water outlet pipe, the condensed water can be prevented from entering the movable hole, and the normal use of the electromagnet can be guaranteed. When the electromagnet is powered off, the spring can squeeze the limit pin, and the limit pin can be retracted into the movable hole, so that the transmission shaft and the cylindrical disk can be separated from each other, and the transmission shaft can rotate freely in the cylindrical disk. By controlling the power-on state of the electromagnet, it is possible to selectively adjust whether the transmission shaft and the cylindrical disk are fixed, and only the connecting plate can be driven to slide up and down during the initial heating process of separation, which can further reduce the load on the output end of the motor and increase the service life of the motor.

[0066] Working principle: First, the reacted chlorobenzene mixed liquid is injected into the heating tube 12 through the feed pipe 6 on the separation kettle body 1, and then the heat transfer liquid is heated by the heater 13. When in use, the motor 2 can be controlled by the PLC controller 8 to be powered on. At this time, the motor 2 can drive the transmission shaft 16 to rotate in the cooling chamber 10 and the heating chamber 14. At this time, the reciprocating screw rod 22 at the bottom end of the transmission shaft 16 can rotate in the heating chamber 14. At this time, the threaded hole 26 at the center of the movable ring 25 cooperates with the reciprocating screw rod 22 to enable the connecting frame 23 to slide up and down along the slide groove 11 in the heating chamber 14. At this time, the connecting plate 24 drives the heat transfer liquid heated by the heater 13 in the heating chamber 14 during the up and down movement. The up and down surging of the hot liquid can make the reaction liquid in the heating tube 12 heated evenly, and can ensure the heating efficiency. The connecting plate 24 set at a 45° angle can reduce the contact area between it and the heat-conducting liquid, and can reduce the resistance encountered by the connecting plate 24 during the movement, and can reduce the load of the motor 2, and can make the temperature distribution of the heat-conducting liquid uniform, and can improve the heating effect. By changing the power of the heater 13, the temperature of the heat-conducting liquid can be gradually increased, and the components with different boiling points in the by-product can be separated, which is beneficial to the separation of the by-products. In the process of the transmission shaft 16 rotating, the cylindrical disk 17 can rotate at the same time, and at this time, the paddle 21 in the stirring blade 20 can drive the cold water in the cooling chamber 10 and the condenser tube 15 quick contact, can make the by-product separated during separation and distillation quickly cooled and discharged from the discharge pipe 9, can improve the efficiency of by-product separation during distillation, and can continuously replenish condensed water through the water inlet pipe 4 and the water outlet pipe 3, can ensure the condensation effect, in use, the power-on state of the electromagnet 7 can be controlled by the PLC controller 8, when the electromagnet 7 is energized, the electromagnet 7 can push the limit pin 28 to slide outward, at this time the limit pin 28 can be embedded in the limit groove 29, at this time the transmission shaft 16 is fixedly connected to the cylindrical disk 17, at this time the rotation of the transmission shaft 16 can drive the cylindrical disk 17 to rotate, at this time the stirring blade 20 and the paddle 21 on the cylindrical disk 17 can rotate synchronously, can be convenient The condensed water is stirred, and because the cylindrical disk 17 is located above the water outlet pipe 3, the condensed water can be prevented from entering the movable hole 31, and the normal use of the electromagnet 7 can be guaranteed. When the electromagnet 7 is powered off, the spring 30 can squeeze the limit pin 28, and the limit pin 28 can shrink to the movable hole 31, so that the transmission shaft 16 and the cylindrical disk 17 can be separated from each other, and the transmission shaft 16 can rotate freely in the cylindrical disk 17. By controlling the power-on state of the electromagnet 7, it is possible to selectively adjust whether the transmission shaft 16 and the cylindrical disk 17 are fixed, and only the connecting plate 24 can be driven to slide up and down during the initial heating process of separation, so that the load on the output end of the motor 2 can be reduced, and the service life of the motor 2 can be increased.

[0067] Embodiment 3:

[0068] Take 16g of treated benzene, 4g of chlorine and 16g of catalyst ferric chloride to react in a chlorinator. The temperature in the chlorinator is less than 70°C and greater than 50°C. The obtained product is directly passed into a separator for separation. After separation, it is dehydrated and purified to obtain the product. After testing, the content of chlorobenzene reaches more than 99.8%, and the total yield is 98.2%.

[0069] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technician familiar with this profession can make some changes or modifications to equivalent embodiments of equivalent changes by using the methods and technical contents disclosed above without departing from the scope of the technical solution of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A chlorobenzene production process, characterized in that: The following steps are involved: S1: Raw material preparation: treating benzene and chlorine; S2: Chlorination reaction: Benzene and chlorine are transported to the chlorinator respectively, and the chlorination reaction is carried out under the action of the catalyst, and the chlorinator is cooled during the reaction; S3: separation of chlorinated products: separation of the products using a separator; S4: Purification: Dehydrating the separated chlorobenzene to obtain chlorobenzene.

2. A chlorobenzene production process according to claim 1, characterized in that: In step S1, the water content in the treated benzene is less than 0.04% by mass.

3. A chlorobenzene production process according to claim 1, characterized in that: In step S1, the mass fraction of water in the treated chlorine gas is less than 0.04%.

4. A chlorobenzene production process according to claim 1, characterized in that: In step S2, the catalyst is ferric chloride, and the amount of ferric chloride dissolved in benzene is 0.007% to 0.009% (mass fraction).

5. A chlorobenzene production process according to claim 1, characterized in that: In step S2, the catalyst is an iron ring arranged in a chlorinator.

6. A chlorobenzene production process according to claim 1, characterized in that: In step S2, the benzene feed amount is 2.0-2.5m 3 / h, chlorine feed rate 200-250m 3 / h.

7. A chlorobenzene production process according to claim 1, characterized in that: In step S2, two circulating coolers are externally installed at the lower part of the chlorinator.

8. A chlorobenzene production process according to claim 7, characterized in that: In step S2, a condenser is provided on top of the chlorinator.

9. A chlorobenzene production process according to claim 1, characterized in that: In step S4, chlorobenzene is filtered through a filter to remove impurities therein, and then the chlorobenzene is brought into contact with a desiccant to allow it to absorb water, and then a dehydration treatment is performed.

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