High-purity tetrachloroethylene continuous synthesis process and equipment

Abstract

The invention discloses continuous synthesis equipment for high-purity tetrachloroethylene. The continuous synthesis equipment comprises a chlorination synthesis device, an energy-saving device, a cooling and washing device, a carbon tetrachloride refining device and a tetrachloroethylene refining device. The invention further discloses a continuous synthesis process of the high-purity tetrachloroethylene. The continuous synthesis process comprises the steps of chlorination synthesis, cooling and washing, carbon tetrachloride refining and tetrachloroethylene refining. The reaction in the tube nest of the chlorination reaction kettle generates carbon tetrachloride, the carbon tetrachloride in the shell pass reacts to generate tetrachloroethylene, and the heat released by the first-step reaction promotes the forward proceeding of the second-step reaction. The heat-conducting oil is used for removing heat after reaction and supplying the heat to the rectification system, so that the energy consumption of the system is reduced. According to the invention, the carbon tetrachloride crude product is refined and then returns to the system, the tetrachloroethylene yield is high, and the conversion rate of tetrachloroethylene in the synthesis kettle is not influenced. The heat transfer oil is used for heating the rectification system and a tetrachloroethylene high-low pressure rectification mode, and the energy of the system is saved by more than 50%.

Description

Technical Field

[0001] The invention belongs to the field of chemical industry, specifically to the field of dry cleaning agent, fire extinguishing agent and metal degreasing solvent, and relates to a high-purity tetrachloroethylene continuous synthesis process and equipment. Background Art

[0002] Perchloroethylene is an important raw material for synthesizing trichloroethylene and fluorine-containing organic compounds. It is widely used in dry cleaning agents, fire extinguishing agents, metal degreasing solvents and other fields. Perchloroethylene produced by traditional processes has low purity, high energy consumption and low product yield. In recent years, with the upgrading of the refrigeration industry, perchloroethylene produced by traditional processes cannot meet the needs of the refrigerant industry. It is urgent to develop a production process for high-purity perchloroethylene.

[0003] There are four main production processes for tetrachloroethylene: 1. Acetylene method: acetylene and chlorine are used as raw materials to first synthesize trichloroethylene, which is further chlorinated to produce pentachloroethane, and then hydrogen chloride is removed to produce tetrachloroethylene, that is, a two-step chlorination and two-step saponification method; 2. Oxychlorination method: ethylene and chlorine are used as raw materials, and dichloroethane is generated through an addition reaction. Dichloroethane then undergoes an oxychlorination reaction with chlorine and oxygen to obtain tetrachloroethylene; 3. Ethylene direct chlorination method: ethylene or C2 chlorocarbon liquid phase pressure chlorination produces chlorocarbons mainly composed of tetrachloroethane and pentachloroethane, and then thermal cracking produces trichloroethylene and tetrachloroethylene; 4. Low-carbon hydrocarbon thermal chlorination method: C1~C3 alkanes or chlorocarbons are used as raw materials, chlorine and low-carbon alkanes or chlorocarbons and other circulating materials are mixed and fed into a reactor, and the reaction temperature is maintained at 500℃~700℃ to produce tetrachloroethylene and carbon tetrachloride.

[0004] At present, the fourth production method is mainly used in China, which mainly includes chlorination synthesis, cooling washing, and tetrachloroethylene refining. This method uses methane chloride and chlorine as raw materials to synthesize tetrachloroethylene in a chlorination reactor. The main reactions are as follows:

[0005] CH3Cl+3Cl2=CCl4+3HCl

[0006] CH2Cl2+2Cl2=CCl4+2HCl

[0007] 2CCl4=C2Cl4+2Cl2

[0008] The overall chemical reaction equation is as follows: CH3Cl+CH2Cl2+3Cl2=C2Cl4+5HCl

[0009] Chinese patent CN 103113184 A is divided into two-stage reaction, a secondary chlorination reactor is added after the primary chlorination reactor, dichloromethane and chloroform are introduced into the secondary chlorination reactor, and the excess chlorine in the gas outlet of the primary chlorination reactor is completely converted, and the remaining dichloromethane and chloroform are returned to the primary chlorination reactor for use after fractionation. Although the purpose of completely consuming the chlorine in the synthesis gas is achieved, the heat of reaction after the secondary reaction further increases the system cooling energy consumption, and does not achieve the effect of increasing the product yield. Chinese patent CN 103588615 A ​​flashes the carbon tetrachloride condensate obtained by the three-stage condenser to remove light and refine and remove heavy treatment, and then returns to the reactor to continue to participate in the chlorination reaction, reducing the initial raw material tetrachloroethylene content in the reactor and improving the reaction yield. However, carbon tetrachloride is mainly condensed in the first and second condensers, and the carbon tetrachloride refluxed to the reactor at the second stage still contains a large amount of tetrachloroethylene, and the reaction yield is not greatly improved. Summary of the invention

[0010] The invention aims to solve the problems of low yield, high energy consumption, low production capacity, poor product quality and low safety of the existing process, and to provide a new high-purity tetrachloroethylene continuous synthesis equipment and a process for continuously producing high-purity tetrachloroethylene based on the equipment. The production process uses chlorine, a first raw material and a second raw material as raw materials, and through chlorination synthesis, cooling and washing, carbon tetrachloride refining and tetrachloroethylene refining, the reaction heat is fully recovered, the reaction energy consumption is reduced, the reaction yield is improved, the process has less three wastes and higher safety.

[0011] The objective of the present invention is achieved through the following technical solutions:

[0012] A high-purity tetrachloroethylene continuous synthesis device, comprising a chlorination synthesis device, an energy-saving device, a cooling and washing device, a carbon tetrachloride refining device, and a tetrachloroethylene refining device;

[0013] The chlorination synthesis device comprises a first superheater 1, a second superheater 2, a venturi ejector 3, a diluent vaporizer 4, and a chlorination reaction kettle 5; the chlorination reaction kettle 5 comprises a cylinder, an upper head, a lower head, an upper tube sheet 46, and a lower tube sheet 47; a plurality of tubes 43 are arranged between the upper and lower tube sheets, and a plurality of connecting holes 48 are arranged on the lower tube sheet 47 so that the material discharged from the lower end of the tubes enters the shell through the connecting holes; a baffle 44 is arranged in the cylinder; a raw material mixer is arranged on the top feed pipeline of the chlorination reaction kettle 5, and the raw material mixer comprises a pipeline body, a feed port is arranged on the top of the pipeline body for feeding chlorine (or chlorine and carbon tetrachloride), a discharge port is arranged at the bottom of the pipeline body, and the raw material mixer is provided with at least one pair of The feeding mechanism is used for feeding the mixed gas of the first raw material and the second raw material. Each pair of feeding mechanisms includes symmetrically arranged feeding devices, each feeding device includes a plurality of inner extension pipes 49 extending into the pipeline body, and a plurality of distribution holes 50 are respectively opened on both sides of the tube body of the inner extension pipe 49 extending into the raw material mixer. The opening direction of the distribution holes 50 is parallel to the vertical section of the raw material mixer. After the mixed gas of the first raw material and the second raw material passes into the inner extension pipe, a gas wall is generated in the mixer to strengthen the mixing with the inlet raw material chlorine; the bottom of the chlorination reaction kettle 5 is provided with a second raw material feeding port; the upper part of the cylinder of the chlorination reaction kettle 5 is provided with a reaction gas outlet; the cylinder of the chlorination reaction kettle 5 is provided with a jacket 45, and the jacket 45 is provided with an electric heater;

[0014] The energy-saving device includes an energy saver 6 and a heat-conducting oil tank 7;

[0015] The reaction gas outlet of the chlorination reactor 5 is connected to the inlet of the cooling and washing device through the economizer 6, and the reaction gas exchanges heat with the heat transfer oil in the economizer to remove the reaction heat by using the heat transfer oil;

[0016] The cooling and washing device comprises a quenching tower 9, a primary condenser 10, a secondary cryogenic freezer 11, a carbon tetrachloride crude product tank 12, and a tetrachloroethylene crude product tank 14; the top gas outlet of the quenching tower 9 is connected to the primary condenser 10 and the secondary cryogenic freezer 11 in sequence, the liquid outlet of the primary condenser 10 and the liquid outlet of the secondary cryogenic freezer 11 are connected to the carbon tetrachloride crude product tank 12 respectively, and the outlet of the carbon tetrachloride crude product tank 12 is connected to the reflux port of the quenching tower 9 and the feed port of the carbon tetrachloride refining device respectively; the side line extraction pipeline of the quenching tower 9 is connected to the lower feed port of the tetrachloroethylene light removal tower 23 of the tetrachloroethylene refining device; hydrogen chloride and heavy components are mainly separated by the cooling and washing device to obtain carbon tetrachloride crude product and tetrachloroethylene crude product;

[0017] The carbon tetrachloride refining device comprises a carbon tetrachloride refining tower 18, a carbon tetrachloride refining tower reboiler 17, and a carbon tetrachloride refining tower condenser 19; the feed port of the carbon tetrachloride refining tower 18 is connected to the outlet of the carbon tetrachloride crude product tank 12, and the top gas outlet of the carbon tetrachloride refining tower 18 is connected to the reflux port of the carbon tetrachloride refining tower 18 and the outlet of the diluent vaporizer 4 through the carbon tetrachloride refining tower condenser 19; the non-condensable gas outlet of the carbon tetrachloride refining tower condenser 19 is connected to the outlet of the carbon tetrachloride refining tower 18 and the outlet of the diluent vaporizer 4 respectively; The outlet of the carbon tetrachloride refining tower 18 is connected to the suction pipe outlet of the venturi ejector 3; the outlet of the tower kettle of the carbon tetrachloride refining tower 18 is connected to the upper feed port of the tetrachloroethylene light removal tower 23 of the tetrachloroethylene refining device; the crude carbon tetrachloride separated by the cooling and washing device is refined by the carbon tetrachloride refining device, and the qualified carbon tetrachloride product obtained by refining is returned to the chlorination reaction kettle after vaporization, and the material in the tower kettle of the carbon tetrachloride refining tower 18 is further transported to the tetrachloroethylene refining device to be refined to obtain tetrachloroethylene;

[0018] The tetrachloroethylene refining device comprises a tetrachloroethylene light removal tower 23, a tetrachloroethylene light removal tower top condenser 24, a tetrachloroethylene light removal tower reboiler 27, a tetrachloroethylene low-pressure tower 29, a tetrachloroethylene low-pressure tower top condenser 30, a tetrachloroethylene thermal coupling reboiler 33, a tetrachloroethylene low-pressure tower kettle pump 34, a tetrachloroethylene high-pressure tower 35, a tetrachloroethylene high-pressure tower top condenser 38, a tetrachloroethylene high-pressure tower reboiler 36, and a tetrachloroethylene product cooler 41; the tetrachloroethylene light removal tower 23 is provided with an upper inlet The feed port and the lower feed port are connected, the lower feed port is connected to the side line extraction pipeline of the quench tower 9, and the upper feed port is connected to the outlet of the tower kettle of the carbon tetrachloride refining tower 18; the top gas outlet of the tetrachloroethylene light removal tower 23 is connected to the inlet of the top condenser 24 of the tetrachloroethylene light removal tower, the liquid outlet of the top condenser 24 of the tetrachloroethylene light removal tower is connected to the reflux port of the tetrachloroethylene light removal tower 23, and the non-condensable gas outlet of the top condenser 24 of the tetrachloroethylene light removal tower is connected to the suction pipe port of the venturi ejector 3; the tetrachloroethylene light removal tower The kettle outlet of tower 23 is connected to the feed inlet of the tetrachloroethylene low-pressure tower 29; the top gas outlet of the tetrachloroethylene low-pressure tower 29 is connected to the inlet of the tetrachloroethylene low-pressure tower top condenser 30, and the liquid outlet of the tetrachloroethylene low-pressure tower top condenser 30 is respectively connected to the reflux port of the tetrachloroethylene low-pressure tower 29 and the inlet of the tetrachloroethylene product cooler 41; the kettle outlet of the tetrachloroethylene low-pressure tower 29 is connected to the feed inlet of the tetrachloroethylene high-pressure tower 35; the top gas outlet of the tetrachloroethylene high-pressure tower 35 is connected to the inlet of the tetrachloroethylene high-pressure tower 35. It is connected to the heating medium inlet of the tetrachloroethylene heat-coupled reboiler 33, the heating medium outlet of the tetrachloroethylene heat-coupled reboiler 33 is connected to the inlet of the tetrachloroethylene high-pressure tower top condenser 38, the liquid outlet of the tetrachloroethylene high-pressure tower top condenser 38 is respectively connected to the reflux port of the tetrachloroethylene high-pressure tower 35 and the inlet of the tetrachloroethylene product cooler 41, and the high-purity tetrachloroethylene product is extracted from the tetrachloroethylene product cooler 41; the tower kettle outlet of the tetrachloroethylene high-pressure tower 35 is connected to the tower kettle feed port of the quenching tower 9.

[0019] Preferably, the first superheater 1 and the second superheater 2 are both heated by steam, and the first superheater 1 is provided with a feed port at the bottom and a discharge port at the top, and the second superheater 2 is provided with a feed port at the bottom and a discharge port at the top. The discharge ports of the first superheater 1 and the second superheater 2 are respectively connected to the feed main pipe, and the superheated first raw material and the superheated second raw material are mixed in the feed main pipe; the feed main pipe is connected to the feed mechanism of the chlorination reaction kettle 5 through the feed branch pipe.

[0020] Preferably, the inlet of the venturi injector 3 is connected to the raw material chlorine gas pipe, the suction pipe port of the venturi injector 3 is respectively connected to the non-condensable gas outlet of the carbon tetrachloride refining tower condenser 19 and the non-condensable gas outlet of the tetrachloroethylene light removal tower top condenser 24, and the outlet of the venturi injector 3 is connected to the feed port at the top of the chlorination reaction kettle 5.

[0021] Preferably, the diluent vaporizer 4 is heated by heat transfer oil, and the outlet of the diluent vaporizer 4 is connected to the outlet pipeline of the Venturi ejector 3 .

[0022] Preferably, the upper tube plate 46 is arranged at the connection between the upper head and the cylinder, and the lower tube plate 47 is arranged at the connection between the lower head and the cylinder.

[0023] Preferably, the upper and lower tube sheets are respectively provided with mounting holes for mounting the tubes, and both ends of the tubes 43 are respectively fixed to the mounting holes of the upper and lower tube sheets.

[0024] Preferably, the total opening area of ​​the communicating holes of the lower tube plate is not less than the total opening area of ​​the mounting holes.

[0025] Preferably, the upper and lower adjacent layers of baffles are arranged in a staggered manner to enhance the turbulence of the airflow in the cylinder, which is beneficial to the heat exchange of the inlet and outlet raw gases.

[0026] Preferably, one end of the inner extension tube extending into the raw material mixer is closed, or one end of the inner extension tube extending into the raw material mixer is closed and a plurality of air outlet holes with a smaller diameter than that of the inner extension tube are opened at the closed end.

[0027] Preferably, the raw material mixer is provided with a pair of feeding mechanisms, which include a left feeding device and a right feeding device which are symmetrically arranged, and the left feeding device and the right feeding device have the same structure. The left feeding device or the right feeding device includes a feeding pipe and a plurality of inner extension tubes 49, one end of each inner extension tube 49 is connected to the feeding pipe, and the other end extends into the pipeline body, and one end of the inner extension tube 49 extending into the pipeline body is closed, or one end of the inner extension tube 49 extending into the pipeline body is closed and 1 to 2 air outlet holes with a smaller aperture than the inner extension tube diameter are opened at the closed end, and a plurality of distribution holes 50 are respectively opened on both sides of the tube body where the inner extension tube 49 extends into the pipeline body, and the opening direction is parallel to the vertical section of the raw material mixer.

[0028] Preferably, the multiple inner extension tubes 49 in the same feeding device are arranged horizontally, vertically or staggered.

[0029] Preferably, a reaction gas outlet is provided on each of the two sides of the upper part of the cylinder of the chlorination reaction kettle 5 .

[0030] Preferably, a heat transfer oil inlet and a heat transfer oil outlet are respectively provided at the upper and lower ends of the jacket, the heat transfer oil inlet is connected to the outlet of the heat transfer oil tank 7, and the heat transfer oil outlet is connected to the inlet of the heat transfer oil tank 7. Heat transfer oil can be introduced into the jacket of the chlorination reaction kettle 5, and the electric heater heats the chlorination reaction kettle 5 to reach the reaction temperature when starting, and the electric heater stops heating during normal operation. When the chlorination reaction kettle 5 is over-temperatured, heat transfer oil is introduced to cool it down in time.

[0031] Preferably, the economizer 6 is a flue gas heat exchanger; the two ends of the economizer 6 are respectively provided with a heating medium inlet and a heating medium outlet, and the economizer 6 is provided with a condenser as a heat transfer oil channel; the heating medium inlet of the economizer 6 is connected to the reaction gas outlet of the chlorination reactor 5, and the heating medium outlet is connected to the gas phase feed port of the reactor of the quench tower 9; the inlet of the condenser in the economizer 6 is connected to the outlet of the heat transfer oil tank 7, and the outlet of the condenser is respectively connected to the heating medium inlet of the carbon tetrachloride refining tower reboiler 17, the tetrachloroethylene light removal tower reboiler 27, and the tetrachloroethylene high-pressure tower reboiler 36 through the electric heater 42, and the heating medium outlets of the carbon tetrachloride refining tower reboiler 17, the tetrachloroethylene light removal tower reboiler 27, and the tetrachloroethylene high-pressure tower reboiler 36 are respectively connected to the inlet of the heat transfer oil tank 7. The present invention uses heat transfer oil to remove reaction heat for heating the subsequent distillation system.

[0032] Preferably, a heat transfer oil pump 8 is provided at the outlet pipeline of the heat transfer oil tank 7; the outlet of the heat transfer oil pump 8 is respectively connected to the heat transfer oil inlet of the jacket of the chlorination reactor 5 and the inlet of the condenser in the economizer 6.

[0033] Preferably, a crude carbon tetrachloride pump 13 is provided at the outlet pipeline of the crude carbon tetrachloride tank 12, and the outlet pipeline of the crude carbon tetrachloride pump 13 is respectively connected to the reflux port of the quench tower 9 and the feed port of the carbon tetrachloride refining tower 18 of the carbon tetrachloride refining device.

[0034] Preferably, the side line extraction pipeline of the quench tower 9 is connected to the crude tetrachloroethylene tank 14; the outlet pipeline of the crude tetrachloroethylene tank 14 is provided with a crude tetrachloroethylene pump 15, and the outlet of the crude tetrachloroethylene pump 15 is connected to the lower feed port of the tetrachloroethylene light removal tower 23 of the tetrachloroethylene refining device.

[0035] Preferably, the outlet pipeline of the kettle of the quench tower 9 is provided with a recombinant pump 16 .

[0036] Preferably, the liquid outlet of the carbon tetrachloride refining tower condenser 19 is connected to the inlet of the carbon tetrachloride refining tower reflux tank 20, and the outlet of the carbon tetrachloride refining tower reflux tank 20 is connected to the reflux port of the carbon tetrachloride refining tower 18 and the inlet of the diluent vaporizer 4 respectively.

[0037] More preferably, the outlet pipeline of the carbon tetrachloride refining tower reflux tank 20 is provided with a carbon tetrachloride refining tower reflux pump 21, and the outlet of the carbon tetrachloride refining tower reflux pump 21 is connected to the reflux port of the carbon tetrachloride refining tower 18 and the outlet of the diluent vaporizer 4 respectively.

[0038] Preferably, the outlet pipeline of the tower kettle of the carbon tetrachloride refining tower 18 is provided with a carbon tetrachloride refining tower kettle pump 22.

[0039] Preferably, the upper feed port of the tetrachloroethylene light removal tower 23 is connected to the bottom outlet of the carbon tetrachloride refining tower 18 via the carbon tetrachloride refining tower bottom pump 22, and the lower feed port of the tetrachloroethylene light removal tower 23 is connected to the outlet of the crude tetrachloroethylene tank 14 via the crude tetrachloroethylene pump 15.

[0040] Preferably, the liquid outlet of the tetrachloroethylene light removal tower top condenser 24 is connected to the reflux port of the tetrachloroethylene light removal tower 23 via the tetrachloroethylene light removal tower reflux tank 25.

[0041] More preferably, a tetrachloroethylene light-removal tower reflux pump 26 is provided in the outlet pipeline of the tetrachloroethylene light-removal tower reflux tank 25 .

[0042] Preferably, the kettle outlet pipeline of the tetrachloroethylene light-removal tower 23 is provided with a kettle pump 28 of the tetrachloroethylene light-removal tower.

[0043] Preferably, the liquid outlet of the tetrachloroethylene low-pressure tower top condenser 30 is connected to the inlet of the tetrachloroethylene low-pressure tower reflux tank 31, and the outlet of the tetrachloroethylene low-pressure tower reflux tank 31 is respectively connected to the reflux port of the tetrachloroethylene low-pressure tower 29 and the inlet of the tetrachloroethylene product cooler 41.

[0044] More preferably, the outlet pipeline of the tetrachloroethylene low-pressure tower reflux tank 31 is provided with a tetrachloroethylene low-pressure tower reflux pump 32, and the outlet of the tetrachloroethylene low-pressure tower reflux pump 32 is respectively connected to the reflux port of the tetrachloroethylene low-pressure tower 29 and the inlet of the tetrachloroethylene product cooler 41.

[0045] Preferably, the tetrachloroethylene low-pressure tower 29 bottom outlet pipeline is provided with a tetrachloroethylene low-pressure tower bottom pump 34.

[0046] Preferably, the liquid outlet of the tetrachloroethylene high-pressure tower top condenser 38 is connected to the inlet of the tetrachloroethylene high-pressure tower reflux tank 39, and the outlet of the tetrachloroethylene high-pressure tower reflux tank 39 is respectively connected to the reflux port of the tetrachloroethylene high-pressure tower 35 and the inlet of the tetrachloroethylene product cooler 41.

[0047] More preferably, the outlet pipeline of the tetrachloroethylene high-pressure tower reflux tank 39 is provided with a tetrachloroethylene high-pressure tower reflux pump 40, and the outlet of the tetrachloroethylene high-pressure tower reflux pump 40 is respectively connected to the reflux port of the tetrachloroethylene high-pressure tower 35 and the inlet of the tetrachloroethylene product cooler 41.

[0048] Preferably, the tetrachloroethylene high-pressure tower 35 kettle outlet pipeline is provided with a tetrachloroethylene high-pressure tower kettle pump 37.

[0049] Another object of the present invention is to provide a high-purity tetrachloroethylene continuous synthesis process based on the tetrachloroethylene continuous synthesis equipment, comprising the following steps:

[0050] Step (1), chlorination synthesis: the first raw material and the second raw material are mixed after heat treatment, and symmetrically fed from the side of the raw material mixer of the chlorination reactor 5. The raw chlorine is mixed with vaporized carbon tetrachloride through a venturi injector or the raw chlorine enters the raw material mixer of the chlorination reactor from the top through a venturi injector. The mixed reaction gas in the raw material mixer enters the tube array. The first raw material and the second raw material react with excess chlorine to generate carbon tetrachloride, which is discharged from the lower end of the tube array into the lower head. A small amount of the second raw material is added to the lower head of the chlorination reactor to consume the unreacted chlorine. The material in the lower head enters the shell side through the connecting hole of the lower tube plate, and carbon tetrachloride generates tetrachloroethylene in the shell side; the reaction gas enters the economizer 6, and part of the heat is removed by heat exchange with the heat transfer oil, and then enters the quenching tower 9;

[0051] Step (2), cooling and washing: the reaction gas enters the quench 9 for cooling and washing, the gas phase at the top of the quench tower is sequentially condensed through the primary condenser 10 and the secondary cryogenic freezer 11 to obtain a liquid phase crude carbon tetrachloride, the crude carbon tetrachloride enters the crude carbon tetrachloride tank 12, part of which is refluxed to the quench tower 9 to wash the heavy components, and the rest is transported to the carbon tetrachloride refining tower 18, and the uncondensed hydrogen chloride is discharged from the gas outlet of the secondary cryogenic freezer to the downstream system; the quench tower side line produces a crude tetrachloroethylene product, the crude tetrachloroethylene product enters the crude tetrachloroethylene tank 14, and then is transported to the tetrachloroethylene light removal tower 23;

[0052] Step (3), refining carbon tetrachloride: the crude carbon tetrachloride enters the carbon tetrachloride refining tower 18 for refining, the gas phase at the top of the carbon tetrachloride refining tower is condensed to obtain qualified carbon tetrachloride products, the qualified carbon tetrachloride products are vaporized by the diluent vaporizer and returned to the chlorination reactor, the uncondensed gas is returned to the chlorination reactor via the venturi ejector, and the heavy components in the reactor are transported to the tetrachloroethylene light removal tower 23;

[0053] Step (4), tetrachloroethylene refining: the crude tetrachloroethylene obtained in step (2) and the heavy components in the bottom of the carbon tetrachloride refining tower obtained in step (3) enter the tetrachloroethylene light-removing tower 23, the top gas phase of the tetrachloroethylene light-removing tower is condensed, the light components of the gas phase are returned to the chlorination reaction kettle through a venturi ejector, the liquid phase is refluxed to the tetrachloroethylene light-removing tower, the bottom material (tetrachloroethylene) of the tetrachloroethylene light-removing tower is transported to the tetrachloroethylene low-pressure tower 29, the top gas phase of the tetrachloroethylene low-pressure tower is condensed to produce the tetrachloroethylene product, the bottom material is transported to the tetrachloroethylene high-pressure tower 35, the top gas phase of the tetrachloroethylene high-pressure tower is firstly heat-exchanged with the tetrachloroethylene thermally coupled reboiler 33, and then condensed to produce the tetrachloroethylene product, the bottom material is transported to the quenching tower 9, the tetrachloroethylene products produced from the tetrachloroethylene high- and low-pressure towers are cooled by the tetrachloroethylene product cooler, and then produced out of the boundary.

[0054] In step (1), the first raw material is one or more of methane, methyl chloride, dichloromethane, chloroform, and natural gas; the second raw material is one or more of methane, methyl chloride, dichloromethane, chloroform, and natural gas.

[0055] The purity of the first raw material is ≥99%wt, the feed temperature is 90-110°C, and the feed pressure is 0.5-1.2MPaG.

[0056] The purity of the second raw material is ≥99%wt, the feed temperature is 90-110°C, and the feed pressure is 0.5-1.2MPaG.

[0057] The purity of the chlorine gas is ≥99%wt, the feed temperature is 80-120°C, and the feed pressure is 0.5-1.0MPaG.

[0058] The purity of the carbon tetrachloride is ≥95%wt, the feed temperature is 30-60°C, and the feed pressure is 0.5-0.8MPaG.

[0059] The temperature of the first superheater 1 is 130-180°C, preferably 140-160°C.

[0060] The temperature of the second superheater 2 is 130-180°C, preferably 140-160°C.

[0061] The feed ratio of the first raw material to the second raw material can be any ratio. Specifically, the mass ratio of the first raw material to the second raw material is 1:1.2 to 1:1.2.

[0062] The second raw material fed from the second raw material feeding port of the chlorination reactor accounts for 2% of the total second raw material feed amount.

[0063] The mass ratio of the carbon tetrachloride to the chlorine feed flow rate is 0:1 to 10:1, preferably 2:1 to 8:1.

[0064] The ratio of the total feed flow mass of the first raw material and the second raw material to the feed flow mass of chlorine is 1:1.4 to 1:3, preferably 1:1.5 to 1:2.6; the present invention strictly controls the feed flow rates of chlorine, the first raw material and the second raw material through flow adjustment ratio control to prevent excessive chlorine from causing a decrease in chlorine yield and too little chlorine from causing carbonization inside the reactor.

[0065] When the first raw material is one or more of chloroform, dichloromethane, and chloroform, and the second raw material is one or more of chloroform, dichloromethane, and chloroform, the ratio of the total feed flow mass of the first raw material and the second raw material to the feed flow mass of chlorine is 1:1.4 to 1:2.0, preferably 1:1.5 to 1:1.8. When the first raw material is at least one of methane and natural gas, and the second raw material is at least one of methane and natural gas, the ratio of the total feed flow mass of the first raw material and the second raw material to the feed flow mass of chlorine is 1:2 to 1:3, preferably 1:2.1 to 1:2.6.

[0066] The temperature of the diluent vaporizer 4 is 110-200° C., preferably 150-180° C., and the pressure of the diluent vaporizer 4 is 0.2-0.7 MPaG, preferably 0.3-0.5 MPaG.

[0067] The temperature of the chlorination reaction kettle 5 is 500-650° C., preferably 550-600° C., and the pressure of the chlorination reaction kettle 5 is 0.05-0.3 MPaG, preferably 0.07-0.12 MPaG.

[0068] The temperature of the heat transfer oil at the outlet of the economizer 6 is 150-260° C., preferably 180-245° C.; the pressure of the economizer 6 is 0.2-0.8 MPaG, preferably 0.3-0.5 MPaG.

[0069] In step (2), the quenching tower 9 is a plate tower.

[0070] The operating temperature of the bottom of the quench tower 9 is 150-230° C., preferably 170-220° C.; the pressure of the quench tower 9 is 0.04-0.3 MPaG, preferably 0.06-0.12 MPaG; the reflux ratio is 2-20, preferably 3-15.

[0071] The side plates of the quench tower 9 are 5 to 20 plates away from the bottom of the tower, preferably 7 to 15 plates away from the bottom of the tower.

[0072] The recombinant components of the quench tower kettle are a mixture of hexachloroethane, hexachlorobutadiene and hexachlorobenzene, which are transported to the outside.

[0073] The condensation temperature of the primary condenser 10 is 30 to 70°C, preferably 35 to 50°C; the temperature of the secondary cryogenic freezer 11 is -10 to -40°C, preferably -15 to -25°C.

[0074] The content of hydrogen chloride is ≥98%.

[0075] The temperature of the crude tetrachloroethylene tank 14 is 100-150° C., preferably 110-140° C., and the pressure of the crude tetrachloroethylene tank 12 is 0.005-0.1 MPaG, preferably 0.02-0.07 MPaG.

[0076] In step (3), the pressure of the carbon tetrachloride refining tower 18 is 0-0.1 MPaG, preferably 0-10 KPaG; the top operating temperature of the carbon tetrachloride refining tower 18 is 80-100° C., preferably 85-95° C.; and the reflux ratio is 10-30, preferably 15-20.

[0077] The carbon tetrachloride refining tower is a plate tower.

[0078] Preferably, the gas phase at the top of the carbon tetrachloride refining tower enters the carbon tetrachloride refining tower condenser and is condensed to obtain qualified carbon tetrachloride products.

[0079] The temperature of the carbon tetrachloride refining tower condenser is 40-60°C, preferably 45-55°C.

[0080] The content of the qualified carbon tetrachloride product is ≥99%.

[0081] After the gas phase at the top of the carbon tetrachloride refining tower is condensed, the uncondensed gases are dichloromethane and chloroform; the bottom of the carbon tetrachloride refining tower is reorganized into tetrachloroethylene and carbon tetrachloride.

[0082] In step (4), the crude tetrachloroethylene obtained in step (2) enters the tetrachloroethylene light removal tower 23 from the lower feed port; the heavy components in the bottom of the carbon tetrachloride refining tower obtained in step (3) enter the tetrachloroethylene light removal tower 23 from the upper feed port.

[0083] The tetrachloroethylene light-removing tower 23 is a plate tower.

[0084] The pressure of the tetrachloroethylene light removal tower 23 is 0-0.1 MPaG, preferably 0-10 KPaG; the tower top operating temperature is 90-110° C., preferably 95-100° C.; the reflux ratio is 60-90, preferably 65-80.

[0085] The temperature of the top condenser of the tetrachloroethylene light removal tower is 50-70°C, preferably 55-65°C.

[0086] The tetrachloroethylene low-pressure tower is a plate tower.

[0087] The pressure of the tetrachloroethylene low-pressure tower is 0-0.1 MPaG, preferably 0-10 KPaG, the top operating temperature is 110-140° C., preferably 120-130° C., and the reflux ratio is 20-30, preferably 23-27.

[0088] The bottom material of the tetrachloroethylene low-pressure tower 29 is tetrachloroethylene containing heavy components, specifically tetrachloroethylene, hexachloroethane, hexachlorobutadiene and hexachlorobenzene.

[0089] The temperature of the tetrachloroethylene low-pressure tower top condenser is 80-130°C, preferably 90-120°C.

[0090] The tetrachloroethylene high-pressure tower is a plate tower.

[0091] The pressure of the tetrachloroethylene high-pressure tower is 0.2-0.5 MPaG, preferably 0.3-0.4 MPaG, the top operating temperature is 180-210° C., preferably 190-200° C., and the reflux ratio is 22-35, preferably 25-30.

[0092] The materials in the bottom of the tetrachloroethylene high-pressure tower 35 are heavy components, specifically hexachloroethane, hexachlorobutadiene and hexachlorobenzene.

[0093] The temperature of the tetrachloroethylene high-pressure tower top condenser is 160-200°C, preferably 170-190°C.

[0094] The content of the tetrachloroethylene product is ≥99.98%.

[0095] The temperature of the tetrachloroethylene product cooler is 30-60°C, preferably 40-50°C.

[0096] As a preferred technical solution of the high-purity tetrachloroethylene continuous synthesis process of the present invention, it also includes:

[0097] Step (5), heat recovery of heat transfer oil: the heat transfer oil discharged from the economizer 6 is heated by the electric heater 42 and then supplied to the carbon tetrachloride refining device and the tetrachloroethylene refining device for heat supply.

[0098] Preferably, the heat transfer oil discharged from the economizer 6 is heated by the electric heater 42 and then supplied to the carbon tetrachloride refining tower reboiler 17, the tetrachloroethylene light removal tower reboiler 27, and the tetrachloroethylene high-pressure tower reboiler 36 for heat supply, and then returned to the heat transfer oil tank 7.

[0099] The heat transfer oil is heated by the electric heater 42 to a temperature of 230-260°C, preferably 240-250°C.

[0100] The process principle of the present invention:

[0101] The existing process directly mixes chlorine, the first raw material, and the second raw material and passes them into the reactor, which easily causes the raw material at the entrance to be taken out of the reactor by the discharge before the reaction, and the chlorine content in the reaction tail gas is high, and the reaction yield is low. The present invention divides the chlorination reactor into two-stage reactions, and methane chloride or methane reacts with chlorine in the tube to generate carbon tetrachloride, and the reaction is exothermic. The carbon tetrachloride in the shell side reacts to generate tetrachloroethylene and absorbs heat, and the heat released by the first step reaction is effectively utilized to promote the forward progress of the second step reaction. A mixer is set at the entrance of the chlorination reactor to fully mix the feed raw materials, which is conducive to the reaction. A small amount of the second raw material is passed through the lower head of the chlorination reactor to consume the chlorine in the raw gas and promote the second step reaction. A jacket is set in the chlorination reactor, and when over-temperature and overpressure occur, heat transfer oil is passed in time to remove the reaction heat, and the system safety is higher.

[0102] In the existing process, the tail gas discharged from the chlorination reactor directly enters the quenching tower, which increases the load of the quenching tower and increases the energy consumption of the device. The present invention reasonably utilizes the economizer and uses heat transfer oil to remove the heat after the reaction and supply it to the distillation system, saving system energy consumption. The heat transfer oil medium is used, and when corrosion penetration occurs, it will not affect the system, which essentially ensures the safety of the system and achieves the purpose of energy saving.

[0103] In the existing process, the crude carbon tetrachloride is directly returned to the diluent vaporizer. Since the crude carbon tetrachloride contains a large amount of tetrachloroethylene, the tetrachloroethylene yield of the system is low and the tetrachloroethylene conversion rate in the chlorination synthesis reactor is low. The present invention purifies the crude carbon tetrachloride and returns it to the system, the tetrachloroethylene yield of the system is high, and the tetrachloroethylene conversion rate in the synthesis reactor is not affected.

[0104] The existing process of refining tetrachloroethylene adopts a single tower, and the system energy consumption is high. The present invention adopts a tetrachloroethylene light removal tower to remove light components, and then refines the tetrachloroethylene in low-pressure and high-pressure towers. The gas phase at the top of the high-pressure tower serves as the heat source of the low-pressure tower reboiler, which can save steam consumption and save more than 40% energy compared with a single tower.

[0105] Compared with the prior art, the present invention has the following beneficial effects:

[0106] (1) Compared with the traditional process, the tetrachloroethylene production process of the present invention adopts a new green reactor, and the product yield is high;

[0107] (2) The present invention uses heat transfer oil to urgently cool the chlorination reaction kettle, and the process system is safer;

[0108] (3) The present invention uses heat transfer oil to heat the distillation system and the high and low pressure distillation mode of tetrachloroethylene, which reduces the system's cooling and heat consumption, and the system saves more than 50% energy;

[0109] (4) The present invention returns the crude carbon tetrachloride to the chlorination synthesis reactor after refining, thereby reducing the circulation of tetrachloroethylene in the system and improving the reaction conversion rate;

[0110] (5) The chlorination synthesis reactor of the present invention adopts a mode in which the chlorine is excessive in the first stage reaction and the chlorine is completely consumed in the second stage reaction. The hydrogen chloride content in the non-condensable gas at the outlet of the secondary cryogenic refrigerator is high (≥98%), which is significantly higher than 90% in the existing process and can be directly used in the downstream system. BRIEF DESCRIPTION OF THE DRAWINGS

[0111] Figure 1 It is a schematic structural diagram of the high-purity tetrachloroethylene continuous synthesis equipment of the present invention.

[0112] Figure 2 It is a schematic diagram of the structure of the chlorination reactor.

[0113] Figure 3 This is a schematic diagram of the tube installation in the chlorination reactor.

[0114] Figure 4 This is a schematic diagram of the top view of the inlet mixer of the chlorination reactor.

[0115] In the figure, 1-first superheater, 2-second superheater, 3-venturi ejector, 4-diluent vaporizer, 5-chlorination reaction kettle, 6-economizer, 7-heat transfer oil tank, 8-heat transfer oil pump, 9-quenching tower, 10-primary condenser, 11-secondary deep freezer, 12-crude carbon tetrachloride product tank, 13-crude carbon tetrachloride pump, 14-crude tetrachloroethylene product tank, 15-crude tetrachloroethylene pump, 16-heavy component pump, 17-reboiler of carbon tetrachloride refining tower, 18-carbon tetrachloride refining tower, 19-condenser of carbon tetrachloride refining tower, 20-reflux tank of carbon tetrachloride refining tower, 21-reflux pump of carbon tetrachloride refining tower, 22-kettle pump of carbon tetrachloride refining tower, 23-tetrachloroethylene light removal tower, 24-top condenser of tetrachloroethylene light removal tower, 25-reflux tank of tetrachloroethylene light removal tower, 26-tetrachloroethylene light removal tower Tower reflux pump, 27-tetrachloroethylene light removal tower reboiler, 28-tetrachloroethylene light removal tower kettle pump, 29-tetrachloroethylene low-pressure tower, 30-tetrachloroethylene low-pressure tower top condenser, 31-tetrachloroethylene low-pressure tower reflux tank, 32-tetrachloroethylene low-pressure tower reflux pump, 33-tetrachloroethylene thermal coupling reboiler, 34-tetrachloroethylene low-pressure tower kettle pump, 35-tetrachloroethylene high-pressure tower, 36-tetrachloroethylene high-pressure tower reboiler, 37-tetrachloroethylene high-pressure tower kettle pump, 38-tetrachloroethylene high-pressure tower top condenser, 39-tetrachloroethylene high-pressure tower reflux tank, 40-tetrachloroethylene high-pressure tower reflux pump, 41-tetrachloroethylene product cooler, 42-electric heater, 43-tube, 44-baffle, 45-jacket, 46-upper tube sheet, 47-lower tube sheet, 48-connecting hole, 49-inner extension tube, 50-distribution hole. DETAILED DESCRIPTION

[0116] The technical solution of the present invention is further described below in conjunction with embodiments. The following embodiments are illustrative rather than restrictive, and the protection scope of the present invention cannot be limited by the following embodiments.

[0117] Example 1

[0118] like Figure 1 and Figure 2 , Figure 3 and Figure 4 As shown, a high-purity tetrachloroethylene continuous synthesis equipment includes a chlorination synthesis device, an energy-saving device, a cooling and washing device, a carbon tetrachloride refining device, and a tetrachloroethylene refining device.

[0119] The chlorination synthesis device comprises a first superheater 1, a second superheater 2, a venturi ejector 3, a diluent vaporizer 4, and a chlorination reaction kettle 5.

[0120] The chlorination reaction kettle 5 comprises a cylinder, upper and lower heads are respectively arranged at the upper and lower ends of the cylinder, an upper tube sheet 46 is arranged at the connection between the upper head and the cylinder, and a lower tube sheet 47 is arranged at the connection between the lower head and the cylinder; the upper and lower tube sheets are respectively provided with mounting holes for mounting the tubes, a plurality of tubes 43 are arranged between the upper and lower tube sheets, and the two ends of the tubes 43 are respectively fixed to the mounting holes of the upper and lower tube sheets; the lower tube sheet 47 is provided with a plurality of connecting holes 48 so that the material discharged from the lower end of the tubes enters the shell through the connecting holes, and the total opening area of ​​the connecting holes of the lower tube sheet is not less than the total opening area of ​​the mounting holes The cylinder is provided with baffles 44, and the upper and lower adjacent layers of baffles are arranged in a staggered manner to enhance the turbulence of the airflow in the cylinder, which is beneficial to the heat exchange of the inlet and outlet raw gas; the top feed pipeline of the chlorination reactor 5 is provided with a raw material mixer, and the raw material mixer includes a pipeline body, the top of the pipeline body is provided with a feed port for feeding chlorine (or chlorine and carbon tetrachloride), and the bottom of the pipeline body is provided with a discharge port. Symmetrical left and right feeding devices for feeding the mixed gas of the first raw material and the second raw material are provided on both sides of the raw material mixer. The left feeding device has the same structure as the right feeding device, and the left The feeding device includes a feeding pipe and three inner extension pipes 49, the three inner extension pipes 49 are arranged horizontally, one end of each inner extension pipe 49 is connected to the feeding pipe, and the other end extends into the pipeline body, and one end of the inner extension pipe 49 extending into the pipeline body is closed, and a plurality of distribution holes 50 are opened on both sides of the tube body of the inner extension pipe 49 extending into the raw material mixer, and the opening direction of the distribution holes 50 is parallel to the vertical section of the raw material mixer (that is, a plurality of distribution holes 50 are opened on both sides of the tube body of the inner extension pipe 49 extending into the raw material mixer); the bottom of the chlorination reaction kettle 5 is provided with a second raw material feeding port, from which the second raw material The second raw material accounting for 2% of the total amount of the second raw material is introduced into the feeding port to consume the unreacted chlorine; a reaction gas outlet is respectively arranged on both sides of the upper part of the cylinder of the chlorination reaction kettle 5; the cylinder of the chlorination reaction kettle 5 is provided with a jacket 45, and an electric heater is arranged in the jacket 45. A heat transfer oil inlet and a heat transfer oil outlet are respectively arranged at the upper and lower ends of the jacket. Heat transfer oil can be introduced into the jacket of the chlorination reaction kettle 5. When starting, the electric heater heats the chlorination reaction kettle 5 to reach the reaction temperature. During normal operation, the electric heater stops heating. When the chlorination reaction kettle 5 is over-temperatured, heat transfer oil is introduced to cool it down in time.

[0121] The first superheater 1 and the second superheater 2 are both heated by steam. The first superheater 1 is provided with a feed port at the bottom and a discharge port at the top. The second superheater 2 is provided with a feed port at the bottom and a discharge port at the top. The discharge ports of the first superheater 1 and the second superheater 2 are respectively connected to the feed main pipe, and the feed main pipe is connected to the left and right feed devices of the chlorination reactor 5 through the left and right feed branches. The inlet of the venturi injector 3 is connected to the raw material chlorine pipe, and the suction pipe port of the venturi injector 3 is respectively connected to the non-condensable gas outlet of the carbon tetrachloride refining tower condenser 19 and the non-condensable gas outlet of the tetrachloroethylene light tower top condenser 24, and the outlet of the venturi injector 3 is connected to the feed port at the top of the chlorination reactor 5. The diluent vaporizer 4 is heated by heat transfer oil, and the outlet of the diluent vaporizer 4 is connected to the outlet pipeline of the venturi injector 3. The first raw material and the second raw material are mixed in the feed main pipe and then enter the raw material mixer through the inner extension pipe, where a gas wall is generated to strengthen the mixing with the chlorine (or chlorine and carbon tetrachloride) introduced from the top.

[0122] The energy-saving device includes an energy saver 6, a thermal oil tank 7, and a thermal oil pump 8;

[0123] The two reaction gas outlets of the chlorination reaction kettle 5 are respectively connected to the heat supply medium inlet of the economizer 6; the economizer 6 is a flue gas heat exchanger, and a condenser is arranged inside the economizer 6 as a heat transfer oil channel; the outlet of the heat transfer oil tank is respectively connected to the heat transfer oil inlet of the chlorination reaction kettle 5 and the inlet of the condenser in the economizer 6 through a heat transfer oil pump 8; the outlet of the condenser in the economizer 6 is connected to the inlet of the electric heater 42, and the outlet of the electric heater 42 is respectively connected to the reboiler 17 of the carbon tetrachloride refining tower, the reboiler 27 of the tetrachloroethylene light removal tower, and the reboiler 28 of the tetrachloroethylene high-pressure tower. The heat supply medium inlet of 36 is connected, and the heat supply medium outlets of the carbon tetrachloride refining tower reboiler 17, the tetrachloroethylene light removal tower reboiler 27, and the tetrachloroethylene high-pressure tower reboiler 36 and the heat transfer oil outlet of the chlorination reaction kettle 5 are respectively connected to the inlet of the heat transfer oil tank 7; the chlorination reaction kettle 5, the economizer 6, the electric heater 42, the heat transfer oil tank 7, the heat transfer oil pump 8, the carbon tetrachloride refining tower reboiler 17, the tetrachloroethylene light removal tower reboiler 27, and the tetrachloroethylene high-pressure tower reboiler 36 constitute a heat transfer oil heat recovery device, which uses the heat transfer oil to remove the reaction heat for heating the subsequent distillation system.

[0124] The cooling and washing device comprises a quenching tower 9, a primary condenser 10 (using water as a cooling medium), a secondary cryogenic refrigerator 11 (using R507 as a cooling medium), a crude carbon tetrachloride tank 12, a crude carbon tetrachloride pump 13, a crude tetrachloroethylene tank 14, a crude tetrachloroethylene pump 15, and a heavy component pump 16; the heat supply medium outlet of the economizer 6 is connected to the gas phase feed port of the kettle of the quenching tower 9; the top gas outlet of the quenching tower 9 is connected to the primary condenser 10 and the secondary cryogenic refrigerator 11 in sequence, and the liquid outlet of the primary condenser 10 and the liquid outlet of the secondary cryogenic refrigerator 11 are respectively connected to the tetrachloride The crude carbon tetrachloride tank 12 is connected, the outlet of the crude carbon tetrachloride tank 12 is connected to the inlet of a crude carbon tetrachloride pump 13, and the outlet pipeline of the crude carbon tetrachloride pump 13 is respectively connected to the reflux port of the quench tower 9 and the feed port in the middle of the carbon tetrachloride refining tower 18 of the carbon tetrachloride refining device; the side line extraction pipeline of the quench tower 9 is connected to the crude tetrachloroethylene tank 14, and the outlet of the crude tetrachloroethylene tank 14 is connected to the lower feed port of the tetrachloroethylene light removal tower 23 of the tetrachloroethylene refining device through a crude tetrachloroethylene pump 15; the kettle outlet of the quench tower 9 is connected to the heavy component pump 16 to discharge the heavy component.

[0125] The carbon tetrachloride refining device comprises a carbon tetrachloride refining tower 18, a carbon tetrachloride refining tower reboiler 17, a carbon tetrachloride refining tower condenser 19, a carbon tetrachloride refining tower reflux tank 20, a carbon tetrachloride refining tower reflux pump 21, and a carbon tetrachloride refining tower kettle pump 22; the top gas outlet of the carbon tetrachloride refining tower 18 is connected to the inlet of the carbon tetrachloride refining tower condenser 19 (using water as a cooling medium), and the non-condensable gas outlet of the carbon tetrachloride refining tower condenser 19 is connected to the suction pipe port of the venturi ejector 3. The liquid outlet of the carbon tetrachloride refining tower condenser 19 is connected to the inlet of the carbon tetrachloride refining tower reflux tank 20, the outlet of the carbon tetrachloride refining tower reflux tank 20 is connected to the carbon tetrachloride refining tower reflux pump 21, and the outlet of the carbon tetrachloride refining tower reflux pump 21 is respectively connected to the reflux port of the carbon tetrachloride refining tower 18 and the inlet of the diluent vaporizer 4; the tower kettle outlet of the carbon tetrachloride refining tower 18 is connected to the upper feed port of the tetrachloroethylene light removal tower 23 of the tetrachloroethylene refining device through the carbon tetrachloride refining tower kettle pump 22;

[0126] The tetrachloroethylene refining device comprises a tetrachloroethylene light-removing tower 23, a tetrachloroethylene light-removing tower top condenser 24, a tetrachloroethylene light-removing tower reflux tank 25, a tetrachloroethylene light-removing tower reflux pump 26, a tetrachloroethylene light-removing tower reboiler 27, a tetrachloroethylene light-removing tower kettle pump 28, a tetrachloroethylene low-pressure tower 29, a tetrachloroethylene low-pressure tower top condenser 30, a tetrachloroethylene low-pressure tower reflux tank 31, a tetrachloroethylene low-pressure tower reflux pump 32, a tetrachloroethylene thermal coupling reboiler 33, a tetrachloroethylene low-pressure tower kettle pump 34, a tetrachloroethylene high-pressure tower 35, a tetrachloroethylene high-pressure tower top condenser 38, a tetrachloroethylene high-pressure tower reflux Flow tank 39, tetrachloroethylene high-pressure tower reflux pump 40, tetrachloroethylene high-pressure tower reboiler 36, tetrachloroethylene high-pressure tower kettle pump 37, tetrachloroethylene product cooler 41; the tetrachloroethylene light removal tower 23 is provided with an upper feed inlet and a lower feed inlet; the upper feed inlet of the tetrachloroethylene light removal tower 23 is connected to the tower kettle outlet of the carbon tetrachloride refining tower 18 through the carbon tetrachloride refining tower kettle pump 22, and the lower feed inlet is connected to the tetrachloroethylene crude product tank 14 through the crude tetrachloroethylene pump 15; the top gas outlet of the tetrachloroethylene light removal tower 23 is connected to the top condenser 24 of the tetrachloroethylene light removal tower (using water as the cooling medium) The inlet of the tetrachloroethylene light-removing tower is connected, the non-condensable gas outlet of the tetrachloroethylene light-removing tower top condenser 24 is connected to the suction pipe port of the venturi ejector 3, the liquid outlet of the tetrachloroethylene light-removing tower top condenser 24 is connected to the inlet of the tetrachloroethylene light-removing tower reflux tank 25, and the outlet of the tetrachloroethylene light-removing tower reflux tank 25 is connected to the reflux port of the tetrachloroethylene light-removing tower 23 through the tetrachloroethylene light-removing tower reflux pump 26; the tower kettle outlet of the tetrachloroethylene light-removing tower 23 is connected to the feed port of the tetrachloroethylene low-pressure tower 29 through the tetrachloroethylene light-removing tower kettle pump 28; the top gas outlet of the tetrachloroethylene low-pressure tower 29 is connected to the inlet of the tetrachloroethylene low-pressure tower The inlet of the top condenser 30 (using water as the cooling medium) is connected, the liquid outlet of the tetrachloroethylene low-pressure tower top condenser 30 is connected to the inlet of the tetrachloroethylene low-pressure tower reflux tank 31, the outlet of the tetrachloroethylene low-pressure tower reflux tank 31 is connected to the inlet of the tetrachloroethylene low-pressure tower reflux pump 32, and the outlet of the tetrachloroethylene low-pressure tower reflux pump 32 is respectively connected to the reflux port of the tetrachloroethylene low-pressure tower 29 and the inlet of the tetrachloroethylene product cooler 41 (using water as the cooling medium); the tower kettle outlet of the tetrachloroethylene low-pressure tower 29 is connected to the feed port of the tetrachloroethylene high-pressure tower 35 via the tetrachloroethylene low-pressure tower kettle pump 34;The top gas outlet of the tetrachloroethylene high-pressure tower 35 is connected to the heating medium inlet of the tetrachloroethylene thermal coupling reboiler 33, the heating medium outlet of the tetrachloroethylene thermal coupling reboiler 33 is connected to the inlet of the tetrachloroethylene high-pressure tower top condenser 38 (using water as the cooling medium), the liquid outlet of the tetrachloroethylene high-pressure tower top condenser 38 is connected to the inlet of the tetrachloroethylene high-pressure tower reflux tank 39, the outlet of the tetrachloroethylene high-pressure tower reflux tank 39 is connected to the inlet of the tetrachloroethylene high-pressure tower reflux pump 40, the outlet of the tetrachloroethylene high-pressure tower reflux pump 40 is respectively connected to the reflux port of the tetrachloroethylene high-pressure tower 35 and the inlet of the tetrachloroethylene product cooler 41, and the high-purity tetrachloroethylene product is extracted from the tetrachloroethylene product cooler 41; the tower kettle outlet of the tetrachloroethylene high-pressure tower 35 is connected to the tower kettle feed port of the quenching tower 9 through the tetrachloroethylene high-pressure tower kettle pump 37. ;

[0127] The continuous synthesis process of high-purity tetrachloroethylene based on the equipment of this embodiment includes:

[0128] Step (1), chlorination synthesis: the feed mass ratio of methyl chloroethane to dichloromethane is 1:1.2, the total feed flow mass ratio of methyl chloroethane and dichloromethane to the feed flow mass ratio of chlorine is 1:1.4, and the feed flow mass ratio of carbon tetrachloride to chlorine is 3:1; the electric heater of the chlorination reaction kettle is turned on and the temperature is raised to 500° C.; carbon tetrachloride (purity 95%wt, temperature 30° C., pressure 0.5MPaG) is vaporized through a diluent vaporizer 4 (temperature 150° C., pressure 0.3MPaG), chlorine (purity 99.2%wt, temperature 90° C., The raw material methyl chloride (purity 99.5%wt, temperature 90°C, pressure 0.6MPaG) is passed through the venturi ejector 3, mixed with the vaporized carbon tetrachloride, and continuously enters the raw material mixer of the chlorination reaction kettle 5 from the top; the raw material methyl chloride (purity 99.5%wt, temperature 90°C, pressure 0.6MPaG) is passed through the first superheater 1 (temperature 140°C, pressure 0.6MPaG) for superheating treatment, and the raw material methylene chloride (purity 99.5%wt, temperature 100°C, pressure 0.6MPaG) is passed through the second superheater 2 (temperature 140°C, pressure 0.6MPaG) for superheating treatment. The superheated chloroform and the superheated dichloromethane are mixed and continuously enter the raw material mixer of the chlorination reactor 5 symmetrically from the left and right sides. The chloroform, dichloromethane, chlorine and carbon tetrachloride are mixed in the material exchange mixer and enter the tube array from the upper head. In the tube array, the chloroform and dichloromethane react with excess chlorine to generate carbon tetrachloride. The material is discharged from the lower end of the tube array and enters the lower head. It is mixed with a small amount of superheated dichloromethane (accounting for 2% of the total amount of dichloromethane) added to the lower head of the chlorination reactor and enters the cylinder from the connecting hole of the lower tube plate. Carbon tetrachloride is generated in the cylinder. The reaction gas discharged from the chlorination reactor (temperature 550°C, pressure 0.07MPaG, tetrachloroethylene mass fraction 25%) enters the economizer 6 (temperature 300°C, pressure 0.07MPaG) and then enters the quenching tower 9 from the bottom after heat exchange with the heat transfer oil. The heat transfer oil is heated to a temperature of 180°C, and then heated to 240°C by the electric heater 42. The heat transfer oil is respectively supplied to the reboiler 17 of the carbon tetrachloride refining tower, the reboiler 27 of the tetrachloroethylene light removal tower, and the reboiler 36 of the tetrachloroethylene high-pressure tower for heat supply, and then returns to the heat transfer oil tank 7, saving 50% of energy;

[0129] Step (2), cooling and washing: the gas phase at the top of the quench tower 9 (plate tower, tower bottom operating temperature 170°C, 0.07MPaG, reflux ratio 4) is sequentially condensed through a primary condenser 10 (condensed to a temperature of 35°C, a gas-liquid mixed pressure of 0.06MPaG) and a secondary deep freezer 11 (condensed to a temperature of -15°C, a gas-liquid mixed pressure of 0.06MPaG) to obtain a liquid phase crude carbon tetrachloride, which enters a crude carbon tetrachloride tank 12, and the uncondensed Hydrogen chloride (content 98.2%) is discharged from the gas outlet of the secondary cryogenic freezer 11 to the downstream system; part of the crude carbon tetrachloride is refluxed into the quench tower 9, and the rest is transported to the carbon tetrachloride refining tower 18; the quench tower 9 extracts tetrachloroethylene (temperature 106°C, pressure 0.02MPaG) from the 8th tower plate side away from the tower bottom to the crude tetrachloroethylene tank 14, and enters the tetrachloroethylene light removal tower 23 from the lower feed port through the crude tetrachloroethylene pump 15, and the heavy component of the tower bottom of the quench tower 9 is transported to the outside through the heavy component pump 16;

[0130] Step (3), refining of carbon tetrachloride: the crude carbon tetrachloride enters a carbon tetrachloride refining tower 18 (a plate tower, a tower top operating temperature of 85° C., a pressure of 2 KPaG, and a reflux ratio of 15), the tower top gas phase is condensed by a carbon tetrachloride refining tower condenser 19, and part of the carbon tetrachloride qualified product (temperature 42° C., content 99.5%) is extracted, and after being vaporized by a diluent vaporizer 4, it returns to the chlorination reaction kettle, and the uncondensed gas (temperature 42° C.) returns to the chlorination reaction kettle through a venturi ejector 3; the heavy component (temperature 92° C.) is extracted from the tower kettle of the carbon tetrachloride refining tower 18, and enters a tetrachloroethylene light-removing tower 23 from an upper feed port through a carbon tetrachloride refining tower kettle pump 22;

[0131] Step (4), tetrachloroethylene refining: the crude tetrachloroethylene and the heavy components extracted from the kettle of the carbon tetrachloride refining tower enter the tetrachloroethylene light-removing tower 23 (plate tower, tower top operating temperature 95°C, pressure 2KPaG, reflux ratio 65), the tower top gas phase is condensed by the tetrachloroethylene light-removing tower top condenser 24, the gas phase light components (temperature 52°C) are extracted and sent to the venturi ejector, and then returned to the chlorination reaction kettle; the tetrachloroethylene light-removing tower kettle extracts tetrachloroethylene (temperature 125°C), which is transported to the tetrachloroethylene low-pressure tower 29 (plate tower, tower top operating temperature 120°C, pressure 2KPaG, reflux ratio 23) through the tetrachloroethylene light-removing tower kettle pump 28, the tetrachloroethylene low-pressure tower top gas phase is condensed by the tetrachloroethylene low-pressure tower top condenser 30, part of which is extracted as the tetrachloroethylene product (temperature 85°C), and the tetrachloroethylene low-pressure tower tower is used for the chlorination reaction. The tetrachloroethylene containing heavy components is extracted from the kettle (temperature 145°C) and transported to the tetrachloroethylene high-pressure tower 35 (plate tower, tower top operating temperature 190°C, pressure 0.25 MPaG, reflux ratio 25) through the tetrachloroethylene low-pressure tower kettle pump 34. The top gas phase of the tetrachloroethylene high-pressure tower first enters the tetrachloroethylene thermal coupling reboiler 33 for heat exchange and then enters the tetrachloroethylene high-pressure tower top condenser 38 for condensation. Part of it is extracted as the tetrachloroethylene product (temperature 165°C). The tetrachloroethylene product extracted from the tetrachloroethylene high- and low-pressure towers passes through the tetrachloroethylene product cooler (temperature 35°C) and is extracted out of the boundary as a product. The purity of the tetrachloroethylene product is 99.98% and the yield is 92%. The heavy components (temperature 195°C) are extracted from the kettle of the tetrachloroethylene high-pressure tower and transported by the tetrachloroethylene high-pressure tower kettle pump 37 to enter the quenching tower 9 from the bottom.

[0132] Example 2

[0133] The continuous synthesis process of high-purity tetrachloroethylene based on the equipment of Example 1 comprises:

[0134] Step (1), chlorination synthesis: the feed mass ratio of methyl chloroethane to dichloromethane is 1:1, the total feed flow mass ratio of methyl chloroethane and dichloromethane to the feed flow mass ratio of chlorine is 1:1.6, and the feed flow mass ratio of carbon tetrachloride to chlorine is 4:1; the electric heater of the chlorination reaction kettle is turned on and the temperature is raised to 500° C.; carbon tetrachloride (purity 97%wt, temperature 30° C., pressure 0.5MPaG) is vaporized through a diluent vaporizer 4 (temperature 160° C., pressure 0.3MPaG), and chlorine (purity 99.5%wt, temperature 95° C., pressure 0 .8MPaG) passes through the venturi ejector 3, is mixed with the vaporized carbon tetrachloride, and continuously enters the raw material mixer of the chlorination reaction kettle 5 from the top; the raw material methyl chloride (purity 99.5%wt, temperature 70°C, pressure 0.7MPaG) is passed into the first superheater 1 (temperature 145°C, pressure 0.6MPaG) for superheating treatment, and the raw material dichloromethane (purity 99.5%wt, temperature 110°C, pressure 0.7MPaG) is passed into the second superheater 2 (temperature 145°C, pressure 0.6MPaG) for superheating treatment. The hot first raw material is mixed with the overheated second raw material, and continuously enters the raw material mixer of the chlorination reactor 5 symmetrically from the left and right sides. Methyl chloride, dichloromethane, chlorine and carbon tetrachloride are mixed in the material exchange mixer and enter the tube array from the upper head. In the tube array, methyl chloride, dichloromethane and excess chlorine react to generate carbon tetrachloride. The material is discharged from the lower end of the tube array and enters the lower head. It is mixed with a small amount of overheated dichloromethane (accounting for 2% of the total amount of dichloromethane) added to the lower head of the chlorination reactor, and enters the shell side from the connecting hole of the lower tube plate. Carbon tetrachloride generates tetrachloroethylene in the shell side. The reaction gas (temperature 560°C, pressure 0.08MPaG, tetrachloroethylene content 28%) discharged from the chlorination reactor enters the economizer 6 to exchange heat with the heat transfer oil. The reaction gas (temperature 305°C, pressure 0.08MPaG) after heat exchange enters the quenching tower 9 from the bottom, the heat transfer oil is heated to a temperature of 185°C, and then further heated to 240°C by the electric heater 42, and respectively supplied to the reboiler 17 of the carbon tetrachloride refining tower, the reboiler 27 of the tetrachloroethylene light removal tower, and the reboiler 36 of the tetrachloroethylene high-pressure tower for heat supply, and then returns to the heat transfer oil tank 7, saving 54%;

[0135] Step (2), cooling and washing: the gas phase at the top of the quench tower 9 (plate tower, tower bottom operating temperature 175°C, 0.08 MPaG, reflux ratio 8) is sequentially condensed through a primary condenser 10 (temperature 40°C, pressure 0.07 MPaG) and a secondary deep freezer 11 (temperature -20°C, pressure 0.07 MPaG) to obtain a liquid phase crude carbon tetrachloride. The crude carbon tetrachloride enters a crude carbon tetrachloride tank 12, and the uncondensed hydrogen chloride (content 98.9 %) is discharged from the gas outlet of the secondary cryogenic device 11 to the downstream system; the crude carbon tetrachloride is partially refluxed into the quench tower 9, and the rest is transported to the carbon tetrachloride refining tower 18; the quench tower 9 extracts tetrachloroethylene (temperature 110°C, pressure 0.05MPaG) from the 8th plate side of the tower bottom to the crude tetrachloroethylene tank 14, and enters the tetrachloroethylene light removal tower 23 from the lower feed port through the crude tetrachloroethylene pump 15, and the heavy component of the tower bottom of the quench tower 9 is transported to the outside through the heavy component pump 16;

[0136] Step (3), refining of carbon tetrachloride: the crude carbon tetrachloride enters a carbon tetrachloride refining tower 18 (a plate tower, a tower top operating temperature of 90° C., a pressure of 3 KPaG, and a reflux ratio of 18), the tower top gas phase is condensed by a carbon tetrachloride refining tower condenser 19, and part of the carbon tetrachloride qualified product (temperature 45° C., content: 99.6%) is extracted, and after being vaporized by a diluent vaporizer 4, it returns to the chlorination reaction kettle, and the uncondensed gas (temperature: 45° C.) enters a venturi ejector 3 and returns to the chlorination reaction kettle; the heavy component (temperature 98° C.) is extracted from the tower kettle of the carbon tetrachloride refining tower 18, and enters a tetrachloroethylene light-removing tower 23 from an upper feed port through a carbon tetrachloride refining tower kettle pump 22;

[0137] Step (4), tetrachloroethylene refining: the crude tetrachloroethylene and the heavy components extracted from the kettle of the carbon tetrachloride refining tower enter the tetrachloroethylene light-removing tower 23 (plate tower, tower top operating temperature 98°C, pressure 3KPaG, reflux ratio 70), the top gas phase is condensed by the tetrachloroethylene light-removing tower top condenser 24, the gas phase light components (temperature 55°C) are extracted and sent to the venturi ejector, and then returned to the chlorination reaction kettle; the tetrachloroethylene light-removing tower kettle extracts tetrachloroethylene (temperature 130°C), which is transported to the tetrachloroethylene low-pressure tower 29 (plate tower, tower top operating temperature 130°C, pressure 3KPaG, reflux ratio 25) through the tetrachloroethylene light-removing tower kettle pump 28, the top gas phase of the tetrachloroethylene low-pressure tower is condensed by the tetrachloroethylene low-pressure tower top condenser 30, part of which is extracted as the tetrachloroethylene product (temperature 90°C), and the tetrachloroethylene low-pressure tower is used as the tower. The tetrachloroethylene containing heavy components is extracted from the kettle (temperature 150°C) and transported to the tetrachloroethylene high-pressure tower 35 (plate tower, tower top operating temperature 195°C, pressure 0.3MPaG, reflux ratio 27) through the tetrachloroethylene low-pressure tower kettle pump 34. The top gas phase of the tetrachloroethylene high-pressure tower first enters the tetrachloroethylene thermal coupling reboiler 33 for heat exchange and then enters the tetrachloroethylene high-pressure tower top condenser 38 for condensation. Part of it is extracted as the tetrachloroethylene product (temperature 170°C). The tetrachloroethylene product extracted from the tetrachloroethylene high- and low-pressure towers passes through the tetrachloroethylene product cooler (temperature 40°C) and is extracted out of the boundary as a product. The purity of the tetrachloroethylene product is 99.99% and the yield is 95.4%. The heavy components (temperature 200°C) are extracted from the kettle of the tetrachloroethylene high-pressure tower and transported by the tetrachloroethylene high-pressure tower kettle pump 37 to enter the quenching tower 9 from the bottom.

[0138] Example 3

[0139] The continuous synthesis process of high-purity tetrachloroethylene based on the equipment of Example 1 comprises:

[0140] Step (1), chlorination synthesis: the feed mass ratio of methyl chloroethane to dichloromethane is 1.2:1, the total feed flow mass ratio of methyl chloroethane and dichloromethane to the feed flow mass ratio of chlorine is 1:1.8, and the feed flow mass ratio of carbon tetrachloride to chlorine is 2:1; the electric heater of the chlorination reaction kettle is turned on and the temperature is raised to 500° C.; carbon tetrachloride (purity 97%wt, temperature 30° C., pressure 0.5MPaG) is vaporized through a diluent vaporizer 4 (temperature 185° C., pressure 0.4MPaG), and chlorine (purity 99.5%wt, temperature 95° C., The raw material methyl chloride (purity 99.5%wt, temperature 70°C, pressure 0.7MPaG) is passed through the venturi ejector 3, mixed with the vaporized carbon tetrachloride, and continuously enters the raw material mixer of the chlorination reaction kettle 5 from the top; the raw material methyl chloride (purity 99.5%wt, temperature 70°C, pressure 0.7MPaG) is passed through the first superheater 1 (temperature 150°C, pressure 0.6MPaG) for superheating treatment, and the raw material methylene chloride (purity 99.5%wt, temperature 100°C, pressure 0.7MPaG) is passed through the second superheater 2 (temperature 160°C, pressure 0.6MPaG) for superheating treatment. The superheated chloroform and the superheated dichloromethane are mixed and continuously enter the raw material mixer of the chlorination reactor 5 symmetrically from the left and right sides. The chloroform, dichloromethane, chlorine and carbon tetrachloride are mixed in the material exchange mixer and enter the tube array from the upper head. In the tube array, the chloroform and dichloromethane react with excess chlorine to generate carbon tetrachloride. The material is discharged from the lower end of the tube array and enters the lower head. It is mixed with a small amount of superheated dichloromethane (accounting for 2% of the total amount of dichloromethane) added to the lower head of the chlorination reactor and enters the shell side from the connecting hole of the lower tube plate. Carbon tetrachloride is generated in the shell side. The reaction gas (temperature 610°C, pressure 0.08MPaG, content of tetrachloroethylene 26%) discharged from the tetrachloroethylene chlorination reactor enters the economizer 6 to exchange heat with the heat transfer oil. The reaction gas (temperature 320°C, pressure 0.08MPaG) after heat exchange enters the quenching tower 9 from the bottom, the heat transfer oil is heated to a temperature of 185°C, and then heated to 240°C by the electric heater 42, and respectively supplied to the reboiler 17 of the carbon tetrachloride refining tower, the reboiler 27 of the tetrachloroethylene light removal tower, and the reboiler 36 of the tetrachloroethylene high-pressure tower for heat supply, and then returns to the heat transfer oil tank 7, saving 58% of energy;

[0141] Step (2), cooling and washing: the gas phase at the top of the quench tower 9 (plate tower, tower bottom operating temperature 180°C, 0.08 MPaG, reflux ratio 6) is sequentially condensed through a primary condenser 10 (temperature 50°C, pressure 0.07 MPaG) and a secondary deep freezer 11 (temperature -25°C, pressure 0.07 MPaG) to obtain a liquid phase crude carbon tetrachloride. The crude carbon tetrachloride enters a crude carbon tetrachloride tank 12, and the uncondensed hydrogen chloride (content 97.9 %) is discharged from the gas outlet of the secondary cryogenic device 11 to the downstream system; the crude carbon tetrachloride is partially refluxed into the quench tower 9, and the rest is transported to the carbon tetrachloride refining tower 18; the quench tower 9 extracts tetrachloroethylene (temperature 145°C, pressure 0.05MPaG) from the 9th plate side of the tower bottom to the crude tetrachloroethylene tank 14, and enters the tetrachloroethylene light removal tower 23 from the lower feed port through the crude tetrachloroethylene pump 15, and the heavy component of the tower bottom of the quench tower 9 is transported to the outside through the heavy component pump 16;

[0142] Step (3), refining of carbon tetrachloride: the crude carbon tetrachloride enters a carbon tetrachloride refining tower 18 (a plate tower, with a tower top operating temperature of 95° C., a pressure of 3 KPaG, and a reflux ratio of 20), the tower top gas phase is condensed by a carbon tetrachloride refining tower condenser 19, and part of the carbon tetrachloride qualified product (temperature 45° C., content: 99.6%) is extracted, and after being vaporized by a diluent vaporizer 4, it returns to the chlorination reaction kettle, and the uncondensed gas (temperature: 45° C.) enters a venturi ejector 3 and returns to the chlorination reaction kettle; the heavy component (temperature 110° C.) is extracted from the tower kettle of the carbon tetrachloride refining tower 18, and enters a tetrachloroethylene light-removing tower 23 from an upper feed port through a carbon tetrachloride refining tower kettle pump 22;

[0143] Step (4), tetrachloroethylene refining: the crude tetrachloroethylene and the heavy components extracted from the kettle of the carbon tetrachloride refining tower enter the tetrachloroethylene light-removing tower 23 (plate tower, tower top operating temperature 100°C, pressure 5KPaG, reflux ratio 75), the tower top gas phase is condensed by the tetrachloroethylene light-removing tower top condenser 24, the gas phase light components (temperature 65°C) are extracted into the venturi ejector, and then returned to the chlorination reaction kettle; the tetrachloroethylene light-removing tower kettle extracts tetrachloroethylene (temperature 140°C), which is transported to the tetrachloroethylene low-pressure tower 29 (plate tower, tower top operating temperature 130°C, pressure 5KPaG, reflux ratio 27) through the tetrachloroethylene light-removing tower kettle pump 28, the tetrachloroethylene low-pressure tower top gas phase is condensed by the tetrachloroethylene low-pressure tower top condenser 30, part of which is extracted as the tetrachloroethylene product (temperature 100°C), and the tetrachloroethylene low-pressure tower is used as the chlorination reaction kettle. The tetrachloroethylene containing heavy components is extracted from the tower kettle (temperature 150°C) and transported to the tetrachloroethylene high-pressure tower 35 (plate tower, tower top operating temperature 200°C, pressure 0.5MPaG, reflux ratio 30) through the tetrachloroethylene low-pressure tower kettle pump 34. The top gas phase of the tetrachloroethylene high-pressure tower first enters the tetrachloroethylene thermal coupling reboiler 33 for heat exchange and then enters the tetrachloroethylene high-pressure tower top condenser 38 for condensation. Part of it is extracted as the tetrachloroethylene product (temperature 190°C). The tetrachloroethylene product extracted from the tetrachloroethylene high- and low-pressure towers passes through the tetrachloroethylene product cooler (temperature 40°C) and is extracted out of the boundary as a product. The purity of the tetrachloroethylene product is 99.99% and the yield is 94%. The heavy components (temperature 210°C) are extracted from the tetrachloroethylene high-pressure tower kettle and transported through the tetrachloroethylene high-pressure tower kettle pump 37 to enter the quenching tower 9 from the bottom.

[0144] Example 4

[0145] The continuous synthesis process of high-purity tetrachloroethylene based on the equipment of Example 1 comprises:

[0146] Step (1), chlorination synthesis: the feed mass ratio of methyl chloroethane to dichloromethane is 1:1, the total feed flow mass ratio of methyl chloroethane and dichloromethane to the feed flow mass ratio of chlorine is 1:1.65, and the feed flow mass ratio of carbon tetrachloride to chlorine is 4:1; the electric heater of the chlorination reaction kettle is turned on and the temperature is raised to 500° C.; carbon tetrachloride (purity 97%wt, temperature 30° C., pressure 0.5MPaG) is vaporized through a diluent vaporizer 4 (temperature 160° C., pressure 0.3MPaG), and chlorine (purity 99.5%wt, temperature 95° C., pressure 0.8MPaG) passes through the venturi ejector 3, is mixed with the vaporized carbon tetrachloride, and continuously enters the raw material mixer of the chlorination reaction kettle 5 from the top; the raw material methyl chloride (purity 99.6%wt, temperature 70°C, pressure 0.7MPaG) is passed into the first superheater 1 (temperature 145°C, pressure 0.6MPaG) for superheat treatment, and the raw material methylene chloride (purity 99.6%wt, temperature 110°C, pressure 0.7MPaG) is passed into the second superheater 2 (temperature 145°C, pressure 0.6MPaG) for superheat treatment. Hot chloroform is mixed with superheated dichloromethane, and continuously enters the raw material mixer of the chlorination reactor 5 symmetrically from the left and right sides. Chloromethane, dichloromethane, chlorine and carbon tetrachloride are mixed in the material exchange mixer and enter the tube array from the upper head. In the tube array, chloroform, dichloromethane and excess chlorine react to generate carbon tetrachloride. The material is discharged from the lower end of the tube array and enters the lower head. It is mixed with a small amount of superheated dichloromethane (accounting for 2% of the total amount of dichloromethane) added to the lower head of the chlorination reactor, and enters the shell side from the connecting hole of the lower tube plate. Carbon tetrachloride generates tetrachloroethylene in the shell side. The reaction gas (temperature 560°C, pressure 0.08MPaG, tetrachloroethylene content 28.8%) discharged from the chlorination reactor enters the economizer 6 to exchange heat with the heat transfer oil. The reaction gas (temperature 305°C, pressure 0.08MPaG) after heat exchange enters the quenching tower 9 from the bottom, and the heat transfer oil is heated to a temperature of 185°C, and then further heated to 240°C by the electric heater 42, and respectively supplied to the reboiler 17 of the carbon tetrachloride refining tower, the reboiler 27 of the tetrachloroethylene light removal tower, and the reboiler 36 of the tetrachloroethylene high-pressure tower for heat supply, and then returns to the heat transfer oil tank 7, saving 54%;

[0147] Step (2), cooling and washing: the gas phase at the top of the quench tower 9 (plate tower, tower bottom operating temperature 175°C, 0.08 MPaG, reflux ratio 8) is sequentially condensed through a primary condenser 10 (temperature 40°C, pressure 0.07 MPaG) and a secondary deep freezer 11 (temperature -20°C, pressure 0.07 MPaG) to obtain a liquid phase crude carbon tetrachloride. The crude carbon tetrachloride enters a crude carbon tetrachloride tank 12, and the uncondensed hydrogen chloride (content 98.9 %) is discharged from the gas outlet of the secondary cryogenic device 11 to the downstream system; the crude carbon tetrachloride is partially refluxed into the quench tower 9, and the rest is transported to the carbon tetrachloride refining tower 18; the quench tower 9 extracts tetrachloroethylene (temperature 110°C, pressure 0.05MPaG) from the 8th plate side of the tower bottom to the crude tetrachloroethylene tank 14, and enters the tetrachloroethylene light removal tower 23 from the lower feed port through the crude tetrachloroethylene pump 15, and the heavy component of the tower bottom of the quench tower 9 is transported to the outside through the heavy component pump 16;

[0148] Step (3), refining of carbon tetrachloride: the crude carbon tetrachloride enters a carbon tetrachloride refining tower 18 (a plate tower, a tower top operating temperature of 90° C., a pressure of 3 KPaG, and a reflux ratio of 18), the tower top gas phase is condensed by a carbon tetrachloride refining tower condenser 19, and part of the carbon tetrachloride qualified product (temperature 45° C., content: 99.6%) is extracted, and after being vaporized by a diluent vaporizer 4, it returns to the chlorination reaction kettle, and the uncondensed gas (temperature: 45° C.) enters a venturi ejector 3 and returns to the chlorination reaction kettle; the heavy component (temperature 98° C.) is extracted from the tower kettle of the carbon tetrachloride refining tower 18, and enters a tetrachloroethylene light-removing tower 23 from an upper feed port through a carbon tetrachloride refining tower kettle pump 22;

[0149] Step (4), tetrachloroethylene refining: the crude tetrachloroethylene and the heavy components extracted from the kettle of the carbon tetrachloride refining tower enter the tetrachloroethylene light-removing tower 23 (plate tower, tower top operating temperature 98°C, pressure 3KPaG, reflux ratio 70), the top gas phase is condensed by the tetrachloroethylene light-removing tower top condenser 24, the gas phase light components (temperature 55°C) are extracted and sent to the venturi ejector, and then returned to the chlorination reaction kettle; the tetrachloroethylene light-removing tower kettle extracts tetrachloroethylene (temperature 130°C), which is transported to the tetrachloroethylene low-pressure tower 29 (plate tower, tower top operating temperature 130°C, pressure 3KPaG, reflux ratio 25) through the tetrachloroethylene light-removing tower kettle pump 28, the top gas phase of the tetrachloroethylene low-pressure tower is condensed by the tetrachloroethylene low-pressure tower top condenser 30, part of which is extracted as the tetrachloroethylene product (temperature 90°C), and the tetrachloroethylene low-pressure tower is used as the tower. The tetrachloroethylene containing heavy components is extracted from the kettle (temperature 150°C) and transported to the tetrachloroethylene high-pressure tower 35 (plate tower, tower top operating temperature 195°C, pressure 0.3MPaG, reflux ratio 27) through the tetrachloroethylene low-pressure tower kettle pump 34. The top gas phase of the tetrachloroethylene high-pressure tower first enters the tetrachloroethylene thermal coupling reboiler 33 for heat exchange and then enters the tetrachloroethylene high-pressure tower top condenser 38 for condensation. Part of it is extracted as the tetrachloroethylene product (temperature 170°C). The tetrachloroethylene product extracted from the tetrachloroethylene high- and low-pressure towers passes through the tetrachloroethylene product cooler (temperature 40°C) and is extracted out of the boundary as a product. The purity of the tetrachloroethylene product is 99.99% and the yield is 95.5%. The heavy components (temperature 200°C) are extracted from the kettle of the tetrachloroethylene high-pressure tower and transported by the tetrachloroethylene high-pressure tower kettle pump 37 to enter the quenching tower 9 from the bottom.

[0150] Example 5

[0151] The continuous synthesis process of high-purity tetrachloroethylene based on the equipment of Example 1 comprises:

[0152] Step (1), chlorination synthesis: the feed mass ratio of methyl chloride to methane is 1:1, the total feed flow mass ratio of methyl chloride and methane to the feed flow mass ratio of chlorine is 1:2, and the feed flow mass ratio of carbon tetrachloride to chlorine is 4:1; the electric heater of the chlorination reaction kettle is turned on and the temperature is raised to 500° C.; carbon tetrachloride (purity 97%wt, temperature 30° C., pressure 0.5MPaG) is vaporized through a diluent vaporizer 4 (temperature 160° C., pressure 0.3MPaG), and chlorine (purity 99.5%wt, temperature 95° C., pressure 0. 8MPaG) passes through the venturi ejector 3, is mixed with the vaporized carbon tetrachloride, and continuously enters the raw material mixer of the chlorination reaction kettle 5 from the top; the raw material methyl chloride (purity 99.5%wt, temperature 70°C, pressure 0.7MPaG) is passed into the first superheater 1 (temperature 150°C, pressure 0.6MPaG) for superheating treatment, and the raw material methane (purity 99.5%wt, temperature 110°C, pressure 0.7MPaG) is passed into the second superheater 2 (temperature 150°C, pressure 0.6MPaG) for superheating treatment, The superheated methyl chloride is mixed with the superheated methane, and continuously enters the raw material mixer of the chlorination reactor 5 symmetrically from the left and right sides. The methyl chloride, methane, chlorine and carbon tetrachloride are mixed in the material exchange mixer and enter the tube array from the upper head. In the tube array, the methyl chloride, methane and excess chlorine react to generate carbon tetrachloride. The material is discharged from the lower end of the tube array and enters the lower head. It is mixed with a small amount of superheated methane (accounting for 1% of the total methane) added to the lower head of the chlorination reactor, and enters the shell side from the connecting hole of the lower tube plate. In the shell side, carbon tetrachloride generates tetrachloroethylene, and the chlorination The reaction gas (temperature 565°C, pressure 0.08MPaG, tetrachloroethylene content 28%) discharged from the reactor enters the economizer 6 to exchange heat with the heat transfer oil. The reaction gas (temperature 310°C, pressure 0.08MPaG) after heat exchange enters the quenching tower 9 from the bottom, and the heat transfer oil is heated to a temperature of 190°C, and then further heated to 240°C by the electric heater 42, and respectively supplied to the reboiler 17 of the carbon tetrachloride refining tower, the reboiler 27 of the tetrachloroethylene light removal tower, and the reboiler 36 of the tetrachloroethylene high-pressure tower for heat supply, and then returns to the heat transfer oil tank 7, saving 56% of energy;

[0153] Step (2), cooling and washing: the gas phase at the top of the quench tower 9 (plate tower, tower bottom operating temperature 175°C, 0.08 MPaG, reflux ratio 8) is sequentially condensed through a primary condenser 10 (temperature 40°C, pressure 0.07 MPaG) and a secondary deep freezer 11 (temperature -20°C, pressure 0.07 MPaG) to obtain a liquid phase crude carbon tetrachloride. The crude carbon tetrachloride enters a crude carbon tetrachloride tank 12, and the uncondensed hydrogen chloride (content 98.9 %) is discharged from the gas outlet of the secondary cryogenic device 11 to the downstream system; the crude carbon tetrachloride is partially refluxed into the quench tower 9, and the rest is transported to the carbon tetrachloride refining tower 18; the quench tower 9 extracts tetrachloroethylene (temperature 110°C, pressure 0.05MPaG) from the 8th plate side of the tower bottom to the crude tetrachloroethylene tank 14, and enters the tetrachloroethylene light removal tower 23 from the lower feed port through the crude tetrachloroethylene pump 15, and the heavy component of the tower bottom of the quench tower 9 is transported to the outside through the heavy component pump 16;

[0154] Step (3), refining of carbon tetrachloride: the crude carbon tetrachloride enters a carbon tetrachloride refining tower 18 (a plate tower, a tower top operating temperature of 90° C., a pressure of 3 KPaG, and a reflux ratio of 18), the tower top gas phase is condensed by a carbon tetrachloride refining tower condenser 19, and part of the carbon tetrachloride qualified product (temperature 45° C., content: 99.6%) is extracted, and after being vaporized by a diluent vaporizer 4, it returns to the chlorination reaction kettle, and the uncondensed gas (temperature: 45° C.) enters a venturi ejector 3 and returns to the chlorination reaction kettle; the heavy component (temperature 98° C.) is extracted from the tower kettle of the carbon tetrachloride refining tower 18, and enters a tetrachloroethylene light-removing tower 23 from an upper feed port through a carbon tetrachloride refining tower kettle pump 22;

[0155] Step (4), tetrachloroethylene refining: the crude tetrachloroethylene and the heavy components extracted from the kettle of the carbon tetrachloride refining tower enter the tetrachloroethylene light-removing tower 23 (plate tower, tower top operating temperature 98°C, pressure 3KPaG, reflux ratio 70), the top gas phase is condensed by the tetrachloroethylene light-removing tower top condenser 24, the gas phase light components (temperature 55°C) are extracted and sent to the venturi ejector, and then returned to the chlorination reaction kettle; the tetrachloroethylene light-removing tower kettle extracts tetrachloroethylene (temperature 130°C), which is transported to the tetrachloroethylene low-pressure tower 29 (plate tower, tower top operating temperature 130°C, pressure 3KPaG, reflux ratio 25) through the tetrachloroethylene light-removing tower kettle pump 28, the top gas phase of the tetrachloroethylene low-pressure tower is condensed by the tetrachloroethylene low-pressure tower top condenser 30, part of which is extracted as the tetrachloroethylene product (temperature 90°C), and the tetrachloroethylene low-pressure tower is used as the tower. The tetrachloroethylene containing heavy components is extracted from the kettle (temperature 150°C) and transported to the tetrachloroethylene high-pressure tower 35 (plate tower, tower top operating temperature 195°C, pressure 0.3MPaG, reflux ratio 27) through the tetrachloroethylene low-pressure tower kettle pump 34. The top gas phase of the tetrachloroethylene high-pressure tower first enters the tetrachloroethylene thermal coupling reboiler 33 for heat exchange and then enters the tetrachloroethylene high-pressure tower top condenser 38 for condensation. Part of it is extracted as the tetrachloroethylene product (temperature 170°C). The tetrachloroethylene product extracted from the tetrachloroethylene high- and low-pressure towers passes through the tetrachloroethylene product cooler (temperature 40°C) and is extracted out of the boundary as a product. The purity of the tetrachloroethylene product is 99.99% and the yield is 95.2%. The heavy components (temperature 200°C) are extracted from the kettle of the tetrachloroethylene high-pressure tower and transported by the tetrachloroethylene high-pressure tower kettle pump 37 to enter the quenching tower 9 from the bottom.

Claims

1. A high-purity tetrachloroethylene continuous synthesis equipment, characterized in that: It includes chlorination synthesis unit, energy-saving unit, cooling and washing unit, carbon tetrachloride refining unit and tetrachloroethylene refining unit; The chlorination synthesis device comprises a first superheater, a second superheater, a venturi ejector, a diluent vaporizer, and a chlorination reaction kettle; the chlorination reaction kettle comprises a cylinder, an upper head, a lower head, an upper tube sheet, and a lower tube sheet; a plurality of tubes are arranged between the upper and lower tube sheets, and a plurality of connecting holes are arranged on the lower tube sheet so that the material discharged from the lower end of the tubes enters the shell through the connecting holes; a baffle is arranged in the cylinder; a raw material mixer is arranged on the top feed pipeline of the chlorination reaction kettle, and the raw material mixer comprises a pipeline body, and a feed port is arranged on the top of the pipeline body for chlorine or chlorine and tetrachloride Carbon feeding, the raw material mixer is provided with at least one pair of feeding mechanisms for feeding the mixed gas of the first raw material and the second raw material, each pair of feeding mechanisms includes symmetrically arranged feeding devices, each feeding device includes a plurality of inner extension pipes extending into the pipeline body, and a plurality of distribution holes are respectively opened on both sides of the tube body of the inner extension pipe extending into the pipeline body, and the opening direction is parallel to the vertical section of the raw material mixer; the bottom of the chlorination reactor is provided with a second raw material feeding port; the upper part of the cylinder of the chlorination reactor is provided with a reaction gas outlet; the cylinder of the chlorination reactor is provided with a jacket, and an electric heater is provided in the jacket; The energy-saving device includes an energy saver and a heat-conducting oil tank; The reaction gas outlet of the chlorination reaction kettle is connected to the inlet of the cooling and washing device through an economizer; The cooling and washing device comprises a quenching tower, a primary condenser, a secondary cryogenic freezer, a carbon tetrachloride crude product tank, and a tetrachloroethylene crude product tank; the top gas outlet of the quenching tower is connected to the primary condenser and the secondary cryogenic freezer in sequence, the liquid outlet of the primary condenser and the liquid outlet of the secondary cryogenic freezer are respectively connected to the carbon tetrachloride crude product tank, and the outlet of the carbon tetrachloride crude product tank is respectively connected to the reflux port of the quenching tower and the feed port of the carbon tetrachloride refining device; the side line extraction pipeline of the quenching tower is connected to the lower feed port of the tetrachloroethylene light removal tower of the tetrachloroethylene refining device; The carbon tetrachloride refining device comprises a carbon tetrachloride refining tower, a carbon tetrachloride refining tower reboiler, and a carbon tetrachloride refining tower condenser; the feed port of the carbon tetrachloride refining tower is connected to the outlet of the carbon tetrachloride crude product tank, the gas outlet at the top of the carbon tetrachloride refining tower is respectively connected to the reflux port of the carbon tetrachloride refining tower and the outlet of the diluent vaporizer through the carbon tetrachloride refining tower condenser; the non-condensable gas outlet of the carbon tetrachloride refining tower condenser is connected to the suction pipe port of the venturi ejector; the tower kettle outlet of the carbon tetrachloride refining tower is connected to the upper feed port of the tetrachloroethylene light removal tower of the tetrachloroethylene refining device; The tetrachloroethylene refining device comprises a tetrachloroethylene light-removing tower, a tetrachloroethylene light-removing tower top condenser, a tetrachloroethylene light-removing tower reboiler, a tetrachloroethylene low-pressure tower, a tetrachloroethylene low-pressure tower top condenser, a tetrachloroethylene thermal coupling reboiler, a tetrachloroethylene low-pressure tower kettle pump, a tetrachloroethylene high-pressure tower, a tetrachloroethylene high-pressure tower top condenser, a tetrachloroethylene high-pressure tower reboiler, and a tetrachloroethylene product cooler; the tetrachloroethylene light-removing tower is provided with an upper feed inlet and a lower feed inlet, the lower feed inlet is connected to the quench tower side line extraction pipeline, and the upper feed inlet is connected to the tower kettle outlet of the carbon tetrachloride refining tower; the top gas outlet of the tetrachloroethylene light-removing tower is connected to the reflux port of the tetrachloroethylene light-removing tower through the top condenser of the tetrachloroethylene light-removing tower, and the non-condensable gas outlet of the top condenser of the tetrachloroethylene light-removing tower is connected to the suction pipe outlet of the venturi ejector ; The kettle outlet of the tetrachloroethylene light-removal tower is connected to the feed port of the tetrachloroethylene low-pressure tower; the top gas outlet of the tetrachloroethylene low-pressure tower is respectively connected to the reflux port of the tetrachloroethylene low-pressure tower and the inlet of the tetrachloroethylene product cooler through the tetrachloroethylene low-pressure tower top condenser; the kettle outlet of the tetrachloroethylene low-pressure tower is connected to the feed port of the tetrachloroethylene high-pressure tower; the top gas outlet of the tetrachloroethylene high-pressure tower is connected to the heating medium inlet of the tetrachloroethylene thermal coupling reboiler, the heating medium outlet of the tetrachloroethylene thermal coupling reboiler is connected to the inlet of the tetrachloroethylene high-pressure tower top condenser, and the liquid outlet of the tetrachloroethylene high-pressure tower top condenser is respectively connected to the reflux port of the tetrachloroethylene high-pressure tower and the inlet of the tetrachloroethylene product cooler; the kettle outlet of the tetrachloroethylene high-pressure tower is connected to the feed port of the kettle of the quenching tower.

2. The high-purity tetrachloroethylene continuous synthesis equipment according to claim 1, characterized in that: The discharge ports of the first superheater and the second superheater are respectively connected to a feed main pipe, and the superheated first raw material and the superheated second raw material are mixed in the feed main pipe; the feed main pipe is connected to a feed mechanism of a chlorination reactor via a feed branch pipe; the air intake port of the venturi ejector is respectively connected to a non-condensable gas outlet of a carbon tetrachloride refining tower condenser and a non-condensable gas outlet of a tetrachloroethylene light removal tower top condenser, and the outlet of the venturi ejector is connected to a feed port at the top of the chlorination reactor; the outlet of the diluent vaporizer is connected to an outlet pipeline of the venturi ejector.

3. The high-purity tetrachloroethylene continuous synthesis equipment according to claim 1, characterized in that: The upper and lower adjacent layers of baffles are arranged alternately; one end of the inner extension pipe extending into the raw material mixer is closed or one end of the inner extension pipe extending into the raw material mixer is closed and a number of air outlets with a smaller diameter than the inner extension pipe are opened at the closed end; a heat transfer oil inlet and a heat transfer oil outlet are respectively provided at the upper and lower ends of the jacket, the heat transfer oil inlet is connected to the outlet of the heat transfer oil tank, and the heat transfer oil outlet is connected to the inlet of the heat transfer oil tank.

4. The high-purity tetrachloroethylene continuous synthesis equipment according to claim 1 or 3, characterized in that: The raw material mixer is provided with a pair of feeding mechanisms, which include a symmetrically arranged left feeding device and a right feeding device, the left feeding device and the right feeding device have the same structure, the left feeding device or the right feeding device includes a feeding pipe and a plurality of inner extension pipes, one end of each inner extension pipe is connected to the feeding pipe, and the other end extends into the pipeline body, and one end of the inner extension pipe extending into the pipeline body is closed or one end of the inner extension pipe extending into the pipeline body is closed and 1 to 2 air outlet holes with a smaller aperture than the inner extension pipe diameter are opened at the closed end, and a plurality of distribution holes are opened on both sides of the tube body of the inner extension pipe extending into the raw material mixer, and the opening direction is parallel to the vertical section of the raw material mixer.

5. The high-purity tetrachloroethylene continuous synthesis equipment according to claim 1, characterized in that: The economizer is a flue gas heat exchanger; a heating medium inlet and a heating medium outlet are respectively arranged at both ends of the economizer, and a condenser is arranged inside the economizer as a heat transfer oil channel; the heating medium inlet of the economizer is connected to the reaction gas outlet of the chlorination reactor, and the heating medium outlet is connected to the gas phase feed port of the quench tower kettle; the inlet of the condenser in the economizer is connected to the outlet of the heat transfer oil tank, and the outlet of the condenser is respectively connected to the heating medium inlets of the carbon tetrachloride refining tower reboiler, the tetrachloroethylene light removal tower reboiler, and the tetrachloroethylene high-pressure tower reboiler through an electric heater, and the heating medium outlets of the carbon tetrachloride refining tower reboiler, the tetrachloroethylene light removal tower reboiler, and the tetrachloroethylene high-pressure tower reboiler are respectively connected to the inlet of the heat transfer oil tank.

6. The high-purity tetrachloroethylene continuous synthesis equipment according to claim 1, characterized in that: The side line extraction pipeline of the quench tower is connected to the crude tetrachloroethylene tank; the liquid outlet of the carbon tetrachloride refining tower condenser is connected to the inlet of the carbon tetrachloride refining tower reflux tank, and the outlet of the carbon tetrachloride refining tower reflux tank is respectively connected to the reflux port of the carbon tetrachloride refining tower and the inlet of the diluent vaporizer; the liquid outlet of the top condenser of the tetrachloroethylene light-removing tower is connected to the reflux port of the tetrachloroethylene light-removing tower through the tetrachloroethylene light-removing tower reflux tank; the liquid outlet of the top condenser of the tetrachloroethylene low-pressure tower is connected to the inlet of the tetrachloroethylene low-pressure tower reflux tank, and the outlet of the tetrachloroethylene low-pressure tower reflux tank is respectively connected to the reflux port of the tetrachloroethylene low-pressure tower and the inlet of the tetrachloroethylene product cooler; the liquid outlet of the top condenser of the tetrachloroethylene high-pressure tower is connected to the inlet of the tetrachloroethylene high-pressure tower reflux tank, and the outlet of the tetrachloroethylene high-pressure tower reflux tank is respectively connected to the reflux port of the tetrachloroethylene high-pressure tower and the inlet of the tetrachloroethylene product cooler.

7. A high-purity tetrachloroethylene continuous synthesis process based on the synthesis equipment according to claim 1, characterized in that: The following steps are involved: Step (1), chlorination synthesis: the first raw material and the second raw material are mixed after heat treatment, and are fed from the side of the raw material mixer of the chlorination reactor. The raw chlorine is mixed with vaporized carbon tetrachloride through a venturi injector or the raw chlorine enters the raw material mixer of the chlorination reactor from the top through a venturi injector. The mixed reaction gas in the raw material mixer enters the tube array. The first raw material and the second raw material react with excess chlorine to generate carbon tetrachloride, which is discharged from the lower end of the tube array into the lower head. A small amount of the second raw material is added to the lower head of the chlorination reactor to consume the unreacted chlorine. The material in the lower head enters the shell side from the connecting hole, and carbon tetrachloride generates tetrachloroethylene in the shell side; the reaction gas enters the economizer, exchanges heat with the heat transfer oil, and then enters the quenching tower; Step (2), cooling and washing: the reaction gas enters a quench tower for cooling and washing, the gas phase at the top of the quench tower is sequentially condensed through a primary condenser and a secondary cryogenic freezer to obtain a liquid phase crude carbon tetrachloride product, the crude carbon tetrachloride product enters a crude carbon tetrachloride product tank, part of which is refluxed to the quench tower, and the rest is transported to a carbon tetrachloride refining tower, and the uncondensed hydrogen chloride is discharged from the gas outlet of the secondary cryogenic freezer; the crude tetrachloroethylene product is extracted from the quench tower side line, the crude tetrachloroethylene product enters a crude tetrachloroethylene product tank, and then transported to a tetrachloroethylene light removal tower; Step (3), refining carbon tetrachloride: the crude carbon tetrachloride enters a carbon tetrachloride refining tower for refining, the gas phase at the top of the carbon tetrachloride refining tower is condensed to obtain qualified carbon tetrachloride products, the qualified carbon tetrachloride products are vaporized by a diluent vaporizer and returned to the chlorination reactor, the uncondensed gas is returned to the chlorination reactor via a venturi ejector, and the heavy components in the reactor are transported to a tetrachloroethylene light removal tower; Step (4), tetrachloroethylene refining: the crude tetrachloroethylene and the heavy components in the bottom of the carbon tetrachloride refining tower are introduced into the tetrachloroethylene light removal tower, the gas phase at the top of the tetrachloroethylene light removal tower is condensed, the gas phase is returned to the chlorination reaction kettle through a venturi ejector, the liquid phase is refluxed to the tetrachloroethylene light removal tower, the bottom material of the tetrachloroethylene light removal tower is transported to the tetrachloroethylene low-pressure tower, the gas phase at the top of the tetrachloroethylene low-pressure tower is condensed to produce the tetrachloroethylene product, the bottom material is transported to the tetrachloroethylene high-pressure tower, the gas phase at the top of the tetrachloroethylene high-pressure tower is firstly heat-exchanged with the tetrachloroethylene thermal coupling reboiler, and then the tetrachloroethylene product is produced after condensation, the bottom material is transported to the quenching tower, and the tetrachloroethylene products produced from the tetrachloroethylene high-pressure and low-pressure towers are cooled by the tetrachloroethylene product cooler.

8. The continuous synthesis process of high-purity tetrachloroethylene according to claim 7, characterized in that: In step (1), the first raw material is one or more of methane, methyl chloride, dichloromethane, chloroform, and natural gas; the second raw material can be replaced by one or more of methane, methyl chloride, dichloromethane, chloroform, and natural gas.

9. The continuous synthesis process of high-purity tetrachloroethylene according to claim 7, characterized in that: In step (1), the mass ratio of the carbon tetrachloride to the chlorine feed flow rate is 0:1 to 10:1, preferably 2:1 to 8:1; the mass ratio of the total feed flow rate of the first raw material and the second raw material to the mass ratio of the chlorine feed flow rate is 1:1.4 to 1:3, preferably 1:1.5 to 1:2.6; The temperature of the first superheater is 130-180°C, preferably 140-160°C; The temperature of the second superheater is 130-180°C, preferably 140-160°C; The temperature of the diluent vaporizer is 110-200°C, preferably 150-180°C; The temperature of the chlorination reaction kettle is 500-650°C, preferably 550-600°C, and the pressure of the chlorination reaction kettle is 0.05-0.3MPaG, preferably 0.07-0.12MPaG; After heat exchange, the temperature of the heat transfer oil is 150-260°C, preferably 180-245°C; In step (2), the operating temperature of the quenching tower kettle is 150-230° C., preferably 170-220° C.; the pressure of the quenching tower is 0.04-0.3 MPaG, preferably 0.06-0.12 MPaG; the reflux ratio is 2-20, preferably 3-15; The condensation temperature of the primary condenser is 30 to 70°C, preferably 35 to 50°C; the temperature of the secondary cryogenic freezer is -10 to -40°C, preferably -15 to -25°C; The content of hydrogen chloride is ≥98%; In step (3), the pressure of the carbon tetrachloride refining tower is 0-0.1 MPaG, preferably 0-10 KPaG; the top operating temperature of the carbon tetrachloride refining tower 18 is 80-100° C., preferably 85-95° C.; the reflux ratio is 10-30, preferably 15-20; The content of the qualified carbon tetrachloride product is ≥99%; In step (4), the crude tetrachloroethylene enters the tetrachloroethylene light removal tower from the lower feed inlet; The heavy components in the kettle of the carbon tetrachloride refining tower enter the tetrachloroethylene light removal tower from the upper feed port; The pressure of the tetrachloroethylene light removal tower is 0-0.1 MPaG, preferably 0-10 KPaG; the tower top operating temperature is 90-110°C, preferably 95-100°C; the reflux ratio is 60-90, preferably 65-80; The temperature of the top condenser of the tetrachloroethylene light removal tower is 50-70°C, preferably 55-65°C; The pressure of the tetrachloroethylene low-pressure tower is 0-0.1 MPaG, preferably 0-10 KPaG, the top operating temperature is 110-140°C, preferably 120-130°C; the reflux ratio is 20-30, preferably 23-27; The temperature of the tetrachloroethylene low-pressure tower top condenser is 80-130°C, preferably 90-120°C; The pressure of the tetrachloroethylene high-pressure tower is 0.2-0.5 MPaG, preferably 0.3-0.4 MPaG, the top operating temperature is 180-210°C, preferably 190-200°C, and the reflux ratio is 22-35, preferably 25-30; The temperature of the tetrachloroethylene high-pressure tower top condenser is 160-200°C, preferably 170-190°C; The content of the tetrachloroethylene product is ≥99.98%.

10. The high-purity tetrachloroethylene continuous synthesis process according to claim 7, characterized in that: It also includes heat recovery of heat transfer oil: the heat transfer oil discharged from the economizer is heated by an electric heater and then supplied to a carbon tetrachloride refining device and a tetrachloroethylene refining device for heat supply; the heat transfer oil is heated by the electric heater to a temperature of 230-260°C, preferably 240-250°C.

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