CN111606777B - Preparation method and device of tetrachloroethylene - Google Patents
Preparation method and device of tetrachloroethylene Download PDFInfo
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Abstract
The invention provides a preparation method and a device of tetrachloroethylene, wherein the method comprises the steps of firstly exchanging heat between a high-temperature chlorination reaction product and molten salt to obtain a chlorination reaction product with reduced temperature and molten salt with increased temperature, carrying out quenching treatment on the chlorination reaction product with reduced temperature, and using the molten salt with increased temperature as a heat source to be used at a hot end. The method of the invention stabilizes the operation of the tetrachloroethylene quench tower, reduces the dosage of the quench solvent, recovers part of heat energy, saves energy and reduces consumption.
Description
Technical Field
The invention belongs to the technical field of tetrachloroethylene preparation, and particularly relates to a method and a device for preparing tetrachloroethylene.
Background
Tetrachloroethylene is an organic chlorine solvent, and is used as an important chlorine-consuming product mainly as a metal degreasing agent, a metal cleaning agent, a metal part processing surface treating agent, a solvent, an organic extracting agent, a fabric and wool dry cleaning agent and the like.
Tetrachloroethylene can be prepared by mixing chlorine gas with one or more of natural gas, methyl chloride, methylene chloride, chloroform, carbon tetrachloride, pentachloroethane, hexachloroethane, dichloropropane and hexachlorobutadiene in various proportions. Among them, the tetrachloroethylene-carbon tetrachloride co-decomposition method uses environmentally-friendly carbon tetrachloride as a raw material, and solves the problem of sustainable development of methane chloride, thus becoming the mainstream process of tetrachloroethylene. The process system mainly comprises a chlorination reaction system, a chlorinolysis reaction system, a product rectification system, a hydrogen chloride recovery and chlorine gas circulating system and an auxiliary process unit. In order to maintain the reaction equilibrium achieved and avoid the formation of excessive amounts of by-products, the gaseous product leaving the reactor of the chlorination reaction system enters the bottom of the quench tower and is rapidly cooled by the quench solvent (e.g., carbon tetrachloride) flowing down from the uppermost tray. In the process, liquid rich in tetrachloroethylene is extracted from the lateral line of the quench tower, gas phase extracted from the top of the quench tower is subjected to three-stage condenser to extract non-condensable gas hydrogen chloride, the non-condensable gas hydrogen chloride enters a recovery system, and condensed liquid rich in carbon tetrachloride is obtained and used as a coolant to flow down from a reflux port at the top of the quench tower for recycling.
Disclosure of Invention
The chlorination reaction in the preparation of the tetrachloroethylene by mixing one or more of natural gas, chloromethane, dichloromethane, trichloromethane, carbon tetrachloride, pentachloroethane, hexachloroethane, dichloropropane and hexachlorobutadiene with chlorine in different proportions is a violent exothermic reversible reaction process, and a polychloride (such as hexachlorobenzene, the melting point of which is 230 ℃) with higher melting point is byproduct, so that the existing process is to send the gas of the chlorination reaction with the temperature of 550-600 ℃ into a quenching tower and a low-temperature quenching solvent for heat exchange as soon as possible to reduce the temperature of the gas to be below 100 ℃, but the operation of the method can cause the temperature of the quenching tower to be increased due to insufficient cold energy of the quenching solvent, the proportion of tetrachloroethylene at the tower top is increased, and the product yield is reduced; meanwhile, the high temperature of about 600 ℃ is directly quenched, and high-quality heat energy contained in high-temperature reaction gas is lost.
In order to overcome the defects of the prior art, the invention aims to provide a method and a device for preparing tetrachloroethylene, wherein a high-temperature chlorination reaction product is subjected to heat exchange with molten salt to obtain a chlorination reaction product with a reduced temperature and molten salt with an increased temperature, the chlorination reaction product with the reduced temperature is subjected to quenching treatment, and the molten salt with the increased temperature is used as a heat source to be used at a hot end. By adopting the method, the operation of the tetrachloroethylene quenching tower is stabilized, the dosage of a quenching solvent is reduced, partial heat energy is recovered, and energy conservation and consumption reduction are realized.
The invention aims to realize the following technical scheme:
a process for the preparation of tetrachloroethylene, said process comprising the steps of:
(1) Firstly, carrying out chlorination reaction on raw materials for preparing tetrachloroethylene to obtain a high-temperature chlorination reaction product;
(2) Exchanging heat between the high-temperature chlorination reaction product and the molten salt to obtain a chlorination reaction product with a reduced temperature and the molten salt with an increased temperature;
(3) And carrying out quenching treatment on the chlorination reaction product with the reduced temperature, and using the molten salt with the increased temperature as a heat source to be used at a hot end.
According to the invention, in step (1), the chlorination reaction temperature is 400-700 ℃, such as 400 ℃, 500 ℃, 600 ℃, 700 ℃; the reaction pressure is 0.1-0.2MPa.
According to the invention, in step (1), the chlorination reaction is carried out in a chlorination reactor.
According to the invention, in the step (1), the raw materials for preparing tetrachloroethylene comprise chlorine, carbon tetrachloride and other chlorohydrocarbons; wherein the other chlorinated hydrocarbon is selected from one or more mixtures of methane chloride, methylene chloride, trichloromethane, dichloroethane, trichloroethane, pentachloroethane, hexachloroethane, dichloropropane and hexachlorobutadiene.
According to the invention, in the step (1), the molar ratio of chlorine gas to carbon tetrachloride to other chlorinated hydrocarbons is 3-6.
According to the invention, in the step (1), the high-temperature chlorination reaction product contains tetrachloroethylene, unconverted other chlorohydrocarbons, carbon tetrachloride and chlorine, by-product hydrogen chloride, by-product polychlorides (such as hexachloropropane, hexachlorobutadiene, hexachlorobenzene and the like) and the like.
According to the invention, in the step (2), the molten salt refers to a molten mass formed after the salt is melted; for example, a melt of halides, nitrates, nitrites, sulfates of alkali metals, alkaline earth metals; also for example, it is a binary molten salt composed of 55wt% potassium nitrate and 45wt% sodium nitrite.
According to the invention, in step (2), the temperature of the molten salt before heat exchange is 250-350 ℃, such as 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃, 350 ℃; the temperature of the molten salt after heat exchange is 300-450 deg.C, such as 300 deg.C, 310 deg.C, 320 deg.C, 330 deg.C, 340 deg.C, 350 deg.C, 360 deg.C, 370 deg.C, 380 deg.C, 390 deg.C, 400 deg.C, 410 deg.C, 420 deg.C, 430 deg.C, 440 deg.C, 450 deg.C. In the invention, the fused salt (the temperature of the fused salt is generally 250-350 ℃) is used as a heat exchange medium, the temperature of a heat exchange interface is not lower than the melting point of the by-product, and the by-product can be effectively prevented from being separated out.
According to the present invention, in the step (2), the temperature of the high temperature chlorination reaction product before heat exchange is 400 to 700 ℃, such as 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, and the temperature of the chlorination reaction product after heat exchange is 300 to 500 ℃, such as 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃, 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃, 420 ℃, 430 ℃, 440 ℃, 450 ℃, 480 ℃, 500 ℃.
According to the present invention, in the step (3), the quenching treatment is carried out in a quenching tower.
According to the present invention, in the step (3), the quenching treatment is performed using a quenching solvent selected from carbon tetrachloride. Wherein, the carbon tetrachloride can be fresh carbon tetrachloride or carbon tetrachloride in raw materials for preparing tetrafluoroethylene, such as condensate at the top of a quenching tower in quenching treatment.
According to the invention, in the step (3), a gas phase component, a liquid phase component and a heavy component are obtained after quenching treatment; for example, a gas phase component is obtained at the top of a quenching tower, a heavy component is obtained at the bottom of the quenching tower, and a liquid phase component is obtained at the lateral line of the quenching tower; the gas phase component contains hydrogen chloride, chlorine, carbon tetrachloride and tetrachloroethylene; and condensing the gas phase component to obtain a condensate and a non-condensable gas, returning the condensate to a quenching treatment step (such as returning to a quenching tower), and further treating the non-condensable gas, the heavy component and the liquid phase component.
And (3) wherein the non-condensable gas contains hydrogen chloride, chlorine and carbon tetrachloride, further separation and hydrogen chloride recovery are carried out, and the chlorine and the carbon tetrachloride are returned to the step (1) for reuse.
Wherein the condensate contains carbon tetrachloride and tetrachloroethylene and returns to the step of quenching treatment (such as a quenching tower).
Wherein the liquid phase component contains tetrachloroethylene and carbon tetrachloride, and is further separated, the tetrachloroethylene is recovered, and the carbon tetrachloride is returned to the step (1) for reuse.
Wherein, the heavy component contains polychloride and carbon tetrachloride, and is further separated, the polychloride is recovered, and the carbon tetrachloride is returned to the step (1) for recycling.
The invention also provides a device for implementing the method, which comprises a chlorination reactor, a heat exchanger, a quenching tower and a condenser; the chlorination reactor is connected with a heat exchanger, the heat exchanger is connected with the lower part of a quenching tower, and a condenser is arranged at the top of the quenching tower.
According to the invention, the bottom of the quenching tower is provided with a first pipeline for discharging heavy components in the quenching tower, wherein the heavy components comprise polychloride and carbon tetrachloride.
According to the invention, a second pipeline is arranged on the side line of the quenching tower and is used for discharging liquid components, the second pipeline can be connected with a tetrachloroethylene recovery device, the liquid components comprise tetrachloroethylene and carbon tetrachloride for example, and the tetrachloroethylene recovery device is used for returning the carbon tetrachloride to the chlorination reactor after further separating and recovering the tetrachloroethylene.
According to the invention, a third pipeline is arranged at the top of the quenching tower and used for discharging gas-phase components, the third pipeline can be connected with a condenser, the gas-phase components are condensed by the condenser, and the obtained condensate containing carbon tetrachloride and tetrachloroethylene returns to the quenching tower; the non-condensable gas contains hydrogen chloride, chlorine and carbon tetrachloride, and the chlorine and the carbon tetrachloride return to the chlorination reactor after the hydrogen chloride is further separated and recovered.
The invention has the beneficial effects that:
the invention provides a preparation method and a device of tetrachloroethylene, wherein the method comprises the steps of firstly exchanging heat between a high-temperature chlorination reaction product and molten salt to obtain a chlorination reaction product with a reduced temperature and the molten salt with an increased temperature, carrying out quenching treatment on the chlorination reaction product with the reduced temperature, and using the molten salt with the increased temperature as a heat source to be used at a hot end. By adopting the method, the operation of the tetrachloroethylene quench tower is stabilized, the consumption of the quench solvent is reduced, partial heat energy is recovered, and energy conservation and consumption reduction are realized.
Drawings
FIG. 1 is a flow chart of a process for preparing tetrachloroethylene.
Reference numerals are as follows: r, chlorination reactor, C, condenser, E, heat exchanger, T, quench tower, 1, chlorine, 2, carbon tetrachloride, 3, chlorohydrocarbon, 4, high-temperature reaction gas, 5, heat exchange cooling back reaction gas, 6, molten salt feeding, 7, molten salt discharging, 8, quench tower top gas phase stream, 9, quench tower top condensate, 10, quench tower top noncondensable gas, 11, side draw tetrachloroethylene crude product, 12, quench tower bottom heavy component.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
The process flow diagram used in the following examples is as follows:
the device for producing tetrafluoroethylene comprises a chlorination reactor R, a heat exchanger E, a quench tower T and a condenser C; the chlorination reactor R is connected with a heat exchanger E, the heat exchanger E is connected with the lower part of a quenching tower T, and a condenser C is arranged at the top of the quenching tower T;
chlorine 1, carbon tetrachloride 2 and chlorohydrocarbon 3 are fed into a chlorination reactor R to carry out chlorination reaction to obtain high-temperature reaction gas 4, the high-temperature reaction gas 4 passes through a heat exchanger E and then exchanges heat with molten salt in the heat exchanger E to obtain reaction gas 5 after heat exchange and temperature reduction; fused salt in the heat exchanger E gets into from fused salt feeding 6, discharge from fused salt ejection of compact 7, reaction gas 5 gets into quench tower T after the heat transfer cooling and carries out the quench treatment, through the quench treatment back, quench tower top of the tower obtains quench tower top of the tower gas-phase commodity circulation 8, this quench tower top of the tower gas-phase commodity circulation 8 obtains quench tower top condensate 9 backward flow through condenser C condensation after, quench tower top of the tower noncondensable gas 10 goes for further processing, quench tower side draw tetrachloroethylene crude 11, obtain quench tower bottom of the tower heavy component 12.
Example 1
Take a tetrachloroethylene apparatus with the capacity of 5 ten thousand tons/year as an example.
The reaction raw materials are chlorine, carbon tetrachloride and dichloropropane, and the chlorine, the carbon tetrachloride and the dichloropropane are added into a chlorination reactor for reaction, the temperature of the chlorination reactor is 560 ℃, the high-temperature reaction gas with 0.17MPa, the flow rate is 2400 kg/h, and the chlorination reactor comprises 44.2wt% of carbon tetrachloride, 2.0wt% of chlorine, 21.1wt% of hydrogen chloride, 28.1wt% of tetrachloroethylene, 2.2wt% of hexachloroethane and 2.4wt% of hexachlorobenzene.
The high temperature reaction gas enters the heat exchanger E to exchange heat with 12000kg/h of molten salt, the molten salt composition is 55 percent by weight of potassium nitrate and 45 percent by weight of sodium nitrite; the feeding temperature of the molten salt is 300 ℃, the temperature of the molten salt obtained after heat exchange is 495 ℃, and the temperature of the high-temperature molten salt after heat exchange is reduced to 300 ℃ for recycling.
Reducing the temperature of the reaction gas after heat exchange to 350 ℃, feeding the reaction gas into a quenching tower from the bottom of the quenching tower, carrying out quenching treatment, obtaining 42700kg/h of gas-phase product with the temperature of 98 ℃ from the top of the tower, carrying out heat exchange in a condenser C, obtaining 28500kg/h of condensate with the temperature of 50 ℃ after heat exchange, wherein the content of carbon tetrachloride is 91wt%, and taking the condensate as reflux liquid to return to the quenching tower from the top of the quenching tower; the tower top noncondensable gas is 14145kg/h for further cooling and separating hydrogen chloride, chlorine and carbon tetrachloride; 4955kg/h of crude tetrachloroethylene is extracted from a side line, wherein the crude tetrachloroethylene contains 91wt% of tetrachloroethylene and 9wt% of carbon tetrachloride, and tetrachloroethylene is removed for refining treatment; 5400kg/h of heavy component substances are extracted from the tower bottom, wherein the heavy component substances comprise 44wt% of tetrachloroethylene, 48wt% of hexachloride and 8wt% of carbon tetrachloride, and the heavy component removing treatment unit is used for further separation.
Comparative example 1
Take a tetrachloroethylene apparatus with the capacity of 5 ten thousand tons/year as an example.
The reaction raw materials are a mixture of chlorine, carbon tetrachloride and dichloropropane which are added into a chlorination reactor for reaction, the temperature of the chlorination reactor is 560 ℃, the high-temperature reaction gas with 0.17MPa is 2450 kg/h, and the chlorination reactor comprises 44.2wt% of carbon tetrachloride, 2.0wt% of chlorine, 21.1wt% of hydrogen chloride, 28.1wt% of tetrachloroethylene, 2.2wt% of hexachloroethane and 2.4wt% of hexachlorobenzene.
High-temperature reaction gas enters a quenching tower from the bottom of the quenching tower, gas-phase products with the temperature of 98 ℃ are obtained at the top of the quenching tower after quenching treatment, the gas-phase products with the temperature of 61700kg/h are sent to a condenser C for heat exchange, condensate with the temperature of 50 ℃ is obtained after heat exchange, wherein the content of carbon tetrachloride is 91wt%, and the condensate is used as reflux liquid and enters the quenching tower from the top of the quenching tower again; the tower top noncondensable gas is 14150kg/h for further cooling and separating hydrogen chloride, chlorine and carbon tetrachloride; 4960kg/h of crude tetrachloroethylene is extracted from a side line, wherein the crude tetrachloroethylene contains 90.6wt% of tetrachloroethylene and 8.4wt% of carbon tetrachloride, and tetrachloroethylene is removed for refining treatment; 5400kg/h of heavy component substances are extracted from the tower bottom, wherein the heavy component substances comprise 44wt% of tetrachloroethylene, 48wt% of hexachloride and 8wt% of carbon tetrachloride, and the heavy component removing treatment unit is used for further treatment.
It can be seen from comparative example 1 that the reaction gas enters the quenching tower after heat exchange and temperature reduction, the output of tetrachloroethylene is not influenced, but the load of a condenser at the top of the quenching tower is obviously reduced, and the reflux liquid amount only needs 28500/47500 multiplied by 100% =60%, so that the gas phase temperature at the top of the tower can be ensured to be 98 ℃ for discharging.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (5)
1. A process for the preparation of tetrachloroethylene, said process comprising the steps of:
(1) Firstly, carrying out chlorination reaction on raw materials for preparing tetrachloroethylene to obtain a high-temperature chlorination reaction product;
(2) Exchanging heat between the high-temperature chlorination reaction product and the molten salt to obtain a chlorination reaction product with a reduced temperature and the molten salt with an increased temperature;
(3) Carrying out quenching treatment on the chlorination reaction product with the reduced temperature, and using the molten salt with the increased temperature as a heat source to be used at a hot end;
in the step (1), raw materials for preparing tetrachloroethylene comprise chlorine, carbon tetrachloride and other chlorohydrocarbons; wherein the other chlorinated hydrocarbon is selected from one or more of methyl chloride, methylene dichloride, trichloromethane, dichloroethane, trichloroethane, pentachloroethane, hexachloroethane, dichloropropane and hexachlorobutadiene;
in the step (1), the high-temperature chlorination reaction product contains tetrachloroethylene, unconverted other chlorohydrocarbons, carbon tetrachloride and chlorine, and byproducts of hydrogen chloride and polychloride;
in the step (2), the molten salt is a molten mass of alkali metal, alkaline earth metal halide, nitrate, nitrite and sulfate; the temperature of the molten salt before heat exchange is 250-350 ℃; the temperature of the fused salt after heat exchange is 300-450 ℃;
the temperature of the high-temperature chlorination reaction product before heat exchange is 400-700 ℃, and the temperature of the chlorination reaction product after heat exchange is 300-500 ℃;
the method is implemented by adopting the following device, wherein the device comprises a chlorination reactor, a heat exchanger, a quenching tower and a condenser; the chlorination reactor is connected with a heat exchanger, the heat exchanger is connected with the lower part of a quenching tower, and a condenser is arranged at the top of the quenching tower;
the bottom of the quenching tower is provided with a first pipeline for discharging heavy components in the quenching tower, wherein the heavy components contain polychloride and carbon tetrachloride;
a second pipeline is arranged on the side line of the quenching tower and used for discharging liquid components, the second pipeline is connected with a tetrachloroethylene recovery device, the liquid phase components contain tetrachloroethylene and carbon tetrachloride, and the tetrachloroethylene recovery device is used for further separating and recovering tetrachloroethylene and then returning the carbon tetrachloride to the chlorination reactor;
the top of the quenching tower is provided with a third pipeline for discharging gas-phase components, the third pipeline is connected with a condenser, the gas-phase components are condensed by the condenser, and the obtained condensate containing carbon tetrachloride and tetrachloroethylene returns to the quenching tower; the non-condensable gas contains hydrogen chloride, chlorine and carbon tetrachloride, and after the hydrogen chloride is further separated and recovered, the chlorine and the carbon tetrachloride return to the chlorination reactor.
2. The method of claim 1, wherein in the step (1), the chlorination reaction temperature is 400-700 ℃; the reaction pressure is 0.1-0.2MPa.
3. The process of claim 1 or 2, wherein in step (1), the byproduct polychloride is at least one of hexachloropropane, hexachlorobutadiene, hexachlorobenzene.
4. The method according to claim 1, wherein in the step (2), the molten salt is a binary molten salt consisting of 55wt% potassium nitrate and 45wt% sodium nitrite.
5. The method according to claim 1, wherein in the step (3), after the quenching treatment, a gas phase component and a liquid phase component are obtained; the gas phase component contains hydrogen chloride, chlorine, carbon tetrachloride and tetrachloroethylene; the liquid phase component contains tetrachloroethylene and carbon tetrachloride.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103588615A (en) * | 2013-11-01 | 2014-02-19 | 聊城市鲁西化工工程设计有限责任公司 | Device and technology for recovery of tetrachloroethylene |
| CN204779413U (en) * | 2015-07-07 | 2015-11-18 | 重庆海洲化学品有限公司 | Production perchlorethylene's reaction gas processing system |
| CN207745852U (en) * | 2017-09-30 | 2018-08-21 | 刘世刚 | A kind of methane chloride reaction heat treatment system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588615A (en) * | 2013-11-01 | 2014-02-19 | 聊城市鲁西化工工程设计有限责任公司 | Device and technology for recovery of tetrachloroethylene |
| CN204779413U (en) * | 2015-07-07 | 2015-11-18 | 重庆海洲化学品有限公司 | Production perchlorethylene's reaction gas processing system |
| CN207745852U (en) * | 2017-09-30 | 2018-08-21 | 刘世刚 | A kind of methane chloride reaction heat treatment system |
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