CN212425916U - Ultra-high-purity methane chloride production system - Google Patents

Ultra-high-purity methane chloride production system Download PDF

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CN212425916U
CN212425916U CN202020684710.1U CN202020684710U CN212425916U CN 212425916 U CN212425916 U CN 212425916U CN 202020684710 U CN202020684710 U CN 202020684710U CN 212425916 U CN212425916 U CN 212425916U
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methane chloride
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methanol
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高永宝
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Abstract

The utility model discloses an ultra-pure methane chloride production system, which comprises a methane chloride reaction system and a carbon tetrachloride conversion reaction system which are produced by a methanol gas phase hydrochlorination dry method, wherein the two systems are connected with a sulfuric acid drying system and a methane chloride rectification system in sequence to obtain a methane chloride finished product; the sulfuric acid drying system is also connected with a compressor, and a gas outlet of the compressor and a gas outlet at the top of the methane chloride rectification system are connected and mixed to form a reaction system for producing methane chloride by a methane chloride-methane gas phase thermal chlorination method from crude methane chloride; the reaction system for producing methane chloride by using the methane chloride gas-phase thermal chlorination method sequentially enables the obtained mixed gas after the reaction of methane chloride and chlorine to enter a steam generation system, a chiller III, a condensation separation system, a light component removal system, a dichloromethane refining system, a trichloromethane refining system and a carbon tetrachloride refining system. The system realizes the coupling energy conservation of the whole process, the free adjustment of the proportion of the whole series of products and the compound water removal of the whole system, and changes the condition of single proportion of the products.

Description

Ultra-high-purity methane chloride production system
Technical Field
The utility model relates to an ultra-high purity methane chloride production system and process method technical field especially relate to an ultra-high purity methane chloride production system.
Background
The single set of methane chloride has small production capacity, high consumption, more byproducts, basically 1:1 ratio of the dichloromethane to the trichloromethane, small adjustment range and common purity. The crude methane chloride has high moisture content and serious corrosion to the device. The two-step reaction heat, the material heat and the material cold are not comprehensively utilized. The byproduct carbon tetrachloride is mainly used for matching production of tetrachloroethylene, and has the advantages of long production flow, large investment and more three wastes.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects of the prior art, the utility model provides a full-flow coupling energy-saving device, which makes full use of two-step reaction heat, material heat and material cold, reduces energy consumption, effectively saves energy and reduces emission; the dry method is used for treating the crude methane chloride, so that the water content of the crude methane chloride is effectively reduced, and the generation amount of three wastes is reduced. The single-set capacity of producing methane chloride by the dry-method hydrochlorination of methanol is improved by 3 times. The single-set capacity of methane chloride production by a methane chloride gas phase thermal chlorination method is improved by 1 time. The single condition of the product proportion is changed, the proportion of dichloromethane and trichloromethane can be infinitely adjusted, dichloromethane and trichloromethane can not be produced, carbon tetrachloride can be used as a commodity and can also be converted into methane chloride, the height is high, and the requirements in various aspects are met; the purity of dichloromethane, trichloromethane and carbon tetrachloride can reach ultra-high purity level, and common pure and high-grade pure products can also be produced; the whole system material is subjected to composite dewatering and drying, so that the corrosion of the device is avoided, and the service life of the device is prolonged. The process can meet the requirements of high quality, low consumption, long period, high load, multifunction, green environmental protection and integration modern engineering on the ultra-high purity methane chloride production system and the process.
The utility model adopts the technical proposal that: an ultra-high purity methane chloride production system comprising:
a reaction system for producing methane chloride by a methanol gas phase hydrochlorination dry method, wherein the gas phase methanol reacts with hydrogen chloride to generate methane chloride, and the reaction system is sequentially connected with a sulfuric acid drying system and a methane chloride rectification system;
a carbon tetrachloride conversion reaction system, wherein gas-phase methanol, hydrogen chloride and gas-phase carbon tetrachloride are reacted to generate methane chloride, and the methane chloride is sequentially connected with a sulfuric acid drying system and a methane chloride rectification system to obtain a methane chloride finished product;
the sulfuric acid drying system is also connected with a first compressor, a gas outlet of the first compressor is connected with a gas outlet at the top of the methane chloride rectification system, the two gas flows are mixed into crude methane chloride, and the crude methane chloride is connected to a methane chloride gas-phase thermal chlorination method production methane chloride reaction system for generating methane chloride;
a methane chloride production reaction system by a methane chloride gas-phase thermal chlorination method, wherein mixed gas obtained after reaction of methane chloride and chlorine sequentially enters a steam generation system, a chiller III, a condensation separation system, a light component removal system, a dichloromethane refining system, a trichloromethane refining system and a carbon tetrachloride refining system;
the dichloromethane refining system is used for obtaining a dichloromethane product and providing a raw material for the trichloromethane refining system;
the trichloromethane refining system is used for obtaining a trichloromethane product and providing a raw material for the carbon tetrachloride refining system;
the carbon tetrachloride refining system obtains a carbon tetrachloride product, and the carbon tetrachloride product is supplied to the carbon tetrachloride conversion reaction system for recycling;
wherein: the hydrogen chloride separated by the condensation separation system is supplied to a methane chloride reaction system and a carbon tetrachloride conversion reaction system for producing methane chloride by a methanol gas phase hydrochlorination dry method through a cryogenic separation system.
The sulfuric acid drying system comprises a sulfuric acid drying tower I, a sulfuric acid drying tower II, a sulfuric acid drying tower III and a sulfuric acid demister which are connected in sequence.
Further, a reaction system for producing methane chloride by a methanol gas phase hydrochlorination dry method comprises a hydrochlorination reactor and a methanol recovery tower I, wherein the hydrochlorination reactor is mixed with three gas flows to carry out a gas phase fixed bed catalytic hydrochlorination reaction to generate methane chloride, and the three gas flows are respectively as follows:
the first air flow: the methanol is sequentially superheated by a methanol preheater I, a methanol vaporizer I, a methanol heater I and a methanol superheater I to obtain superheated methanol;
and (2) airflow II: hydrogen chloride separated from a methane chloride production reaction system by a methane chloride gas phase thermal chlorination method is superheated by a hydrogen chloride superheater to obtain superheated hydrogen chloride;
airflow III: the mixed gas after the reaction of the hydrochlorination reactor sequentially passes through a first chilling tower, a first chilling tank, a first methanol recovery tower and a first methanol recovery vaporizer, and the vaporized methanol obtained after vaporization is recovered;
the first chilling tower is sequentially connected with a first chilling tank, a first acid condenser, a first separator, a first demister, a sulfuric acid drying system and a first compressor;
the first compressor is connected with the top of the methane chloride rectification system, gas separated from the top of the methane chloride rectification system is mixed into crude methane chloride, so that light component raw materials are provided for a methane chloride production reaction system by a methane chloride gas-phase thermal chlorination method, and meanwhile, the first compressor is directly connected with the methane chloride rectification system to obtain a methane chloride finished product.
Further, the carbon tetrachloride conversion reaction system comprises a carbon tetrachloride conversion reactor and a methanol recovery tower II, and the carbon tetrachloride conversion reactor mixes four gas flows and then carries out gas phase fixed bed catalytic hydrochlorination reaction to generate methane chloride, wherein the four gas flows are respectively as follows:
the first air flow: the methanol is sequentially superheated by a methanol preheater II, a methanol vaporizer II, a methanol heater II and a methanol superheater II to obtain superheated methanol;
and (2) airflow II: hydrogen chloride separated by a methane chloride production reaction system by a methane chloride gas phase thermal chlorination method is superheated hydrogen chloride provided after being superheated by a hydrogen chloride superheater II;
airflow III: the mixed gas after the reaction of the carbon tetrachloride conversion reactor is vaporized by a second chilling tower, a second chilling tank, a second methanol recovery tower and a second methanol recovery vaporizer in sequence to obtain vaporized recovered methanol;
and (4) airflow: the carbon tetrachloride is vaporized by a carbon tetrachloride vaporizer and enters a carbon tetrachloride superheater to obtain superheated carbon tetrachloride;
the second chilling tower is sequentially connected with a second chilling tank, a second acid condenser, a second separator, a second demister, a sulfuric acid drying system and a first compressor;
the first compressor is connected with the top of the methane chloride rectification system, gas separated from the top of the methane chloride rectification system is mixed into crude methane chloride, so that light component raw materials are provided for a methane chloride production reaction system by a methane chloride gas-phase thermal chlorination method, and meanwhile, the first compressor is directly connected with the methane chloride rectification system to obtain a methane chloride finished product.
Further, methane chloride production reaction system of methane chloride vapour phase hot chlorination process is including the gas mixture heater, two injection jet mixers, methane chloride hot chlorination reactor, reaction heat transfer ware and the quench tower third that connect gradually, and the quench tower third connects gradually one-level condenser, one-level separator, gas entering heat exchanger, second grade separator, tertiary condenser, tertiary separator and separates and the heat exchange, wherein:
the first-stage separator is used for inputting the separated gas into a heat exchanger to exchange heat with cold materials and then inputting the gas into a second-stage separator, and the separated liquid enters a primary material storage tank;
the primary material storage tank is sequentially connected with a tower bottom heat exchanger of the light component removal tower and a tower bottom cooler of the light component removal tower, so that methane chloride from the primary material storage tank is subjected to light component removal and cooling and then is conveyed to an ultra-high purity methane chloride product separation system;
the third-stage separator is connected with a heat exchanger feed chute, so that the heat exchanger feed chute is used for providing cold materials for the heat exchanger, and the gas separated by the third-stage separator is used for providing hydrogen chloride gas as a raw material for a methane chloride gas production system by a methanol gas phase hydrochlorination dry method;
the reaction heat transfer device is connected with the steam generation system and the hot water tank to obtain steam.
Furthermore, the top of the light component removal tower is connected with a tower top condenser and a light component groove, and light components are provided for a methane chloride production reaction system by a methane chloride gas phase thermal chlorination method.
Further, the dichloromethane refining system comprises a dichloromethane refining tower, a dichloromethane reflux tank, a dichloromethane alkaline washing tank and a dichloromethane azeotropic tower which are connected in sequence; the trichloromethane refining system comprises a trichloromethane refining tower, a trichloromethane reflux tank, a trichloromethane alkaline washing tank and a trichloromethane azeotropic tower which are connected in sequence; a carbon tetrachloride refining tower, a carbon tetrachloride reflux tank, a carbon tetrachloride alkaline washing tank and a carbon tetrachloride azeotropic tower which are sequentially connected with the carbon tetrachloride refining system.
Furthermore, the bottom of the dichloromethane refining tower is connected with a dichloromethane kettle bottom heat exchanger, the bottom of the trichloromethane refining tower is connected with a trichloromethane kettle bottom heat exchanger, and the dichloromethane kettle bottom heat exchanger is connected with the trichloromethane kettle bottom heat exchanger.
Furthermore, the condensation separation system is connected with a methane chloride production reaction system by a methane chloride gas-phase thermal chlorination method through a cryogenic separation system, and the obtained hydrogen chloride and methanol are supplied to a methane chloride production reaction system by a methanol gas-phase hydrochlorination dry method and a carbon tetrachloride conversion reaction system for recycling.
The process method of the ultra-high purity methane chloride production system at least comprises the following steps:
a. the method comprises the steps of feeding methyl chloride produced by a methyl chloride reaction system produced by a methanol gas phase hydrochlorination dry method and methyl chloride produced by a carbon tetrachloride conversion reaction system into a sulfuric acid drying system for drying treatment, feeding one part of the methyl chloride into a methyl chloride rectification system for treatment to obtain a methyl chloride finished product, compressing the other part of the methyl chloride by a compressor, mixing the compressed part of the methyl chloride with the methyl chloride separated by the methyl chloride rectification system to obtain crude methyl chloride, and feeding the crude methyl chloride into a methyl chloride gas phase thermal chlorination method to produce a methane chloride reaction system for generating methane chloride;
b. the mixed gas obtained by the reaction system for producing methane chloride by using the methane chloride gas-phase thermal chlorination method and reacting methane chloride with chlorine sequentially enters a steam generation system, a third chiller, a condensation separation system, a light component removal system, a dichloromethane refining system, a trichloromethane refining system and a carbon tetrachloride refining system, wherein the dichloromethane refining system obtains a dichloromethane product, the trichloromethane refining system obtains a trichloromethane product, and the carbon tetrachloride product separated by the carbon tetrachloride refining system is supplied to a carbon tetrachloride conversion reaction system for recycling;
wherein: the hydrogen chloride separated by the condensation separation system is supplied to a methane chloride reaction system and a carbon tetrachloride conversion reaction system for producing methane chloride by a methanol gas phase hydrochlorination dry method through a cryogenic separation system.
Compared with the prior art, the beneficial effects of the utility model are that: 1. coupling energy conservation and ultra-low energy consumption. Steam condensate water collected in the methane chloride production is used for preheating methanol; the heat released by the reaction of methanol and hydrogen chloride is totally used for vaporizing the methanol and heating the reaction raw materials; the produced methane chloride gas is pressurized by a compressor and then directly sent to a methane chloride thermal chlorination device without condensation liquefaction and then vaporization; the byproduct steam of the heat chlorination reaction of methane chloride is used in the process; the cold energy of the condensate of the three-stage condenser is utilized; the tower kettle discharge of the light component separation tower exchanges heat with the tower feed; the tower bottom discharge of the dichloromethane rectification tower exchanges heat with the tower feed, the tower bottom discharge of the trichloromethane rectification tower exchanges heat with the tower feed, and the reaction heat of methane chloride produced by the conversion of carbon tetrachloride is fully utilized to heat the raw material; the steam condensate water of the device is completely collected and is preheated as a raw material, and then is sent to an ion-free device to be used as the raw material.
The method has the advantages that no water washing and alkali washing are carried out, three wastes are less, the three-stage sulfuric acid series drying is directly carried out after cooling, and the water content of the methane chloride is ultra-low.
The dry methane chloride gas (containing a small amount of hydrogen chloride) is pressurized by a compressor, and then the dry methane chloride gas is directly sent to a methane chloride thermal chlorination reaction device instead of being cooled, liquefied, stored and then vaporized to be sent to the methane chloride thermal chlorination reaction device, so that the process is short, and the energy-saving effect is good. And the redundant crude chloromethane is separated from hydrogen chloride by a dry method to obtain the product chloromethane.
3. The purity of products such as dichloromethane, trichloromethane and carbon tetrachloride of the system reaches ultra-high purity level, common level and high-purity level products can also be produced, the product proportion of dichloromethane and trichloromethane can be infinitely adjusted, and the product proportion can be as follows: 0-20% of methane chloride, 100-0% of dichloromethane, 0-100% of trichloromethane and 0-30% of carbon tetrachloride.
4. The methane chloride thermal chlorination reaction system adopts a high-power double-injection jet mixing technology to fully mix the raw material gas and the chlorine; the high-power explosion-proof electric heating technology is adopted, so that the temperature of the thermal chlorination reactor can be raised, and the temperature of the reactor can be stabilized; the reaction capacity is doubled, the production capacity of a single set of chloromethane thermal chlorination reactor provided with a high-power explosion-proof electric heater and a high-power double-injection jet mixer can reach 12 ten thousand tons per year, and the capacity can be doubled.
5. The intermediate liquid materials of the methane chloride heat chlorination device and the product separation device are circularly dried by adopting a drying agent, so that the moisture of the materials is ensured to reach the standard, and the devices are prevented from being corroded.
To sum up, the system and the process of the utility model have the advantages that the whole process is coupled and energy-saving, the two-step reaction heat, the material heat and the material cold are fully utilized, the energy consumption is greatly reduced, and the energy is effectively saved and the emission is reduced; the dry method is used for treating the crude methane chloride, so that the water content of the crude methane chloride is effectively reduced, and the generation amount of three wastes is reduced. The single-set capacity of producing methane chloride by the dry-method hydrochlorination of methanol is improved by 3 times. The single-set capacity of methane chloride production by a methane chloride gas phase thermal chlorination method is improved by 1 time. The single condition of the product proportion is changed, the proportion of dichloromethane and trichloromethane can be infinitely adjusted, dichloromethane and trichloromethane can not be produced, carbon tetrachloride can be used as a commodity and can also be converted into methane chloride, the height is high, and the requirements in various aspects are met; the purity of dichloromethane, trichloromethane and carbon tetrachloride can reach ultra-high purity level, and common pure and high-grade pure products can also be produced; the whole system material is subjected to composite dewatering and drying, so that the corrosion of the device is avoided, and the service life of the device is prolonged. The process can meet the modern engineering requirements of high quality, low consumption, long period, high load, multifunction, environmental protection and integration.
Drawings
FIG. 1 is a block diagram of an ultra-high purity methane chloride production system;
FIG. 2 is a schematic diagram of a reaction system 100 for producing methyl chloride by a methanol gas phase hydrochlorination dry method;
fig. 3 is a block diagram of a carbon tetrachloride conversion reaction system 200;
FIG. 4 is a block diagram of a reaction system 300 for producing methane chloride by a methane chloride gas phase thermal chlorination process;
FIG. 5 is a separation block diagram of a dichloromethane refining system 15, a trichloromethane refining system 16 and a carbon tetrachloride refining system 17, i.e., an ultra-high purity methane chloride separation process flow diagram;
wherein: the reaction system comprises a 100-methanol gas-phase hydrochlorination dry-method production methane chloride reaction system, a 101-methanol preheater I, a 102-methanol vaporizer I, a 103-methanol heater I, a 104-methanol superheater I, a 105-hydrogen chloride superheater I, a 106-hydrochlorination reactor, a 107-chilling tower I, a 108-chilling tank I, a 109-acid condenser I, a 110-separator I, a 111-demister I, a 112-methanol recovery tower I and a 113-recovery methanol vaporizer I;
a 200-carbon tetrachloride conversion reaction system, a 201-methanol preheater II, a 202-methanol vaporizer II, a 203-methanol heater II, a 204-methanol superheater II, a 205-hydrogen chloride superheater II, a 206-carbon tetrachloride vaporizer, a 207-carbon tetrachloride superheater, a 208-carbon tetrachloride conversion reactor, a 209-chilling tower II, a 210-chilling tank II, a 211-acid condenser II, a 212-separator II, a 213-demister II, a 214-methanol recovery tower II, and a 215-methanol recovery vaporizer II;
300-methane chloride gas phase thermal chlorination process methane chloride production reaction system, 301-mixed gas heater, 302-double injection jet mixer, 303-methane chloride thermal chlorination reactor, 304-reaction heat transfer device, 305-chilling tower III, 307-hot water tank, 308-first-stage condenser, 309-first-stage separator, 310-initial material storage tank, 311-heat exchanger, 312-second-stage separator, 313-third-stage condenser, 314-third-stage separator, 315-heat exchanger feed tank, 316-lightness-removing tower, 317-tower bottom heat exchanger, 318-lightness-removing tower bottom cooler, 319-tower top condenser and 320-lightness-component tank;
4-sulfuric acid drying system, 401-sulfuric acid drying tower I, 402-sulfuric acid drying tower II, 403-sulfuric acid drying tower III, 404-sulfuric acid demister; 6-a methyl chloride finished product, 7-a cryogenic separation system, 8-a compressor I, 9-a methyl chloride rectification system and 91-a methyl chloride storage tank; 10-trichloromethane product, 11-steam generation system, 12-chiller III, 13-condensation separation system, 14-lightness removing system,
15-dichloromethane refining system, 151-dichloromethane refining tower, 152-dichloromethane reflux tank, 153-dichloromethane alkaline tank, 154-dichloromethane azeotropic tower and 155-dichloromethane kettle bottom heat exchanger;
the system comprises a 16-trichloromethane refining system, a 161-trichloromethane refining tower, a 162-trichloromethane reflux tank, a 163-trichloromethane alkaline washing tank, a 164-trichloromethane azeotropic tower and a 165-trichloromethane kettle bottom heat exchanger;
a 17-carbon tetrachloride refining system, a 171-carbon tetrachloride refining tower, a 172-carbon tetrachloride reflux tank, a 173-carbon tetrachloride alkaline washing tank and a 174-carbon tetrachloride azeotropic tower; 18-carbon tetrachloride product, 19-methylene chloride product.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present invention, and should not be construed as limiting the present invention.
As shown in fig. 1, an ultra-high purity methane chloride production system comprises:
a reaction system 100 for producing methane chloride by a methanol gas phase hydrochlorination dry method, wherein the gas phase methanol reacts with hydrogen chloride to generate methane chloride, and the reaction system is sequentially connected with a sulfuric acid drying system 4 and a methane chloride rectification system 9;
the carbon tetrachloride conversion reaction system 200 is used for generating methane chloride from gas-phase methanol, hydrogen chloride and gas-phase carbon tetrachloride, and is sequentially connected with the sulfuric acid drying system 4 and the methane chloride rectification system 9 to obtain a methane chloride finished product 6;
the sulfuric acid drying system 4 is also connected with a first compressor 8, the gas outlet of the first compressor 8 is connected with the gas outlet at the top of the methane chloride rectification system 9, two gas flows are mixed into crude methane chloride, and the crude methane chloride is connected to a methane chloride gas-phase thermal chlorination method production methane chloride reaction system 300 for generating methane chloride;
the methane chloride production reaction system 300 by using a methane chloride gas-phase thermal chlorination method comprises the steps of enabling obtained mixed gas obtained after reaction of methane chloride and chlorine to sequentially enter a steam generation system 11, a chiller III 12, a condensation separation system 13, a light component removal system 14, a dichloromethane refining system 15, a trichloromethane refining system 16 and a carbon tetrachloride refining system 17;
a dichloromethane refining system 15 for obtaining a dichloromethane product 19 and providing a raw material for a chloroform refining system 16;
a trichloromethane refining system 16 for obtaining a trichloromethane product 10 and providing a raw material for a carbon tetrachloride refining system 17;
a carbon tetrachloride refining system 17 for obtaining a carbon tetrachloride product 18, and the carbon tetrachloride product 18 is supplied to the carbon tetrachloride conversion reaction system 200 for recycling;
wherein: the hydrogen chloride separated by the condensation separation system 13 is supplied to a methyl chloride reaction system 100 and a carbon tetrachloride conversion reaction system 200 for use through a cryogenic separation system 7.
More preferably, the sulfuric acid drying system 4 includes a sulfuric acid drying tower I401, a sulfuric acid drying tower II402, a sulfuric acid drying tower III403, and a sulfuric acid demister 404, which are connected in sequence.
As shown in fig. 2, the reaction system 100 for producing methane chloride by a methanol gas phase hydrochlorination dry method of the present invention includes a hydrochlorination reactor 106 and a methanol recovery tower 112, wherein the hydrochlorination reactor 106 mixes three streams of gas streams to perform a gas phase fixed bed catalytic hydrochlorination reaction to generate methane chloride, and the three streams of gas streams are respectively:
the first air flow: the methanol is superheated by a methanol preheater I101, a methanol vaporizer I102, a methanol heater I103 and a methanol superheater I104 which are connected in sequence to obtain superheated methanol;
and (2) airflow II: hydrogen chloride separated by a methane chloride production reaction system 300 by a methane chloride gas-phase thermal chlorination method is superheated by a hydrogen chloride superheater I105 to obtain superheated hydrogen chloride;
airflow III: the mixed gas after the reaction of the hydrochlorination reactor 106 passes through a first chilling tower 107, a first chilling groove 108, a first methanol recovery tower 112 and a first recovered methanol vaporizer 113 which are connected in sequence, and the methanol is recovered through vaporization obtained after vaporization;
the first chilling tower 107 is also sequentially connected with a first chilling tank 108, a first acid condenser 109, a first separator 110, a first demister 111, a sulfuric acid drying system 4 and a first compressor 8;
the first compressor 8 is connected with the top of the methane chloride rectification system 9, and gas separated from the top of the methane chloride rectification system 9 is mixed into crude methane chloride, so that raw materials are provided for a reaction system 10 for producing methane chloride by a methane chloride gas-phase thermal chlorination method, and meanwhile, the first compressor 8 is also directly connected with the methane chloride rectification system 9 to obtain a methane chloride finished product;
the connection is that the reaction mixed gas from the hydrochlorination reactor 106 firstly enters a quench tower I107 to be quenched, then is condensed by an acid condenser I109 and is separated by a separator I110 to obtain hydrochloric acid condensate, and the separated hydrochloric acid condensate is used as a quench liquid to quench the reaction mixed gas in the quench tower I107;
hydrochloric acid from the first chilling tank 108 enters a methanol recovery tower 112, mixed gas from the first chilling tank 108 is cooled and separated, condensate liquid is discharged from the first chilling tank 107, uncondensed gas enters a sulfuric acid drying system 4 for drying after passing through a demister 111, and then enters a compressor 8, the gas compressed by the compressor 8 is mixed with part of the compressed gas and gas separated from the top of a methane chloride rectification system 9 to form crude methane chloride, so that raw materials are provided for a methane chloride production reaction system 300 by a methane chloride gas-phase thermal chlorination method, and the other part of the compressed gas passes through the methane chloride rectification system 9 to obtain a methane chloride finished product.
The first methanol preheater 101 is configured to preheat methanol using heat of the steam condensate collected by the device. The first methanol vaporizer 102 is configured to vaporize methanol using a heating medium of the hydrochlorination reactor. The first methanol heater 103 is arranged to further heat the vaporized methanol with steam. The first methanol superheater 104 is configured to heat the methanol gas to the feed temperature required by the hydrochlorination reactor using the heating medium of the hydrochlorination reactor. The hydrogen chloride superheater one 105 is arranged to heat the hydrogen chloride gas to the feed temperature required by the hydrochlorination reactor by using the heating medium of the hydrochlorination reactor. The hydrochlorination reactor 106 is configured to produce methyl chloride by a gas phase fixed bed catalytic reaction of superheated hydrogen chloride and methanol at a temperature and pressure. The quench tower one 107 is configured to quench the reaction mixture with liquid acid. The quench tank one 108 is configured to separate acid from the gas. The first acid condenser 109 is arranged to cool the gas exiting the quench tank. The first separator 110 is configured to separate gas and liquid from the material sent from the first acid condenser 109. The first demister 111 is arranged to intercept mist in the gas sent by the first separator 110. The sulfuric acid drying tower I401 is configured to dry the reaction gas for the first time. The sulfuric acid drying tower II402 is configured to dry the reaction gas for a second time. The sulfuric acid drying tower III403 is configured to perform third drying on the reaction gas. The sulfuric acid demister 404 is configured to intercept entrainment in the gas. The first compressor 8 is configured to boost the pressure of the crude methane chloride gas. The methane chloride rectification system 9 is arranged to refine the crude methane chloride to obtain qualified finished product methane chloride from the tower bottom. The methane chloride storage tank 91 is configured to store qualified methane chloride liquid. The methanol recovery column 112 is provided to purify the hydrochloric acid sent from the quench tank 108 and recover methanol therein. The recovered methanol vaporizer 113 is configured to vaporize recovered methanol liquid into the hydrochlorination reactor 106. And cooling the qualified hydrochloric acid discharged from the first 112 tower kettle of the methanol recovery tower to obtain the product.
As shown in fig. 3, the carbon tetrachloride conversion reaction system 200 includes a carbon tetrachloride conversion reactor 208 and a second methanol recovery tower 214, and the carbon tetrachloride conversion reactor 208 mixes four gas flows and then performs a gas phase fixed bed catalytic hydrochlorination reaction to generate methyl chloride, where the four gas flows are:
the first air flow: the methanol is superheated by a second methanol preheater 201, a second methanol vaporizer 202, a second methanol heater 203 and a second methanol superheater 204 which are connected in sequence to obtain superheated methanol;
and (2) airflow II: the hydrogen chloride separated out by the methane chloride production reaction system 300 by the methane chloride gas phase thermal chlorination method is superheated by the hydrogen chloride superheater II 205 to provide superheated hydrogen chloride;
airflow III: the mixed gas after the reaction of the carbon tetrachloride conversion reactor 208 is vaporized by a second chilling tower 209, a second chilling tank 210, a second methanol recovery tower 214 and a second recovered methanol vaporizer 215 in sequence to obtain vaporized recovered methanol;
and (4) airflow: the carbon tetrachloride is vaporized by a carbon tetrachloride vaporizer 206 and enters a carbon tetrachloride superheater 207 to obtain superheated carbon tetrachloride;
the second chilling tower 209 is sequentially connected with a second chilling tank 210, a second acid condenser 211, a second separator 212, a second demister 213, a sulfuric acid drying system 4 and a first compressor 8;
the first compressor 8 is connected with the top of the methane chloride rectification system 9, and gas separated from the top of the methane chloride rectification system 9 is mixed into crude methane chloride, so that raw materials are provided for a reaction system 10 for producing methane chloride by a methane chloride gas-phase thermal chlorination method, and meanwhile, the first compressor 8 is also directly connected with the methane chloride rectification system 9 to obtain a methane chloride finished product;
the purpose of the connection is that the reaction mixed gas obtained by the carbon tetrachloride vaporizer 206 is firstly chilled in the second chilling tower 209, then is condensed by the second acid condenser 211 and is separated by the separator 212 to obtain hydrochloric acid condensate, and the separated hydrochloric acid condensate is used as a chilling liquid to chill the reaction mixed gas in the second chilling tower 209;
the hydrochloric acid from the second quenching tank 210 enters a second methanol recovery tower 214, the mixed gas from the second quenching tank 210 is cooled and separated, the condensate is discharged from the second quenching tower 209, the uncondensed gas passes through a demister 213 and then enters a sulfuric acid drying system 4 for drying, and then enters a first compressor 8, the gas compressed by the first compressor 8 is mixed with a part of compressed gas and the gas separated from the top of a methane chloride rectification system 9 to form crude methane chloride, so that raw materials are provided for a methane chloride production reaction system 300 by a methane chloride gas-phase thermal chlorination method, and the other part of compressed gas passes through a methane chloride rectification system 9 to prepare a methane chloride finished product.
The carbon tetrachloride vaporizer 206 is configured to vaporize liquid carbon tetrachloride using steam, the carbon tetrachloride superheater 207 is configured to further heat saturated carbon tetrachloride gas to a superheated state, and the methanol preheater two 201 is configured to preheat methanol using heat of steam condensate collected by the device. The second methanol vaporizer 202 is configured to vaporize methanol using the heating medium of the hydrochlorination reactor. The second methanol heater 203 is arranged to further heat the vaporized methanol with steam. The second methanol superheater 204 is configured to heat the methanol gas to the feed temperature required by the hydrochlorination reactor using the heating medium of the hydrochlorination reactor. The second hydrogen chloride superheater 205 is configured to heat the hydrogen chloride gas to a feed temperature required by the hydrochlorination reactor using a heating medium of the hydrochlorination reactor. The carbon tetrachloride conversion reactor 208 is configured to produce methyl chloride by a gas phase fixed bed catalytic reaction of hydrogen chloride and methanol at a temperature and pressure. Quench tower two 209 is configured to rapidly cool the reaction mixture with a liquid acid. The second quench tank 210 is configured to separate the acid solution from the gas. And the second acid condenser 211 is used for cooling the gas discharged from the chilling groove. The second separator 212 is configured to separate the gas and the liquid of the material sent by the second acid condenser 213. The second demister 213 is arranged to intercept the mist in the gas sent from the second separator 212. The second methanol recovery column 214 is provided to purify the hydrochloric acid sent from the second quench tank 210 and recover methanol therein. Recovered methanol vaporizer two 215 is configured to vaporize recovered methanol liquid into carbon tetrachloride conversion reactor 208. And cooling the qualified hydrochloric acid discharged from the tower bottom of the second 214 methanol recovery tower to obtain the product.
As shown in fig. 4, the reaction system 300 for producing methane chloride by a methane chloride gas-phase thermal chlorination method includes a mixed gas heater 301, a double-injection mixer 302, a methane chloride thermal chlorination reactor 303, a reaction heat transfer device 304 and a chilling tower third 305 which are connected in sequence, wherein the chilling tower third 305 is connected in sequence with a first-stage condenser 308, a first-stage separator 309, a gas inlet heat exchanger 311, a second-stage separator 312, a third-stage condenser 313 and a third-stage separator 314 for separation and heat exchange, wherein:
the first-stage separator 309, the separated gas is input into a heat exchanger 311 to exchange heat with cold materials and then enters a second-stage separator 312, and the separated liquid enters a primary material storage tank 310;
the primary material storage tank 310 is sequentially connected with a tower bottom heat exchanger 317 of a light component removal tower 316 and a tower bottom cooler 318 of the light component removal tower, so that the methane chloride from the primary material storage tank 310 is subjected to light component removal and cooling, and then is conveyed to an ultra-high purity methane chloride product separation system;
the third-stage separator 314 is connected with a heat exchanger feed chute 315, so that the heat exchanger feed chute provides cooling materials for the heat exchanger, and the gas separated by the third-stage separator provides hydrogen chloride gas as a raw material for a methane chloride gas production system by a methanol gas phase hydrochlorination dry method;
the reaction heat transfer device 304 connects the steam generation system 11 and the hot water tank 307 to obtain steam. More preferably, the top of the light component removing tower 316 is connected with a tower top condenser 319 and a light component tank 320, and the light component is provided for the methane chloride production reaction system 300 by the methane chloride gas phase thermal chlorination method.
The mixed gas heater 301 is configured to mix methane chloride and the light component gas and heat the mixture to a predetermined temperature. The high-power double-injection jet mixer 302 is set to be high in capacity by injecting and mixing methane chloride and light components by using chlorine gas at the first stage of injection, and high in capacity by injecting and mixing reaction gas by using raw material gas at the second stage of injection. The methane chloride thermal chlorination reactor 303 is configured to perform a thermal chlorination reaction of methane chloride, light components and chlorine gas at a certain temperature and under a certain pressure to generate methane chloride. The reaction heat transfer unit 304 is a heat transfer unit for exchanging heat between the high-temperature reaction mixture and the hot water, so that the reaction mixture can be rapidly cooled and the hot water can be rapidly heated. The steam generation system 11 is provided with a container for feeding hot water into the reaction heat transfer device 304, receiving high-temperature hot water sent by the reaction heat transfer device, flashing the hot water to form steam, and a water heating device. The hot water tank 307 is provided as a water supply tank for collecting and storing the system steam condensate for reuse. The third quench tower 305 is a reaction gas quench tower for further rapidly cooling the cooled reaction mixture gas to a temperature below a predetermined temperature by using liquid methane chloride. The primary condenser 308 is provided as a water-cooled condenser that partially condenses the methane chloride mixed gas into a liquid phase. The first-stage separator 309 is provided to separate the gas and liquid of the coolant supplied from the front. The primary feed sump 310 is configured to collect liquid feed from the primary separator 309 and the secondary separator 312. The heat exchanger 311 is arranged to further cool the noncondensable gas from the onward supply by the cold of the after-system material. The second separator 312 separates the coolant sent from the heat exchanger 311 into gas and liquid. The tertiary condenser 313 is provided to cryogenically cool the noncondensable gas supplied from the front side by a refrigerant. The third separator 314 is configured to separate the cryogenic feed from the third condenser 313 into a vapor and a liquid. Heat exchanger feed tank 315 is configured to collect liquid material separated by third stage separator 314. The light component removal column 316 is configured to separate the light component from the heavy component of the chloride mixed liquor. The lightness-removing column bottom heat exchanger 317 is arranged for exchanging heat between the bottom discharge of the lightness-removing column 316 and the feeding of the light-removing column. The light ends column bottoms cooler 318 is configured to further cool the crude methane chloride from the light ends column bottoms heat exchanger 317. The condenser 319 at the top of the lightness-removing column is arranged to partially condense the material coming out of the top of the lightness-removing column 316. The light component tank 320 is provided to separate the gas and liquid of the material sent from the condenser 319 at the top of the light component removal column and store the liquid as a reflux liquid.
Preferably, the condensation separation system 13 is further connected with a methane chloride production reaction system 300 through a cryogenic separation system 7, and the obtained hydrogen chloride and methanol are supplied to the methane chloride production reaction system 100 through methanol gas phase hydrochlorination and the carbon tetrachloride conversion reaction system 200 for recycling.
In a more preferred embodiment, the dichloromethane purification system 15 includes a dichloromethane purification tower 151, a dichloromethane reflux tank 152, a dichloromethane alkali washing tank 153, and a dichloromethane azeotropic tower 154, which are connected in this order; the chloroform refining system 16 comprises a chloroform refining tower 161, a chloroform reflux tank 162, a chloroform alkaline washing tank 163 and a chloroform azeotropic tower 164 which are connected in sequence; the carbon tetrachloride refining system 17 is connected in sequence to a carbon tetrachloride refining tower 171, a carbon tetrachloride reflux tank 172, a carbon tetrachloride alkaline washing tank 173, and a carbon tetrachloride azeotropic tower 174.
In a more preferred embodiment, the bottom of the dichloromethane refining tower 151 is connected to the dichloromethane kettle bottom heat exchanger 155, the bottom of the chloroform refining tower 161 is connected to the chloroform kettle bottom heat exchanger 165, and the dichloromethane kettle bottom heat exchanger 155 is connected to the chloroform kettle bottom heat exchanger 165, thereby realizing heat exchange.
The process method of the ultra-high purity methane chloride production system at least comprises the following steps:
a. the method comprises the steps of feeding methyl chloride produced by a methyl chloride production reaction system 100 by a methanol gas phase hydrochlorination dry method and methyl chloride produced by a carbon tetrachloride conversion reaction system 200 into a sulfuric acid drying system 4 for drying treatment, feeding one part of the methyl chloride into a methyl chloride rectification system 9 for treatment to obtain a methyl chloride finished product 6, compressing the other part of the methyl chloride by a compressor 16, mixing the compressed part of the methyl chloride with the methyl chloride separated by the methyl chloride rectification system 9 to obtain crude methyl chloride, and feeding the crude methyl chloride into a methyl chloride gas phase thermal chlorination methane chloride production reaction system 300 for generating methane chloride;
b. the mixed gas obtained by the reaction system 300 for producing methane chloride by using a methane chloride gas-phase thermal chlorination method and reacting methane chloride with chlorine sequentially enters a steam generation system 11, a chiller III 12, a condensation separation system 13, a light component removal system 14, a dichloromethane refining system 15, a trichloromethane refining system 16 and a carbon tetrachloride refining system 17, the dichloromethane refining system 15 obtains a dichloromethane product 19, the trichloromethane refining system 16 obtains a trichloromethane product 10, and the carbon tetrachloride product 18 separated by the carbon tetrachloride refining system 17 is supplied to a carbon tetrachloride conversion reaction system 200 for recycling;
wherein: the hydrogen chloride separated by the condensation separation system 13 is supplied to a methyl chloride reaction system 100 and a carbon tetrachloride conversion reaction system 200 for use through a cryogenic separation system 7.
The working process of the system of the utility model is that methane chloride is produced by a methane gas phase hydrochlorination dry method production methane chloride reaction system 100, a carbon tetrachloride conversion reaction system 200 production methane chloride, a methane chloride production reaction system 300 and ultra-pure methane chloride product separation and three wastes treatment and public works are matched.
The process for producing methane chloride by a methanol gas phase hydrochlorination dry method comprises the following steps: the method comprises the steps of preheating methanol by a methanol preheater, feeding the preheated methanol into a methanol vaporizer for vaporization, heating by a methanol heater, feeding the preheated methanol into a methanol superheater for superheating, then superheating by a hydrogen chloride superheater together with hydrogen chloride separated from methane chloride produced by methane chloride gas-phase thermal chlorination, mixing three materials obtained by vaporizing recovered methanol by a recovered methanol vaporizer, feeding the mixture into a hydrochlorination reactor for gas-phase fixed-bed catalytic hydrochlorination to generate methane chloride, wherein all reaction heat is used for heating raw materials, the reaction mixed gas is firstly fed into a quench tower for quenching, a hydrochloric acid condensate obtained by acid condenser condensation and acid separator separation is used as a quench liquid for quenching the reaction mixed gas, and hydrochloric acid discharged from a quench tank enters a methanol recovery system. And (3) cooling and separating the mixed gas from the first chilling tank, enabling the condensate to remove the chilling tower, enabling the uncondensed gas to sequentially enter a sulfuric acid drying tower I, a sulfuric acid drying tower II and a sulfuric acid drying tower III after passing through a demister, then entering a sulfuric acid demister I to obtain dry methane chloride, pressurizing by using a compressor, enabling a part of the gas to enter a methane chloride rectification system for separation to obtain a product methane chloride, and enabling a part of the product methane chloride to enter a methane chloride storage tank, and enabling a part of the crude methane chloride and the light component coming out of the top of the tower to enter the next process together to serve as raw materials. Hydrochloric acid from the quenching tank I enters a methanol recovery tower I, and recovered methanol is vaporized by a recovered methanol vaporizer I and then enters a hydrochlorination reactor.
The byproduct carbon tetrachloride of the methane chloride production device enters a carbon tetrachloride conversion production methane chloride system, the vaporized carbon tetrachloride, the vaporized methanol, the recovered methanol and the hydrogen chloride obtained by the previous separation are preheated, heated and mixed and then enter a gas-solid phase carbon tetrachloride conversion reactor to carry out gas-solid phase hydrochlorination, the reaction heat is completely used for heating the raw materials, the reaction mixed gas firstly enters a second chilling tower and a second chilling groove to chill, an acid condensate obtained by a rear system is used as a chilling liquid to chill the reaction mixed gas, and the hydrochloric acid discharged from the second chilling groove enters a methanol recovery system. And cooling and separating the mixed gas from the second quenching tank, de-exciting the second cooling tower by using the condensate, drying the non-condensed gas by using sulfuric acid, pressurizing by using a compressor, and then sending the non-condensed gas to a chloromethane thermal chlorination reaction system to serve as a raw material.
The mixed gas of the methane chloride, the chlorine and the light methane chloride is highly mixed by double injection and then enters a thermal chlorination reactor with an electric heating function to carry out gas-phase high-temperature thermal chlorination reaction to produce crude methane chloride mixed gas, then the mixed gas enters a system utilizing the heat byproduct steam of the thermal chlorination reaction for rapid cooling and byproduct steam, the crude methane chloride mixed gas enters a chilling tower for rapid cooling, then the mixed liquid enters a primary condenser and is cooled by cooling water, a part of condensate is used as chilling liquid and returns to a chilling tower for recycling, a part of condensate enters a light component separation system for separation to obtain crude methane chloride mixed liquid, and the mixed solution enters a methane chloride product separation system, crude products of dichloromethane and trichloromethane and byproducts of carbon tetrachloride are sequentially separated, and the crude products of dichloromethane and trichloromethane are respectively subjected to alkaline cleaning acid removal and azeotropic dehydration to obtain ultra-pure products of dichloromethane and trichloromethane.
And returning the light components from the top of the light component separation tower to the thermal chlorination reactor. The non-condensable gas from the first-stage condenser enters a heat exchanger and exchanges heat with low-temperature condensate obtained by low-temperature cooling of the third-stage condenser, the non-condensable gas from the tube pass of the heat exchanger enters the third-stage condenser, R22 is used as a refrigerant for deep cooling separation, the non-condensable gas mainly comprises hydrogen chloride, the hydrogen chloride enters a methanol dry-process hydrochlorination system to produce methyl chloride, chlorine elements are recycled, and the condensate from the tube pass of the heat exchanger is collected as crude methane chloride. The low-temperature gas coming out of the heat exchanger returns to the thermal chlorination reactor. And (3) allowing the redundant hydrogen chloride from the three-stage condenser to enter a hydrogen chloride absorption and treatment system, absorbing the hydrogen chloride by using hydrochloric acid or water produced by a methanol hydrochlorination system to obtain 31% hydrochloric acid, treating the hydrochloric acid to obtain qualified 31% hydrochloric acid, allowing unabsorbed tail gas to enter a tail gas treatment and recovery system, recovering a small amount of organic matters carried in the hydrogen chloride gas to return to the production system, and discharging the tail gas up to the standard.
Generally, the system and the method of the utility model adopt a new coupling energy-saving technology in the whole process, greatly save energy, reduce consumption and reduce emission, the proportion of products can be infinitely adjusted, the purity grade of the products reaches the ultra-high purity grade, and the single set of capacity reaches 12 ten thousand tons per year. And by adopting a comprehensive dewatering technology, the moisture in the material is greatly reduced, and the service life of the system is effectively prolonged. The requirements of low consumption, large capacity, high quality and long-period production are met.
The embodiment of the present invention discloses a preferred embodiment, but not limited thereto, and those skilled in the art can easily understand the spirit of the present invention according to the above embodiment, and make different extensions and changes, but do not depart from the spirit of the present invention, all of which are within the protection scope of the present invention.

Claims (9)

1. An ultra-high purity methane chloride production system, which is characterized in that: the method comprises the following steps:
a reaction system (100) for producing methane chloride by a methanol gas phase hydrochlorination dry method, wherein the gas phase methanol reacts with hydrogen chloride to generate methane chloride, and the reaction system is sequentially connected with a sulfuric acid drying system (4) and a methane chloride rectification system (9);
the carbon tetrachloride conversion reaction system (200) is used for reacting gas-phase methanol with hydrogen chloride and gas-phase carbon tetrachloride to generate methane chloride, and the methane chloride is sequentially connected with the sulfuric acid drying system (4) and the methane chloride rectifying system (9) to obtain a methane chloride finished product (6);
the sulfuric acid drying system (4) is also connected with a first compressor (8), the gas outlet of the first compressor (8) is connected with the gas outlet at the top of a methane chloride rectification system (9), two gas flows are mixed into crude methane chloride, and the crude methane chloride is connected to a methane chloride gas-phase thermal chlorination reaction system (300) for producing methane chloride;
a methane chloride reaction system (300) for producing methane chloride by a methane chloride gas-phase thermal chlorination method, wherein a methane chloride and chlorine gas mixed gas obtained after the reaction of methane chloride and chlorine gas sequentially enters a steam generation system (11), a chiller III (12), a condensation separation system (13), a light component removal system (14), a dichloromethane refining system (15), a trichloromethane refining system (16) and a carbon tetrachloride refining system (17);
a dichloromethane refining system (15) for obtaining a dichloromethane product (19) and providing a raw material for a chloroform refining system (16);
a trichloromethane refining system (16) for obtaining a trichloromethane product (10) and providing a raw material for a carbon tetrachloride refining system (17);
a carbon tetrachloride refining system (17) for obtaining a carbon tetrachloride product (18), wherein the carbon tetrachloride product (18) is supplied to the carbon tetrachloride conversion reaction system (200) for recycling;
wherein: the hydrogen chloride separated by the condensation separation system (13) is supplied to a methyl chloride gas phase hydrochlorination dry-method production reaction system (100) and a carbon tetrachloride conversion reaction system (200) for use through a cryogenic separation system (7).
2. An ultra-high purity methane chloride production system according to claim 1, wherein: the sulfuric acid drying system (4) comprises a sulfuric acid drying tower I (401), a sulfuric acid drying tower II (402), a sulfuric acid drying tower III (403) and a sulfuric acid demister (404) which are connected in sequence.
3. An ultra-high purity methane chloride production system according to claim 2, wherein: the reaction system (100) for producing the methane chloride by the methanol gas-phase hydrochlorination dry method comprises a hydrochlorination reactor (106) and a methanol recovery tower I (112), wherein the hydrochlorination reactor (106) is mixed with three gas flows to carry out gas-phase fixed-bed catalytic hydrochlorination to generate the methane chloride, and the three gas flows are respectively:
the first air flow: the methanol is superheated through a methanol preheater I (101), a methanol vaporizer I (102), a methanol heater I (103) and a methanol superheater I (104) which are connected in sequence to obtain superheated methanol;
and (2) airflow II: hydrogen chloride separated by a methane chloride production reaction system (300) by a methane chloride gas phase thermal chlorination method is superheated by a hydrogen chloride superheater I (105) to obtain superheated hydrogen chloride;
airflow III: the mixed gas after the reaction of the hydrochlorination reactor (106) passes through a first chilling tower (107), a first chilling groove (108), a first methanol recovery tower (112) and a first recovered methanol vaporizer (113) which are connected in sequence, and the vaporized recovered methanol is obtained after vaporization;
the first chilling tower (107) is also sequentially connected with a first chilling tank (108), a first acid condenser (109), a first separator (110), a first demister (111), a sulfuric acid drying system (4) and a first compressor (8);
the top of methane chloride rectifying system (9) is connected in compressor (8), and the gas mixture that the gas that the top of compressing out and methane chloride rectifying system (9) was separated is crude methane chloride, and then provides the raw materials for methane chloride gas-phase thermal chlorination method production methane chloride reaction system (300), and compressor (8) is still lug connection methane chloride rectifying system (9) simultaneously, and methane chloride rectifying system (9) are through connecting in its last methane chloride storage tank (91) and acquire the methyl chloride finished product.
4. An ultra-high purity methane chloride production system according to claim 2, wherein: the carbon tetrachloride conversion reaction system (200) comprises a carbon tetrachloride conversion reactor (208) and a methanol recovery tower II (214), four gas flows are mixed by the carbon tetrachloride conversion reactor (208) and then subjected to gas phase fixed bed catalytic hydrochlorination to generate methane chloride, and the four gas flows are respectively:
the first air flow: the methanol is sequentially superheated by a second methanol preheater (201), a second methanol vaporizer (202), a second methanol heater (203) and a second methanol superheater (204) to obtain superheated methanol;
and (2) airflow II: hydrogen chloride separated by a methane chloride production reaction system (300) by a methane chloride gas phase thermal chlorination method is superheated by a hydrogen chloride superheater II (205);
airflow III: the mixed gas after the reaction of the carbon tetrachloride conversion reactor (208) is vaporized and recovered with methanol after being vaporized by a second chilling tower (209), a second chilling groove (210), a second methanol recovery tower (214) and a second recovered methanol vaporizer (215) in sequence;
and (4) airflow: the carbon tetrachloride is vaporized by a carbon tetrachloride vaporizer (206) and enters a carbon tetrachloride superheater (207) to obtain superheated carbon tetrachloride;
the second chilling tower (209) is also sequentially connected with a second chilling tank (210), a second acid condenser (211), a second separator (212), a second demister (213), a sulfuric acid drying system (4) and a first compressor (8);
the first compressor (8) is connected with the top of the methane chloride rectification system (9), gas separated from the top of the methane chloride rectification system (9) is mixed to form crude methane chloride, raw materials are further provided for a methane chloride gas-phase thermal chlorination methane production reaction system (300), and meanwhile, the first compressor (8) is directly connected with the methane chloride rectification system (9) to obtain a methane chloride finished product.
5. An ultra-high purity methane chloride production system according to claim 3 or 4, wherein: methane chloride production reaction system (300) of methane chloride vapour phase hot chlorination method is including the gas mixture heater (301), two injection blender (302), methane chloride hot chlorination reactor (303), reaction heat transfer ware (304) and chilling tower three (305) that connect gradually, chilling tower three (305) connect gradually one-level condenser (308), one-level separator (309), gas gets into heat exchanger (311), second grade separator (312), tertiary condenser (313), tertiary separator (314) are separated and the heat exchange, wherein:
the first-stage separator (309), the separated gas is input into a heat exchanger (311) to exchange heat with the cold material and then enters a second-stage separator (312), and the separated liquid enters a primary material storage tank (310);
the primary material storage tank (310) is sequentially connected with a tower bottom heat exchanger (317) of a light component removal tower (316) and a tower bottom cooler (318) of the light component removal tower, so that methane chloride from the primary material storage tank (310) is subjected to light component removal and cooling and then is conveyed to an ultra-high purity methane chloride product separation system;
the third-stage separator (314) is connected with a heat exchanger feed tank (315), so that the heat exchanger feed tank (315) is used for providing cold materials for the heat exchanger (311), and gas separated by the third-stage separator (314) is used for providing hydrogen chloride gas as a raw material for a reaction system (100) for producing methane chloride by a methanol gas phase hydrochlorination dry method;
the reaction heat transfer device (304) is connected with the steam generation system (11) and the hot water tank (307) to obtain steam.
6. An ultra-high purity methane chloride production system according to claim 5, wherein: the top of the light component removal tower (316) is connected with a tower top condenser (319) and a light component groove (320) to provide light components for a methane chloride reaction system (300) produced by a methane chloride gas phase thermal chlorination method.
7. An ultra-high purity methane chloride production system according to claim 6, wherein: the dichloromethane refining system (15) comprises a dichloromethane refining tower (151), a dichloromethane reflux tank (152), a dichloromethane alkaline washing tank (153) and a dichloromethane azeotropic tower (154) which are connected in sequence; the trichloromethane refining system (16) comprises a trichloromethane refining tower (161), a trichloromethane reflux tank (162), a trichloromethane alkaline washing tank (163) and a trichloromethane azeotropic tower (164) which are connected in sequence; a carbon tetrachloride refining tower (171), a carbon tetrachloride reflux tank (172), a carbon tetrachloride alkaline washing tank (173) and a carbon tetrachloride azeotropic tower (174) which are connected with the carbon tetrachloride refining system (17) in sequence.
8. An ultra-high purity methane chloride production system according to claim 7, wherein: the bottom of the dichloromethane refining tower (151) is connected with a dichloromethane kettle bottom heat exchanger (155), the bottom of the trichloromethane refining tower (161) is connected with a trichloromethane kettle bottom heat exchanger (165), and the dichloromethane kettle bottom heat exchanger (155) is connected with the trichloromethane kettle bottom heat exchanger (165).
9. An ultra-high purity methane chloride production system according to claim 1, wherein: the condensation separation system (13) is also connected with a methane chloride production reaction system (300) by a methane chloride gas-phase thermal chlorination method through a cryogenic separation system (7), and the obtained hydrogen chloride and methanol are supplied to a methane chloride production reaction system (100) by a methanol gas-phase hydrochlorination dry method and a carbon tetrachloride conversion reaction system (200) for recycling.
CN202020684710.1U 2020-04-29 2020-04-29 Ultra-high-purity methane chloride production system Active CN212425916U (en)

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