CN101497551B - Methane chlorides production process utilizing chlorination reaction heat - Google Patents
Methane chlorides production process utilizing chlorination reaction heat Download PDFInfo
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- CN101497551B CN101497551B CN200910103331A CN200910103331A CN101497551B CN 101497551 B CN101497551 B CN 101497551B CN 200910103331 A CN200910103331 A CN 200910103331A CN 200910103331 A CN200910103331 A CN 200910103331A CN 101497551 B CN101497551 B CN 101497551B
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Abstract
The invention discloses a process for producing methane chloride by chlorination reaction heat. The process comprises a hydrochlorinate process and a chlorination process, wherein the chlorination process comprises the following steps that: after methane chloride gas prepared by the hydrochlorinate process and subchloride gas separated from mixture of a chlorination reaction are mixed and preheated, the methane chloride gas and the subchloride gas are mixed with chlorine and are introduced to a chlorination reactor to react; reaction mixture exchanges heat with raw material gas mixture of the methane chloride and the subchloride through a heat exchanger to preheat the raw material gas mixture, meanwhile, after the reaction mixture self is cooled, the reaction mixture enters a quenching tower to be cooled and washed, and enters a separating column to be separated; chlorine hydride gas and the subchloride gas are separated from gas vaporized from the top of the separating column through condensing separation, and are used as raw materials of the hydrochlorinate process and the chlorination process to be recycled; and methylene dichloride, methenyl trichloride and carbon tetrachloride are obtained from a mixed liquid obtained from the bottom of the separating column through rectifying separation. The process sufficiently and effectively reclaims mass high-grade heat energy carried by the mixture of high-temperature chlorination reaction, can greatly save energy, and reduce production cost.
Description
Technical field
The present invention relates to the organic cpds production technique, particularly utilize the methane chloride production process of chlorination reaction heat.
Background technology
Methane chloride is the general name of monochloro methane, methylene dichloride, trichloromethane and tetracol phenixin, is important chemical material and organic solvent, also is the main products of chlor-alkali enterprise balance chlorine.In recent years, along with the further expansion of fast development of national economy and methane chloride Application Areas, the production and consumption of domestic methane chloride obtains high speed development.
At present, producer mainly adopts the methyl alcohol method to produce methane chloride both at home and abroad.The methyl alcohol method was divided into for two steps: the first step is that methyl alcohol and hydrogenchloride generation hydrochlorination generate monochloro methane; Second step was monochloro methane and chlorine generation chlorination reaction, generated methylene dichloride, trichloromethane and tetracol phenixin simultaneously, and emitted a large amount of heat.Accordingly; Methyl alcohol method production technique comprises hydrochlorinate operation and chloride process: the hydrochlorinate operation is that methanol gas and hydrogen chloride gas are fed the reaction of hydrochlorination device; Reaction mixture obtains monochloro methane gas after cooling, absorption, drying, subsequent use after compressor compresses; Chloride process is monochloro methane gas, isolated subchloride gas and the reaction of chlorine feeding chlorination reactor from chlorination reaction mixture that the hydrochlorinate operation is made; Reaction mixture is after quenching tower cooling washing; Obtain thick chlorated liquid through recirculated water cooling condenser and refrigerant condenser condenses; The gas that is not condensed obtains subchloride liquid and tail gas hydrogenchloride through the cryogenic unit condensation again; Subchloride liquid returns refrigerant condensing surface raw material recycled as chloride process after the heat exchange gasification, and tail gas hydrogenchloride is as the raw material recycled of hydrochlorinate operation; Thick chlorated liquid gets into knockout tower to be separated, and also as the raw material recycled of chloride process, the mixed solution that the tower still obtains obtains methylene dichloride, trichloromethane and tetracol phenixin through rectifying separation to the subchloride gas that cat head steams.
There is following problem in above-mentioned production technique: the reaction mixture of discharging from chlorination reactor is a high-temperature gas, contains the higher-grade heat energy that can support recycling in a large number, but its fail to obtain fully, effectively recycling, cause the significant wastage of the energy.
Summary of the invention
In view of this, for overcoming the problem that exists in the existing methane chloride production process, the object of the present invention is to provide a kind of methane chloride production process that utilizes chlorination reaction heat.
For reaching this purpose; The methane chloride production process that utilizes chlorination reaction heat of the present invention comprises hydrochlorinate operation and chloride process, chloride process be monochloro methane gas that the hydrochlorinate operation is made and from chlorination reaction mixture isolated subchloride gas mix, after the preheating; Mix with chlorine; The reaction of feeding chlorination reactor, reaction mixture carries out heat exchange with the preheating material gas mixture through the material mixed gas of interchanger and monochloro methane and subchloride earlier, and the back that self lowered the temperature simultaneously gets into quenching tower cooling washing; Getting into knockout tower again separates; The gas that the knockout tower cat head steams obtains hydrogen chloride gas and subchloride liquid through condensation separation, and hydrogen chloride gas is as the raw material recycled of hydrochlorinate operation, the subchloride liquid raw material recycled of back as chloride process that gasified; The mixed solution that separation Tata still obtains obtains methylene dichloride, trichloromethane and tetracol phenixin through rectifying separation.
Further; Said hydrochlorinate operation is that methanol gas and hydrogen chloride gas are mixed the reaction of back feeding hydrochlorination device; Reaction mixture obtains monochloro methane gas after cooling, absorption, drying, utilize self pressure of hydrochlorination system that it is condensed into liquid with refrigerant again; Said chloride process be monochloro methane liquid that the hydrochlorinate operation is made and from chlorination reaction mixture the isolated subchloride liquid back of pumping up respectively mix, after gasification, preheating, mixes again with chlorine, the feeding chlorination reactor reacts;
Further; The gas that said knockout tower cat head steams is the first-stage condenser of refrigerant through the raw materials mix liquid with monochloro methane and subchloride; With recirculated water is the secondary condenser condensation of refrigerant, and phlegma passes back into knockout tower, and the gas that is not condensed is again through with recirculated water being three grades of condensing surfaces of refrigerant, the level Four condenser condenses that refrigerant temperature is-20～10 ℃; Phlegma is a subchloride liquid, and tail gas is hydrogen chloride gas;
Further, said chlorination reactor comprises first order reaction device and second order reaction device, and said first order reaction device comprises reacting cylinder body and is arranged on the heating and heat-insulating device on the reacting cylinder body; Said second order reaction device is a tubular structure, and second order reaction device inlet mouth and second order reaction device air outlet are set on it, and second order reaction device inlet mouth is communicated with the air outlet of first order reaction device;
Further, the first order reaction device of said chlorination reactor also comprises the charge heating conduit, and said charge heating conduit vertically is arranged in the reacting cylinder body, the corresponding setting of inlet mouth of charge heating duct inlet and reacting cylinder body;
Further, the pipeline that the first order reaction device is connected with the second order reaction device in the said chlorination reactor and the cylindrical of second order reaction device are provided with thermal insulation layer;
Further, on the first order reaction device of said chlorination reactor the safe release device is set.
In the present invention, subchloride is meant the mixture of monochloro methane and methylene dichloride.
Beneficial effect of the present invention is: technology of the present invention has increased the step that the material mixed gas with pyritous reaction mixture and monochloro methane and subchloride carries out heat exchange in chloride process; Preheating material gas mixture when making the reaction mixture cooling; Can recycle a large amount of higher-grade heat energy that reaction mixture has fully, effectively; Thereby save energy reduces production costs greatly; Simultaneously; Technology of the present invention changes the subsequent processing steps of reaction mixture into quenching, separation, condensation, rectifying by existing quenching, condensation, separation, rectifying; Reaction mixture after the quenching washing directly gets into knockout tower to be separated; Can further recycle chlorination reaction heat, reduce the steam consumption of knockout tower, reduce cost.
Description of drawings
In order to make the object of the invention, technical scheme and advantage clearer, will combine accompanying drawing that the present invention is made further detailed description below, wherein:
Fig. 1 is the process flow diagram of embodiment one;
Fig. 2 is the process flow diagram of embodiment two;
Fig. 3 is the structural representation of the chlorination reactor of embodiment two.
Embodiment
Below will carry out detailed description to the preferred embodiments of the present invention with reference to accompanying drawing.
Embodiment one
As shown in Figure 1, the methane chloride production process that utilizes chlorination reaction heat of present embodiment comprises hydrochlorinate operation and chloride process:
Hydrochlorinate operation: methanol gas and hydrogen chloride gas are mixed 1 reaction of back feeding hydrochlorination device; Reaction mixture obtains monochloro methane gas behind the water that refrigerating unit 2 cools off, absorption unit 3 is removed the intact hydrogenchloride of unreacted, sulfuric acid drying installation 4 is removed generation; Under hydrochlorination system self pressure of 0.4～0.8Mpa, obtain monochloro methane liquid for-20～10 ℃ condensing surface 5 condensations again through refrigerant temperature; Get into monochloro methane storage tank 6, subsequent use;
Chloride process: the monochloro methane liquid that the hydrochlorinate operation is made and from chlorination reaction mixture isolated subchloride liquid after pump 7 and pump 20 are forced into 0.8～1.2Mpa, mix respectively; Raw materials mix liquid is the first-stage condenser 14 of heating agent, is the first-class heat exchanger 8 of heating agent with the washings of quenching tower, is the secondary heat exchanger 9 of heating agent with the water vapor, mixes with chlorine after being three grades of interchanger 10 heat exchange, gasification, preheating of heating agent with the reaction mixture through the gas that steams with the knockout tower cat head; Feeding chlorination reactor 11 is 350～450 ℃ of reactions down in temperature; Reaction mixture is through three grades of interchanger 10 heat exchange coolings; Quenching tower 12 cooling washing backs get into knockout tower 13 and separate; The gas that the knockout tower cat head steams is through first-stage condenser 14; With recirculated water is secondary condenser 15 condensations of refrigerant; Phlegma passes back into knockout tower 13; Through being that three grades of condensing surfaces 16, refrigerant temperature of refrigerant are-20～10 ℃ level Four condensing surface 17 condensations with recirculated water, phlegma is that subchloride liquid gets into the raw material recycled of low chlorated liquid storage tank 19 as chloride process to the gas that is not condensed again, tail gas hydrogenchloride after 18 preheatings of hydrogenchloride interchanger as the raw material recycled of hydrochlorinate operation; The mixed solution that separation Tata still obtains obtains methylene dichloride, trichloromethane and tetracol phenixin through rectifier unit 21 separation.
Present embodiment has increased the step that the material mixed gas with pyritous reaction mixture and monochloro methane and subchloride carries out heat exchange in chloride process; Preheating material gas mixture when making the reaction mixture cooling; Recycle a large amount of higher-grade heat energy that reaction mixture has fully, effectively; Thereby save energy reduces production costs greatly; Simultaneously; Present embodiment changes the subsequent processing steps of reaction mixture into quenching, separation, condensation, rectifying by existing quenching, condensation, separation, rectifying; Reaction mixture after the quenching washing directly gets into knockout tower to be separated; Further recycle chlorination reaction heat, thereby reduce the steam consumption of knockout tower, reduce cost; It is liquid that present embodiment also adopts the monochloro methane condensation of gas that the hydrochlorinate operation is made; Send into the method for chloride process after pumping up again, gasifying, substitute the monochloro methane gas that in the existing technology hydrochlorinate operation is made is sent into chloride process after compressor compresses method, substitute with low price, pump that energy consumption is low cost an arm and a leg, compressor that energy consumption is high; Not only can reduce investment outlay; Energy efficient, and can avoid the product loss that causes because of compressor leakage, reduce environmental pollution; Reduce cost greatly, make more convenient operation, safer; In addition, the gas that the knockout tower cat head steams promptly gets subchloride liquid and hydrogen chloride gas through recirculated water and temperature for-20～10 ℃ refrigerant condensation, does not need cryogenic unit, can further reduce investment outlay, and energy efficient reduces cost.
Embodiment two
As shown in Figure 2, the methane chloride production process that utilizes chlorination reaction heat of present embodiment and the difference of embodiment one are: adopt improved chlorination reactor and between three grades of interchanger 10 and chlorination reactor 11, increased well heater 22.
As shown in Figure 3; Improved chlorination reactor comprises first order reaction device 111 and second order reaction device 117; First order reaction device 111 comprises reacting cylinder body 112, charge heating conduit 113, inlet pipe 114, is arranged on air outlet 115 and heating and heat-insulating device 116 on the reacting cylinder body 112; Charge heating conduit 113 vertically is arranged in the reacting cylinder body 112, the corresponding setting of inlet mouth of 113 imports of charge heating conduit and reacting cylinder body 112; Second order reaction device 117 is a tubular structure, and second order reaction device inlet mouth 118 and second order reaction device air outlet 1112 are set on it; The air outlet 115 of first order reaction device 111 is connected with second order reaction device inlet mouth 118 through pipeline 119, and second order reaction device air outlet 1112 is connected with three grades of interchanger 10; In addition, the cylindrical at pipeline 119 and second order reaction device 117 also is provided with thermal insulation layer 1110, the minimizing heat radiation; Safe release device 1111 also is set on reacting cylinder body 112, when the intravital gaseous tension of tube surpasses set(ting)value, can reduces pressure, avoid hypertonia to set off an explosion through this device; Heating and heat-insulating device 116 is used for before feeding material mixed gas, making charge heating conduit 113 be preheated to certain temperature.
In the chloride process; After the material mixed gas heater via 22 of monochloro methane, subchloride and chlorine is preheated to 250～350 ℃ of temperature; Feed chlorination reactor 11; In first order reaction device 111, be preheated to earlier temperature and start reaction for 300～400 ℃, get into fully reaction in the second order reaction device 117 again, make chlorine reaction complete.
Compare with the chlorination reactor of being made up of single first order reaction device in the prior art, the improved chlorination reactor of present embodiment is made up of first order reaction device and second order reaction device that split connects, and the first order reaction device is as starting reaction unit; The second order reaction device is as the main reaction device, and the second order reaction device does not receive the influence of heating and heat-insulating device intensification, and top temperature is no more than 450 ℃ during use; Material requires relatively low, so under the situation with equivalent responses ability, improved chlorination reactor investment cost reduces; Manufacture difficulty reduces; Transportation and install more conveniently react more abundant, safer, the raising chlorine utilization.
Explanation is at last; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although through invention has been described with reference to the preferred embodiments of the present invention; But those of ordinary skill in the art should be appreciated that and can make various changes to it in form with on the details, and the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (7)
1. utilize the methane chloride production process of chlorination reaction heat; Comprise hydrochlorinate operation and chloride process; It is characterized in that: chloride process be monochloro methane gas that the hydrochlorinate operation is made and from chlorination reaction mixture isolated subchloride gas mix, after the preheating, mix with chlorine, feed chlorination reactor and react; Reaction mixture carries out heat exchange with the preheating material gas mixture through the material mixed gas of interchanger and monochloro methane and subchloride earlier; The back entering quenching tower cooling of self being lowered the temperature is simultaneously washed, and gets into knockout tower again and separates, and the gas that the knockout tower cat head steams obtains hydrogen chloride gas and subchloride liquid through condensation separation; Hydrogen chloride gas is as the raw material recycled of hydrochlorinate operation, the subchloride liquid raw material recycled of back as chloride process that gasified; The mixed solution that separation Tata still obtains obtains methylene dichloride, trichloromethane and tetracol phenixin through rectifying separation; Said subchloride is meant the mixture of monochloro methane and methylene dichloride.
2. the methane chloride production process that utilizes chlorination reaction heat according to claim 1; It is characterized in that: said hydrochlorinate operation is that methanol gas and hydrogen chloride gas are mixed the reaction of back feeding hydrochlorination device; Reaction mixture obtains monochloro methane gas after cooling, absorption, drying, utilize self pressure of hydrochlorination system that it is condensed into liquid with refrigerant again; Said chloride process be monochloro methane liquid that the hydrochlorinate operation is made and from chlorination reaction mixture the isolated subchloride liquid back of pumping up respectively mix, after gasification, preheating, mixes again with chlorine, the feeding chlorination reactor reacts.
3. the methane chloride production process that utilizes chlorination reaction heat according to claim 2; It is characterized in that: the gas that said knockout tower cat head steams is the first-stage condenser of refrigerant, is the secondary condenser condensation of refrigerant with recirculated water through the raw materials mix liquid with monochloro methane and subchloride; Phlegma passes back into knockout tower; The gas that is not condensed is again through with recirculated water being three grades of condensing surfaces of refrigerant, the level Four condenser condenses that refrigerant temperature is-20～10 ℃; Phlegma is a subchloride liquid, and tail gas is hydrogen chloride gas.
4. based on the described methane chloride production process that utilizes chlorination reaction heat of claim 3; It is characterized in that: said chlorination reactor comprises first order reaction device and second order reaction device, and said first order reaction device comprises reacting cylinder body and is arranged on the heating and heat-insulating device on the reacting cylinder body; Said second order reaction device is a tubular structure, and second order reaction device air inlet and second order reaction device gas outlet are set on it, and second order reaction device air inlet is communicated with the gas outlet of first order reaction device.
5. the methane chloride production process that utilizes chlorination reaction heat according to claim 4; It is characterized in that: the first order reaction device of said chlorination reactor also comprises the charge heating conduit; Said charge heating conduit vertically is arranged in the reacting cylinder body, the corresponding setting of inlet mouth of charge heating duct inlet and reacting cylinder body.
6. the methane chloride production process that utilizes chlorination reaction heat according to claim 5 is characterized in that: the pipeline that the first order reaction device is connected with the second order reaction device in the said chlorination reactor and the cylindrical of second order reaction device are provided with thermal insulation layer.
7. the methane chloride production process that utilizes chlorination reaction heat according to claim 6 is characterized in that: on the first order reaction device of said chlorination reactor the safe release device is set.
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| CN200910103331A CN101497551B (en) | 2009-03-06 | 2009-03-06 | Methane chlorides production process utilizing chlorination reaction heat |
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| CN200910103331A CN101497551B (en) | 2009-03-06 | 2009-03-06 | Methane chlorides production process utilizing chlorination reaction heat |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497085B (en) * | 2012-03-20 | 2017-07-04 | 文乃建化学工程公司 | Two coproduction and three joint production process of production monochloro methane, methane chloride and tetrachloro-ethylene |
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| CN106008146A (en) * | 2016-06-08 | 2016-10-12 | 刘世刚 | Combined production system for chloroethylene and tetrachloroethylene |
| CN106146248B (en) * | 2016-06-28 | 2018-08-21 | 乳源东阳光电化厂 | A kind of energy-efficient methane chloride production process |
| CN106478360B (en) * | 2016-10-08 | 2019-03-12 | 宁波巨化化工科技有限公司 | The catalytic chlorination system of methylene chloride yield ratio can be improved |
| CN106495981A (en) * | 2016-11-25 | 2017-03-15 | 江苏梅兰化工有限公司 | Monochloro methane gas heat Application way and device after compressing in methane chloride production |
| CN106699503B (en) * | 2016-12-22 | 2020-03-27 | 山东东岳氟硅材料有限公司 | Energy-saving thermal chlorination process |
| CN111298726A (en) * | 2018-12-11 | 2020-06-19 | 新特能源股份有限公司 | Fluidization system for fluidized reaction |
| CN109627142B (en) * | 2018-12-12 | 2021-10-22 | 山东东岳氟硅材料有限公司 | Treatment method and treatment system for byproduct tail gas in tetrachloroethylene production |
| CN109647321A (en) * | 2019-01-18 | 2019-04-19 | 江苏海企技术工程股份有限公司 | A kind of energy saving thermal chlorination reaction unit for methane chloride |
| CN110041162A (en) * | 2019-05-16 | 2019-07-23 | 江西理文化工有限公司 | A kind of methane chloride green production process |
| CN110724027A (en) * | 2019-09-26 | 2020-01-24 | 杨皓 | Improved process for green production of methane chloride |
| CN110724028A (en) * | 2019-09-26 | 2020-01-24 | 杨皓 | Improved process for preparing chloroform by carbon tetrachloride gas-phase hydrogenation conversion |
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| CN103497085B (en) * | 2012-03-20 | 2017-07-04 | 文乃建化学工程公司 | Two coproduction and three joint production process of production monochloro methane, methane chloride and tetrachloro-ethylene |
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