CN112337127A - Trichloromethane rectifying device and rectifying method thereof - Google Patents
Trichloromethane rectifying device and rectifying method thereof Download PDFInfo
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- CN112337127A CN112337127A CN202011215749.XA CN202011215749A CN112337127A CN 112337127 A CN112337127 A CN 112337127A CN 202011215749 A CN202011215749 A CN 202011215749A CN 112337127 A CN112337127 A CN 112337127A
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229960001701 chloroform Drugs 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000010992 reflux Methods 0.000 claims abstract description 125
- 239000000047 product Substances 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 35
- 239000012071 phase Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 33
- 238000000605 extraction Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 17
- 239000012043 crude product Substances 0.000 claims description 13
- 230000008676 import Effects 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 8
- 239000007792 gaseous phase Substances 0.000 claims description 3
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 18
- 230000008569 process Effects 0.000 description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000005265 energy consumption Methods 0.000 description 10
- 229910000975 Carbon steel Inorganic materials 0.000 description 8
- 238000009835 boiling Methods 0.000 description 8
- 239000010962 carbon steel Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 230000009467 reduction Effects 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007667 floating Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- VZIAWSKPWXLPHJ-UHFFFAOYSA-L aluminum magnesium difluoride Chemical compound [F-].[F-].[Mg++].[Al+3] VZIAWSKPWXLPHJ-UHFFFAOYSA-L 0.000 description 1
- 230000003444 anaesthetic effect Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical group 0.000 description 1
- 239000002316 fumigant Substances 0.000 description 1
- 238000007038 hydrochlorination reaction Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a trichloromethane rectifying device which comprises a low-pressure rectifying tower, a low-pressure rectifying tower condenser, a low-pressure rectifying tower reboiler, a low-pressure rectifying tower kettle pump, a low-pressure rectifying tower reflux groove, a low-pressure rectifying tower reflux pump, a pressurized rectifying tower reboiler, a pressurized rectifying tower reflux groove and a pressurized rectifying tower reflux pump. The invention also discloses a method for rectifying trichloromethane by using the device. The invention has the advantages of energy saving, high efficiency, less equipment investment, low operation cost and long operation period.
Description
Technical Field
The invention relates to the technical field of methane chloride purification, in particular to a trichloromethane rectifying device and a rectifying method thereof.
Background
Chloroform is also called chloroform, is colorless transparent liquid, has special smell, and can be mixed with ethanol, benzene, ether, petroleum ether, carbon tetrachloride, carbon disulfide, oil, etc. The relative density of the trichloromethane is 1.4840, the freezing point is-63.5 ℃, and the boiling point is 61-62 ℃. Chloroform is an important organic synthetic raw material, is mainly used for producing freon (F-21, F-22 and F-23), dye and medicine, and is commonly used as an anesthetic in medicine. Can be used as solvent and extractant for antibiotics, perfume, oil, resin, and rubber. The trichloromethane and the carbon tetrachloride are mixed to prepare the non-freezing fireproof liquid. It is also used for propellant of aerosol, fumigant of grain and standard liquid for calibrating temperature.
At present, the methods for industrially producing chloroform mainly comprise:
(1) process route using methanol and hydrogen chloride as raw materials
Methane chloride production can be easily controlled by utilizing the reaction of hydrogen chloride with methanol, and thus methanol and hydrogen chloride as starting materials are attractive process routes for producing methane chloride. The process route comprises the steps of firstly reacting methanol with dry hydrogen chloride gas to prepare chloromethane, and then chlorinating and separating under the liquid phase condition to prepare dichloromethane, chloroform and carbon tetrachloride. The separation process comprises the operations of water washing, alkali washing and rectification.
For example, CN110041162A discloses a green production process of methane chloride, which comprises hydrochlorination process, chlorination process, refining process, tail gas absorption process, liquid chlorine vaporization process, waste water treatment process, tail gas absorption and high-boiling residue incineration process, and carbon tetrachloride conversion process.
(2) Process route for preparing chloroform by gas-phase hydrogenation and dechlorination of carbon tetrachloride
The process route is a hydrodechlorination reaction carried out by carbon tetrachloride and hydrogen under the action of a catalyst. The reaction can be carried out either continuously or batchwise; the reaction may be carried out in the liquid phase in the presence of a solvent; gas phase hydrodechlorination may also be carried out.
For example, CN1903810A discloses a method for preparing chloroform by gas-phase hydrodechlorination of carbon tetrachloride, which is a hydrodechlorination reaction of carbon tetrachloride and hydrogen under the action of a catalyst, wherein the carrier of the catalyst is a fluoride, the active component is platinum or a mixture of platinum and palladium, the content of platinum is 0.1-3% of the weight of the catalyst, and the content of palladium is 0-1% of the weight of the catalyst. The method adopts the fluoride carrier, so that the generation of byproducts such as methane and the like is reduced while the higher conversion rate of carbon tetrachloride is kept, the higher chloroform yield is kept, and the longer service life of the catalyst can be kept. It is possible to use only aluminum fluoride or magnesium fluoride as the support, and it is more preferable to use an aluminum fluoride-magnesium fluoride mixture as the support.
At present, a trichloromethane rectification system generally comprises a crude product feed pump, a rectification tower, a tower kettle reboiler, a tower top condenser and a reflux device, wherein when the rectification system operates, a trichloromethane crude product is introduced into the rectification tower through the crude product feed pump, a large amount of steam is introduced through the tower kettle reboiler to provide heat required by the tower kettle, a trichloromethane gas phase product at the tower top enters the tower top condenser, the trichloromethane gas phase is condensed through the cold energy introduced into the tower top condenser, a part of the obtained trichloromethane product flows back to the tower top, and a part of the obtained trichloromethane product is extracted as a product. The disadvantages are that the energy consumption of unit product is higher, the operation cost is high, and the steam consumption of unit product is 450-.
The double-tower double-effect rectifying device is widely applied to rectifying systems for separating materials with different components, and has the advantages of low energy consumption, low pressure reduction, simple operation control and the like. However, the trichloromethane crude product has complex components, and the trichloromethane contains partial heavy-boiling substances, the trichloromethane is easy to decompose and acidify at high temperature, the heavy-boiling substances are carbonized and carbonized to cause corrosion of tower top equipment, a reboiler of a tower kettle is blocked, the boiling point of the trichloromethane is 61 ℃, the double-tower double-effect rectification can be established only when the temperature difference exists between a tower kettle of a low-pressure tower and a pressurized tower top, the conventional plate rectification is adopted in the existing trichloromethane rectification system, so that the double-tower double-effect rectification device is difficult to apply to the rectification and purification of the trichloromethane, and therefore, how to apply the double-tower double-effect rectification device to the rectification and purification of the trichloromethane is required, so that the energy consumption and the operation cost are reduced, the long-period operation.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the trichloromethane rectifying device and the trichloromethane rectifying method which have the advantages of energy conservation, high efficiency, less equipment investment, low operation cost and long operation period.
In order to achieve the purpose, the invention adopts the technical scheme that: a trichloromethane rectifying device comprises a low-pressure rectifying tower, a low-pressure rectifying tower condenser, a low-pressure rectifying tower reboiler, a low-pressure rectifying tower kettle pump, a low-pressure rectifying tower reflux groove, a low-pressure rectifying tower reflux pump, a pressurized rectifying tower reboiler, a pressurized rectifying tower reflux groove and a pressurized rectifying tower reflux pump, and is characterized in that a gas phase outlet of the low-pressure rectifying tower is connected with an inlet of the low-pressure rectifying tower condenser, an outlet of the low-pressure rectifying tower condenser is connected with an inlet of the low-pressure rectifying tower reflux groove, an outlet of the low-pressure rectifying tower reflux groove is connected with an inlet of the low-pressure rectifying tower reflux pump, an outlet of the low-pressure rectifying tower reflux pump is connected with a reflux inlet of the low-pressure rectifying tower, and a tower kettle liquid outlet of the low-pressure rectifying tower is respectively connected with an inlet of the low-pressure rectifying tower kettle pump and a tower kettle liquid inlet of the low-pressure rectifying tower reboiler, the export of low pressure rectifying column tower cauldron pump with the feed inlet of pressurized rectifying column is connected, the tower cauldron liquid export of low pressure rectifying column reboiler with the tower cauldron liquid import of low pressure rectifying column links to each other, the gaseous phase export of pressurized rectifying column with the heat medium access connection of low pressure rectifying column reboiler, the heat medium export of low pressure rectifying column reboiler with the import of pressurized rectifying column reflux groove links to each other, the export of pressurized rectifying column reflux groove with the access connection of pressurized rectifying column reflux pump, the export of pressurized rectifying column reflux pump with the backward flow access connection of pressurized rectifying column, the tower cauldron liquid export of pressurized rectifying column with the tower cauldron liquid access connection of pressurized rectifying column reboiler, the tower cauldron liquid export of pressurized rectifying column reboiler with the tower cauldron liquid access connection of pressurized rectifying column is provided with the inlet pipe between the tower cauldron liquid of low pressure rectifying column reboiler The system comprises a line, wherein the low-pressure rectifying tower is provided with a low-pressure rectifying tower product extraction pipeline, and the pressurized rectifying tower is provided with a pressurized rectifying tower product extraction pipeline.
In a preferred embodiment of the present invention, a high-boiling-point substance branch pipe is further provided between the bottom outlet of the pressure distillation column and the bottom inlet line of the reboiler of the pressure distillation column.
As a preferred embodiment of the present invention, the low pressure rectification column is a packed column to further reduce the pressure drop; the pressurized rectifying tower is a float valve tower.
The invention also discloses a method for rectifying trichloromethane by using the device, wherein a trichloromethane crude product is introduced into a low-pressure rectifying tower reboiler through a feeding pipeline, after a material is evaporated by the low-pressure rectifying tower reboiler, a gas phase at the tower top is condensed by a low-pressure rectifying tower condenser, the obtained condensate sequentially flows back to the low-pressure rectifying tower through a low-pressure rectifying tower reflux groove and a low-pressure rectifying tower reflux pump, and the discharge of the tower kettle of the low-pressure rectifying tower is pumped into a pressurized rectifying tower through the tower kettle of the low-pressure rectifying tower; and (3) introducing all the gas phase at the top of the pressurized rectifying tower into a reboiler of the low-pressure rectifying tower, condensing the gas phase at the top of the pressurized rectifying tower into a liquid phase after exchanging heat with the materials at the bottom of the low-pressure rectifying tower, refluxing the liquid phase into the pressurized rectifying tower through a reflux tank of the pressurized rectifying tower and a reflux pump of the pressurized rectifying tower in sequence, and obtaining a rectified trichloromethane product from a product extraction pipeline of the low-pressure rectifying tower and a product extraction pipeline of the pressurized rectifying tower respectively.
As a preferred embodiment of the invention, the flow rate of the trichloromethane crude product is 5-15 t/h.
In a preferred embodiment of the present invention, the low-pressure distillation column pressure is-30 to-80 KPa, and the pressurized distillation column pressure is 50 to 95 KPa.
In a preferred embodiment of the present invention, the reflux ratio of the low-pressure distillation column is 3.5 to 5.
As a preferred embodiment of the invention, the condenser temperature of the low-pressure rectification column is 35-45 ℃.
As a preferred embodiment of the present invention, the pressurized distillation column reboiler temperature is 105-125 ℃.
In a preferred embodiment of the present invention, the reflux ratio of the pressurized rectifying column is 4 to 6.
The invention relates to a trichloromethane rectifying device, which adopts double-effect rectification and runs in series with two towers, wherein a gas phase outlet of a pressurized rectifying tower is connected with a heating medium inlet of a reboiler of a low-pressure rectifying tower, a heating medium outlet of the reboiler of the low-pressure rectifying tower is connected with an inlet of a reflux groove of the pressurized rectifying tower, a reboiler of a tower kettle of the low-pressure rectifying tower does not need heat supply, the heat is provided by the gas phase of the pressurized rectifying tower, the heat of the trichloromethane gas phase at the tower top of the pressurized rectifying tower is fully utilized, and a condensing system is not needed at the tower top of the pressurized rectifying tower, so that the energy consumption of the whole trichloromethane rectifying system is reduced by 40 percent compared with the prior art.
Compared with the prior art, the invention has the following beneficial effects:
1. the energy consumption is low, the invention changes the existing trichloromethane rectification process, and adopts double-effect rectification, the gas phase outlet of the pressurized rectification tower is connected with the heating medium inlet of the reboiler of the low-pressure rectification tower, the heating medium outlet of the reboiler of the low-pressure rectification tower is connected with the inlet of the reflux groove of the pressurized rectification tower, the reboiler of the tower kettle of the low-pressure rectification tower does not need heat supply, the heat is provided by the gas phase of the pressurized rectification tower, the heat of the trichloromethane gas phase at the top of the pressurized rectification tower is fully utilized, and a condensation system is not needed to be arranged at the top of the pressurized rectification tower, so that the energy consumption of the whole trichloromethane rectification system is obviously reduced compared with the existing process, the high efficiency and energy conservation are really realized on the basis of improving;
2. the equipment investment is small, the operation cost is low, and the gas phase outlet of the pressurized rectifying tower is connected with the heating medium inlet of the reboiler of the low-pressure rectifying tower, so that a condensing system does not need to be arranged at the top of the pressurized rectifying tower, the equipment investment is effectively reduced, the rectifying process is simplified, the operation is convenient, and the operation cost is low;
3. the operation period is long, the invention adopts double-effect rectification, two towers are connected in series for operation, the gas phase outlet of the pressurized rectifying tower is connected with the heating medium inlet of the reboiler of the low-pressure rectifying tower, the heat of the trichloromethane gas phase at the top of the pressurized rectifying tower is fully utilized, the pressure difference and the temperature of the whole tower are reduced, the problems that the trichloromethane is easy to decompose and acidify at high temperature, heavy boilers are easy to carbonize, the corrosion of tower top equipment is caused, and the reboiler of the tower kettle is blocked are thoroughly solved, so that the device can stably operate for a long period;
4. the rectification efficiency is high, and the product purity is over 99.99 percent.
Drawings
FIG. 1 is a schematic diagram of a chloroform rectification apparatus of the present invention.
In the figure, a low-pressure rectifying tower 1, a low-pressure rectifying tower condenser 2, a low-pressure rectifying tower reboiler 3, a low-pressure rectifying tower reflux tank 4, a low-pressure rectifying tower kettle pump 5, a low-pressure rectifying tower reflux pump 6, a pressurized rectifying tower 7, a pressurized rectifying tower reboiler 8, a pressurized rectifying tower reflux tank 9, pressurized rectifying tower reflux pumps 10 and 11 are feeding pipelines, 12 is a low-pressure rectifying tower product extraction pipeline, 13 is a pressurized rectifying tower product extraction pipeline, and 14 is a high-boiling substance branch pipe.
Detailed Description
The invention relates to a trichloromethane rectifying device, which comprises a low-pressure rectifying tower 1, a low-pressure rectifying tower condenser 2, a low-pressure rectifying tower reboiler 3, a low-pressure rectifying tower reflux groove 4, a low-pressure rectifying tower kettle pump 5, a low-pressure rectifying tower reflux pump 6, a pressurized rectifying tower 7, a pressurized rectifying tower reboiler 8, a pressurized rectifying tower reflux groove 9, a pressurized rectifying tower reflux pump 10, wherein a gas phase outlet of the low-pressure rectifying tower 1 is connected with an inlet of the low-pressure rectifying tower condenser 2, an outlet of the low-pressure rectifying tower condenser 2 is connected with an inlet of the low-pressure rectifying tower reflux groove 4, an outlet of the low-pressure rectifying tower reflux groove 4 is connected with an inlet of the low-pressure rectifying tower reflux pump 6, an outlet of the low-pressure rectifying tower reflux pump 6 is connected with a reflux inlet of the low-pressure rectifying tower 1, a tower kettle liquid outlet of the low-pressure rectifying tower 1 is respectively connected with an inlet of the low-pressure rectifying tower kettle pump 5 and a kettle liquid inlet of the low-pressure rectifying tower, the outlet of the tower kettle pump 5 of the low-pressure rectifying tower is connected with the feed inlet of the pressurized rectifying tower 7, the tower kettle outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the tower kettle inlet of the low-pressure rectifying tower 1, the gas phase outlet of the pressurized rectifying tower 7 is connected with the heat medium inlet of the reboiler 3 of the low-pressure rectifying tower, the heat medium outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the inlet of the reflux groove 9 of the pressurized rectifying tower, the outlet of the reflux groove 9 of the pressurized rectifying tower is connected with the inlet of the reflux pump 10 of the pressurized rectifying tower, the outlet of the reflux pump 10 of the pressurized rectifying tower is connected with the reflux inlet of the pressurized rectifying tower 7, the tower kettle outlet of the pressurized rectifying tower 7 is connected with the tower kettle inlet of the pressurized rectifying tower 8, a high-boiling material branch pipe 14 is arranged between the tower kettle outlet of the pressurized rectifying tower 7 and the inlet pipe of the reboiler 8 of the pressurized rectifying tower, and the kettle outlet of the reboiler 8 of the pressurized rectifying tower is connected with the kettle inlet pipe of the pressurized rectifying tower 7. A feeding pipeline 11 is arranged between a tower bottom liquid outlet of the low-pressure rectifying tower 1 and a tower bottom liquid inlet pipeline of the low-pressure rectifying tower reboiler 3, the low-pressure rectifying tower 1 is provided with a low-pressure rectifying tower product extraction pipeline 12, and the pressurized rectifying tower 7 is provided with a pressurized rectifying tower product extraction pipeline 13.
The technological process for purifying the trichloromethane by adopting the trichloromethane rectifying device comprises the following steps: introducing a trichloromethane crude product into a low-pressure rectifying tower reboiler 3 through a feeding pipeline 11, after the material is evaporated by the low-pressure rectifying tower reboiler 3, condensing a gas phase at the top of a low-pressure rectifying tower 1 by a low-pressure rectifying tower condenser 2, refluxing obtained condensate into the low-pressure rectifying tower 1 through a low-pressure rectifying tower reflux groove 4 and a low-pressure rectifying tower reflux pump 6 in sequence, and sending tower kettle discharge of the low-pressure rectifying tower 1 into a pressurized rectifying tower 7 through a low-pressure rectifying tower kettle pump 5; after a material from a tower kettle pump 5 of the low-pressure rectifying tower is heated by steam of a reboiler 8 of the pressurizing rectifying tower, the gas phase at the top of the pressurizing rectifying tower 7 is completely introduced into the reboiler 3 of the low-pressure rectifying tower, after heat exchange is carried out with the material at the bottom of the low-pressure rectifying tower 1, the gas phase at the top of the pressurizing rectifying tower 7 is condensed into a liquid phase, and the liquid phase sequentially flows back into the pressurizing rectifying tower 1 through a reflux groove 9 of the pressurizing rectifying tower and a reflux pump 10 of the pressurizing rectifying tower, and a trichloromethane product is obtained by respectively extracting from a product extraction pipeline 12 of the low-pressure rectifying tower and a product extraction pipeline 13 of the pressurizing rectifying tower. The high boiling substance accumulated in the bottom of the pressurized rectifying tower 7 can be discharged periodically through the branch pipe 14 and can be treated separately.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments and the accompanying drawings, it being understood that the following description is only for the purpose of explaining the present invention and is not intended to limit the present invention.
Example 1
A trichloromethane rectifying device comprises a low-pressure rectifying tower 1 (a structured packing tower, material carbon steel, the diameter of the tower is 1500mm), a low-pressure rectifying tower condenser 2, a low-pressure rectifying tower reboiler 3, a low-pressure rectifying tower reflux groove 4, a low-pressure rectifying tower kettle pump 5, a low-pressure rectifying tower reflux pump 6, a pressurized rectifying tower 7 (a floating valve tower, material carbon steel, the diameter of the tower is 1800mm), a pressurized rectifying tower reboiler 8, a pressurized rectifying tower reflux groove 9, a pressurized rectifying tower reflux pump 10, a gas phase outlet of the low-pressure rectifying tower 1 is connected with an inlet of the low-pressure rectifying tower condenser 2, an outlet of the low-pressure rectifying tower condenser 2 is connected with an inlet of the low-pressure rectifying tower reflux groove 4, an outlet of the low-pressure rectifying tower reflux groove 4 is connected with an inlet of the low-pressure rectifying tower reflux pump 6, an outlet of the low-pressure rectifying tower reflux pump 6 is connected with a reflux inlet of the low-pressure rectifying tower 1, and a kettle outlet of the low-pressure rectifying tower kettle 1 is respectively connected with an inlet of the low-pressure rectifying tower reboiler 5 and an inlet The tower bottom inlet is connected, the outlet of the tower bottom pump 5 of the low-pressure rectifying tower is connected with the feed inlet of the pressurized rectifying tower 7, the tower bottom outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the tower bottom inlet of the low-pressure rectifying tower 1, the gas phase outlet of the pressurized rectifying tower 7 is connected with the heat medium inlet of the reboiler 3 of the low-pressure rectifying tower, the heat medium outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the inlet of the reflux groove 9 of the pressurized rectifying tower, the outlet of the reflux groove 9 of the pressurized rectifying tower is connected with the inlet of the reflux pump 10 of the pressurized rectifying tower, the outlet of the reflux pump 10 of the pressurized rectifying tower is connected with the reflux inlet of the pressurized rectifying tower 7, the tower bottom outlet of the pressurized rectifying tower 7 is connected with the tower bottom inlet of the reboiler 8 of the pressurized rectifying tower, a high-boiling-point substance branch pipe 14 is arranged between a tower bottom outlet of the pressurized rectifying tower 7 and a tower bottom inlet pipe of the pressurized rectifying tower reboiler 8, and the tower bottom outlet of the pressurized rectifying tower reboiler 8 is connected with a tower bottom inlet of the pressurized rectifying tower 7. A feeding pipeline 11 is arranged between a tower bottom liquid outlet of the low-pressure rectifying tower 1 and a tower bottom liquid inlet pipeline of the low-pressure rectifying tower reboiler 3, the low-pressure rectifying tower 1 is provided with a low-pressure rectifying tower product extraction pipeline 12, and the pressurized rectifying tower 7 is provided with a pressurized rectifying tower product extraction pipeline 13.
When the device is used for rectifying the trichloromethane, the technological parameters are as follows:
the feeding speed of the trichloromethane crude product is as follows; flow rate of 7t/h
The pressure of the low-pressure rectifying tower is as follows; -45KPa
The condenser temperature of the low-pressure rectifying tower is as follows; 42 deg.C
The temperature of a reboiler of the low-pressure rectifying tower is as follows; 48 deg.C
The reflux ratio of the low-pressure rectifying tower is as follows: 3.8
The pressure of the pressurized rectifying tower is as follows: 80KPa
The temperature of the reboiler of the pressurized rectifying tower is as follows: 105 ℃ C
The reflux ratio of the pressurized rectifying tower is as follows: 5
And (3) operating results: the device runs stably, unit energy consumption reduction and elastic operation improvement are realized, the product purity reaches 99.99%, the unit steam consumption is reduced by 40%, and the energy-saving effect is obvious.
Example 2
The utility model provides a trichloromethane rectifier unit, including low pressure rectifying column 1 (regular packed column, the material carbon steel, the tower footpath is 1600mm), low pressure rectifying column condenser 2, low pressure rectifying column reboiler 3, low pressure rectifying column backward flow groove 4, low pressure rectifying column cauldron pump 5, low pressure rectifying column backward flow pump 6, pressurized rectifying column 7 (floating valve tower, the material carbon steel, the tower footpath is 2000mm), pressurized rectifying column reboiler 8, pressurized rectifying column backward flow groove 9, pressurized rectifying column backward flow pump 10, the gaseous phase export of low pressure rectifying column 1 links to each other with the import of low pressure rectifying column condenser 2, the export of low pressure rectifying column condenser 2 and the import of low pressure rectifying column backward flow groove 4 are connected, the export of low pressure rectifying column backward flow groove 4 and the import of low pressure rectifying column backward flow pump 6 are connected, the export of low pressure rectifying column backward flow pump 6 and the backward flow import of low pressure rectifying column 1 are connected, the cauldron export of low pressure rectifying column 1 respectively with the import of low pressure rectifying column reboiler 5 and the import of low pressure rectifying column reboiler 3 with low pressure rectifying column The tower bottom inlet is connected, the outlet of the tower bottom pump 5 of the low-pressure rectifying tower is connected with the feed inlet of the pressurized rectifying tower 7, the tower bottom outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the tower bottom inlet of the low-pressure rectifying tower 1, the gas phase outlet of the pressurized rectifying tower 7 is connected with the heat medium inlet of the reboiler 3 of the low-pressure rectifying tower, the heat medium outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the inlet of the reflux groove 9 of the pressurized rectifying tower, the outlet of the reflux groove 9 of the pressurized rectifying tower is connected with the inlet of the reflux pump 10 of the pressurized rectifying tower, the outlet of the reflux pump 10 of the pressurized rectifying tower is connected with the reflux inlet of the pressurized rectifying tower 7, the tower bottom outlet of the pressurized rectifying tower 7 is connected with the tower bottom inlet of the reboiler 8 of the pressurized rectifying tower, a high-boiling-point substance branch pipe 14 is arranged between a tower bottom outlet of the pressurized rectifying tower 7 and a tower bottom inlet pipe of the pressurized rectifying tower reboiler 8, and the tower bottom outlet of the pressurized rectifying tower reboiler 8 is connected with a tower bottom inlet of the pressurized rectifying tower 7. A feeding pipeline 11 is arranged between a tower bottom liquid outlet of the low-pressure rectifying tower 1 and a tower bottom liquid inlet pipeline of the low-pressure rectifying tower reboiler 3, the low-pressure rectifying tower 1 is provided with a low-pressure rectifying tower product extraction pipeline 12, and the pressurized rectifying tower 7 is provided with a pressurized rectifying tower product extraction pipeline 13.
When the device is used for rectifying the trichloromethane, the technological parameters are as follows:
the feeding speed of the trichloromethane crude product is as follows; flow rate of 10t/h
The pressure of the low-pressure rectifying tower is as follows; -50KPa
The condenser temperature of the low-pressure rectifying tower is as follows; 40 deg.C
The temperature of a reboiler of the low-pressure rectifying tower is as follows; 46 deg.C
The reflux ratio of the low-pressure rectifying tower is as follows: 4.0
The pressure of the pressurized rectifying tower is as follows: 85KPa
The temperature of the reboiler of the pressurized rectifying tower is as follows: 107 deg.C
The reflux ratio of the pressurized rectifying tower is as follows: 5.5
And (3) operating results: the device runs stably, unit energy consumption reduction and elastic operation improvement are realized, the product purity reaches 99.99%, the unit steam consumption is reduced by 42%, and the energy-saving effect is obvious.
Example 3
A trichloromethane rectifying device comprises a low-pressure rectifying tower 1 (a structured packing tower, material carbon steel, the diameter of the tower is 1800mm), a low-pressure rectifying tower condenser 2, a low-pressure rectifying tower reboiler 3, a low-pressure rectifying tower reflux groove 4, a low-pressure rectifying tower kettle pump 5, a low-pressure rectifying tower reflux pump 6, a pressurized rectifying tower 7 (a floating valve tower, material carbon steel, the diameter of the tower is 2100mm), a pressurized rectifying tower reboiler 8, a pressurized rectifying tower reflux groove 9, a pressurized rectifying tower reflux pump 10, a gas phase outlet of the low-pressure rectifying tower 1 is connected with an inlet of the low-pressure rectifying tower condenser 2, an outlet of the low-pressure rectifying tower condenser 2 is connected with an inlet of the low-pressure rectifying tower reflux groove 4, an outlet of the low-pressure rectifying tower reflux groove 4 is connected with an inlet of the low-pressure rectifying tower reflux pump 6, an outlet of the low-pressure rectifying tower reflux pump 6 is connected with a reflux inlet of the low-pressure rectifying tower 1, and a kettle outlet of the low-pressure rectifying tower kettle 1 is respectively connected with an inlet of the low-pressure rectifying tower reboiler 5 and an inlet The tower bottom inlet is connected, the outlet of the tower bottom pump 5 of the low-pressure rectifying tower is connected with the feed inlet of the pressurized rectifying tower 7, the tower bottom outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the tower bottom inlet of the low-pressure rectifying tower 1, the gas phase outlet of the pressurized rectifying tower 7 is connected with the heat medium inlet of the reboiler 3 of the low-pressure rectifying tower, the heat medium outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the inlet of the reflux groove 9 of the pressurized rectifying tower, the outlet of the reflux groove 9 of the pressurized rectifying tower is connected with the inlet of the reflux pump 10 of the pressurized rectifying tower, the outlet of the reflux pump 10 of the pressurized rectifying tower is connected with the reflux inlet of the pressurized rectifying tower 7, the tower bottom outlet of the pressurized rectifying tower 7 is connected with the tower bottom inlet of the reboiler 8 of the pressurized rectifying tower, a high-boiling-point substance branch pipe 14 is arranged between a tower bottom outlet of the pressurized rectifying tower 7 and a tower bottom inlet pipe of the pressurized rectifying tower reboiler 8, and the tower bottom outlet of the pressurized rectifying tower reboiler 8 is connected with a tower bottom inlet of the pressurized rectifying tower 7. A feeding pipeline 11 is arranged between a tower bottom liquid outlet of the low-pressure rectifying tower 1 and a tower bottom liquid inlet pipeline of the low-pressure rectifying tower reboiler 3, the low-pressure rectifying tower 1 is provided with a low-pressure rectifying tower product extraction pipeline 12, and the pressurized rectifying tower 7 is provided with a pressurized rectifying tower product extraction pipeline 13.
When the device is used for rectifying the trichloromethane, the technological parameters are as follows:
the feeding speed of the trichloromethane crude product is as follows; flow rate of 12t/h
The pressure of the low-pressure rectifying tower is as follows; -55KPa
The condenser temperature of the low-pressure rectifying tower is as follows; 38 deg.C
The temperature of a reboiler of the low-pressure rectifying tower is as follows; 44 deg.C
The reflux ratio of the low-pressure rectifying tower is as follows: 4.2
The pressure of the pressurized rectifying tower is as follows: 90KPa
The temperature of the reboiler of the pressurized rectifying tower is as follows: 110 deg.C
The reflux ratio of the pressurized rectifying tower is as follows: 5.8
And (3) operating results: the device runs stably, unit energy consumption reduction and elastic operation improvement are realized, the product purity reaches 99.99%, the unit steam consumption is reduced by 44%, and the energy-saving effect is obvious.
Example 4
A trichloromethane rectifying device comprises a low-pressure rectifying tower 1 (a structured packing tower, material carbon steel, the diameter of the tower is 1700mm), a low-pressure rectifying tower condenser 2, a low-pressure rectifying tower reboiler 3, a low-pressure rectifying tower reflux groove 4, a low-pressure rectifying tower kettle pump 5, a low-pressure rectifying tower reflux pump 6, a pressurized rectifying tower 7 (a floating valve tower, material carbon steel, the diameter of the tower is 1900mm), a pressurized rectifying tower reboiler 8, a pressurized rectifying tower reflux groove 9, a pressurized rectifying tower reflux pump 10, a gas phase outlet of the low-pressure rectifying tower 1 is connected with an inlet of the low-pressure rectifying tower condenser 2, an outlet of the low-pressure rectifying tower condenser 2 is connected with an inlet of the low-pressure rectifying tower reflux groove 4, an outlet of the low-pressure rectifying tower reflux groove 4 is connected with an inlet of the low-pressure rectifying tower reflux pump 6, an outlet of the low-pressure rectifying tower reflux pump 6 is connected with a reflux inlet of the low-pressure rectifying tower 1, and a kettle outlet of the low-pressure rectifying tower kettle 1 is respectively connected with an inlet of the low-pressure rectifying tower reboiler 5 and an inlet The tower bottom inlet is connected, the outlet of the tower bottom pump 5 of the low-pressure rectifying tower is connected with the feed inlet of the pressurized rectifying tower 7, the tower bottom outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the tower bottom inlet of the low-pressure rectifying tower 1, the gas phase outlet of the pressurized rectifying tower 7 is connected with the heat medium inlet of the reboiler 3 of the low-pressure rectifying tower, the heat medium outlet of the reboiler 3 of the low-pressure rectifying tower is connected with the inlet of the reflux groove 9 of the pressurized rectifying tower, the outlet of the reflux groove 9 of the pressurized rectifying tower is connected with the inlet of the reflux pump 10 of the pressurized rectifying tower, the outlet of the reflux pump 10 of the pressurized rectifying tower is connected with the reflux inlet of the pressurized rectifying tower 7, the tower bottom outlet of the pressurized rectifying tower 7 is connected with the tower bottom inlet of the reboiler 8 of the pressurized rectifying tower, a high-boiling-point substance branch pipe 14 is arranged between a tower bottom outlet of the pressurized rectifying tower 7 and a tower bottom inlet pipe of the pressurized rectifying tower reboiler 8, and the tower bottom outlet of the pressurized rectifying tower reboiler 8 is connected with a tower bottom inlet of the pressurized rectifying tower 7. A feeding pipeline 11 is arranged between a tower bottom liquid outlet of the low-pressure rectifying tower 1 and a tower bottom liquid inlet pipeline of the low-pressure rectifying tower reboiler 3, the low-pressure rectifying tower 1 is provided with a low-pressure rectifying tower product extraction pipeline 12, and the pressurized rectifying tower 7 is provided with a pressurized rectifying tower product extraction pipeline 13.
When the device is used for rectifying the trichloromethane, the technological parameters are as follows:
the feeding speed of the trichloromethane crude product is as follows; flow rate of 12t/h
The pressure of the low-pressure rectifying tower is as follows; -50KPa
The condenser temperature of the low-pressure rectifying tower is as follows; 40 deg.C
The temperature of a reboiler of the low-pressure rectifying tower is as follows; 46 deg.C
The reflux ratio of the low-pressure rectifying tower is as follows: 4.1
The pressure of the pressurized rectifying tower is as follows: 90KPa
The temperature of the reboiler of the pressurized rectifying tower is as follows: 112 deg.C
The reflux ratio of the pressurized rectifying tower is as follows: 5.5
And (3) operating results: the device runs stably, unit energy consumption reduction and elastic operation improvement are realized, the product purity reaches 99.99%, the unit steam consumption is reduced by 41%, and the energy-saving effect is obvious.
Claims (10)
1. A trichloromethane rectifying device comprises a low-pressure rectifying tower, a low-pressure rectifying tower condenser, a low-pressure rectifying tower reboiler, a low-pressure rectifying tower kettle pump, a low-pressure rectifying tower reflux groove, a low-pressure rectifying tower reflux pump, a pressurized rectifying tower reboiler, a pressurized rectifying tower reflux groove and a pressurized rectifying tower reflux pump, and is characterized in that a gas phase outlet of the low-pressure rectifying tower is connected with an inlet of the low-pressure rectifying tower condenser, an outlet of the low-pressure rectifying tower condenser is connected with an inlet of the low-pressure rectifying tower reflux groove, an outlet of the low-pressure rectifying tower reflux groove is connected with an inlet of the low-pressure rectifying tower reflux pump, an outlet of the low-pressure rectifying tower reflux pump is connected with a reflux inlet of the low-pressure rectifying tower, and a tower kettle liquid outlet of the low-pressure rectifying tower is respectively connected with an inlet of the low-pressure rectifying tower kettle pump and a tower kettle liquid inlet of the low-pressure rectifying tower reboiler, the export of low pressure rectifying column tower cauldron pump with the feed inlet of pressurized rectifying column is connected, the tower cauldron liquid export of low pressure rectifying column reboiler with the tower cauldron liquid import of low pressure rectifying column links to each other, the gaseous phase export of pressurized rectifying column with the heat medium access connection of low pressure rectifying column reboiler, the heat medium export of low pressure rectifying column reboiler with the import of pressurized rectifying column reflux groove links to each other, the export of pressurized rectifying column reflux groove with the access connection of pressurized rectifying column reflux pump, the export of pressurized rectifying column reflux pump with the backward flow access connection of pressurized rectifying column, the tower cauldron liquid export of pressurized rectifying column with the tower cauldron liquid access connection of pressurized rectifying column reboiler, the tower cauldron liquid export of pressurized rectifying column reboiler with the tower cauldron liquid access connection of pressurized rectifying column is provided with the inlet pipe between the tower cauldron liquid of low pressure rectifying column reboiler The system comprises a line, wherein the low-pressure rectifying tower is provided with a low-pressure rectifying tower product extraction pipeline, and the pressurized rectifying tower is provided with a pressurized rectifying tower product extraction pipeline.
2. The chloroform rectification apparatus according to claim 1, wherein a high-boiling-point substance branch pipe is further arranged between the tower bottom outlet of the pressurized rectification tower and the tower bottom inlet pipeline of the reboiler of the pressurized rectification tower.
3. The chloroform rectification apparatus according to claim 1, wherein the low-pressure rectification column is a packed column and the pressurized rectification column is a float valve column.
4. The method for rectifying the trichloromethane by using the device as claimed in claim 1, wherein the trichloromethane crude product is introduced into a reboiler of the low-pressure rectifying tower through a feeding pipeline, after the material is evaporated by the reboiler of the low-pressure rectifying tower, the gas phase at the top of the tower is condensed by a condenser of the low-pressure rectifying tower, the obtained condensate is refluxed into the low-pressure rectifying tower through a reflux tank of the low-pressure rectifying tower and a reflux pump of the low-pressure rectifying tower in sequence, and the discharge of the kettle of the low-pressure rectifying tower is pumped into the pressurized rectifying tower through the kettle of the low-pressure rectifying tower; and (3) introducing all the gas phase at the top of the pressurized rectifying tower into a reboiler of the low-pressure rectifying tower, condensing the gas phase at the top of the pressurized rectifying tower into a liquid phase after exchanging heat with the materials at the bottom of the low-pressure rectifying tower, refluxing the liquid phase into the pressurized rectifying tower through a reflux tank of the pressurized rectifying tower and a reflux pump of the pressurized rectifying tower in sequence, and obtaining a rectified trichloromethane product from a product extraction pipeline of the low-pressure rectifying tower and a product extraction pipeline of the pressurized rectifying tower respectively.
5. The method for rectifying trichloromethane according to claim 4, wherein the flow rate of the trichloromethane crude product is 5-15 t/h.
6. The method for rectifying trichloromethane according to claim 4, wherein the pressure of the low-pressure rectifying tower is-30 KPa to-80 KPa, and the pressure of the pressurized rectifying tower is 50KPa to 95 KPa.
7. The method for rectifying trichloromethane according to claim 4, wherein the reflux ratio of the low-pressure rectifying tower is 3.5-5.
8. The method of claim 4, wherein the condenser temperature of the low pressure distillation column is 35-45 ℃.
9. The method for rectifying trichloromethane according to claim 4, wherein the temperature of the reboiler of the pressurized rectifying tower is 105-125 ℃.
10. The method of claim 4, wherein the pressurized distillation column reflux ratio is from 4 to 6.
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| CN202011215749.XA CN112337127A (en) | 2020-11-04 | 2020-11-04 | Trichloromethane rectifying device and rectifying method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113828001A (en) * | 2021-10-29 | 2021-12-24 | 新疆晶硕新材料有限公司 | Separation system and separation method of chloromethane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113828001A (en) * | 2021-10-29 | 2021-12-24 | 新疆晶硕新材料有限公司 | Separation system and separation method of chloromethane |
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Application publication date: 20210209 |