CN111659322A - Device and process for preparing 1,1,1, 3-tetrachloropropane - Google Patents
Device and process for preparing 1,1,1, 3-tetrachloropropane Download PDFInfo
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- CN111659322A CN111659322A CN201910168007.7A CN201910168007A CN111659322A CN 111659322 A CN111659322 A CN 111659322A CN 201910168007 A CN201910168007 A CN 201910168007A CN 111659322 A CN111659322 A CN 111659322A
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- UTACNSITJSJFHA-UHFFFAOYSA-N 1,1,1,3-tetrachloropropane Chemical compound ClCCC(Cl)(Cl)Cl UTACNSITJSJFHA-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 109
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 98
- 239000005977 Ethylene Substances 0.000 claims abstract description 98
- 238000000605 extraction Methods 0.000 claims abstract description 7
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 47
- 239000003054 catalyst Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 abstract description 9
- 239000012295 chemical reaction liquid Substances 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 150000004696 coordination complex Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 229960002089 ferrous chloride Drugs 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XTTGYFREQJCEML-UHFFFAOYSA-N tributyl phosphite Chemical compound CCCCOP(OCCCC)OCCCC XTTGYFREQJCEML-UHFFFAOYSA-N 0.000 description 2
- LIPPKMMVZOHCIF-UHFFFAOYSA-N 1,1,2-trichloroprop-1-ene Chemical compound CC(Cl)=C(Cl)Cl LIPPKMMVZOHCIF-UHFFFAOYSA-N 0.000 description 1
- FDMFUZHCIRHGRG-UHFFFAOYSA-N 3,3,3-trifluoroprop-1-ene Chemical compound FC(F)(F)C=C FDMFUZHCIRHGRG-UHFFFAOYSA-N 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 229940045803 cuprous chloride Drugs 0.000 description 1
- 238000005237 degreasing agent Methods 0.000 description 1
- 239000013527 degreasing agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940032296 ferric chloride Drugs 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 150000008301 phosphite esters Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- QOPBTFMUVTXWFF-UHFFFAOYSA-N tripropyl phosphite Chemical compound CCCOP(OCCC)OCCC QOPBTFMUVTXWFF-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/26—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton
- C07C17/272—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions
- C07C17/275—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions of hydrocarbons and halogenated hydrocarbons
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a reaction device for preparing 1,1,1, 3-tetrachloropropane, which comprises a reaction kettle, wherein an ethylene circulating system is arranged outside the reaction kettle, a gas distributor is arranged at the bottom of the reaction kettle, the ethylene circulating system comprises an ethylene extraction pipe arranged at the upper part of the reaction kettle, an ethylene press-in pipe arranged at the lower part of the reaction kettle, and an ethylene compressor arranged between the ethylene extraction pipe and the press-in pipe, wherein the ethylene press-in pipe is communicated with the gas distributor; the selectivity of the main product 1,1,1, 3-tetrachloropropane is improved; the reaction kettle does not need a stirring device, and the pressure of ethylene in the reaction kettle is reduced at a similar reaction rate.
Description
Technical Field
The invention relates to the field of organic halide preparation, in particular to a device and a process for preparing 1,1,1, 3-tetrachloropropane.
Background
1,1,1, 3-tetrachloropropane is a key raw material for synthesizing trichloropropene and trifluoropropene, and can be used as a paint remover, a degreasing agent and a solvent. The synthesis method of 1,1,1, 3-tetrachloropropane mainly comprises a peroxide method (CA691213A), an electromagnetic radiation method (CA807638A), a metal complex and a cocatalyst method, wherein the peroxide method and the electromagnetic radiation method are not suitable for industrial production due to low synthesis efficiency or harsh reaction conditions, the metal complex and the cocatalyst method are suitable for industrialization due to mild reaction conditions and high synthesis efficiency, but inevitably generated colloid oil substances are adhered to the inner wall of a reaction kettle and a stirring device, and are very unfavorable for long-term continuous production.
US4605802A discloses a method for preparing 1,1,1, 3-tetrachloropropane by reacting carbon tetrachloride and ethylene, wherein the catalyst is phosphite ester and iron powder, preferably ferric chloride is additionally added, the reaction is carried out for 5.5-22.6 hours at 95 ℃ and 758kPa, the conversion rate is 45-88.5%, and the selectivity is 94.9-96.3%. The iron powder is left in the reactor after the reaction is finished and is used for the next reaction; preferably, the reactor is washed with a solvent such as dichloromethane or acetone before the next reaction.
CN106146247A discloses adding carbon tetrachloride, tributyl phosphate and ferrous chloride into a catalyst preparation tank, and stirring uniformly to obtain a uniform mixture, wherein the molar ratio of each component in the mixture is as follows: adding the prepared uniform mixture into an autoclave with stirring through a metering pump, maintaining the reaction temperature at 90 ℃, continuously introducing ethylene to maintain the reaction pressure at 1.1MPa, keeping the reaction time for 1h, continuously extracting a reaction crude product, and performing chromatographic analysis, CCl4The conversion was 80% and the selectivity to the product 1,1,1, 3-tetrachloropropane was 93%.
JP2017137263A discloses that a metal complex catalyst is dissolved in a liquid phase, ethylene and carbon tetrachloride are subjected to an addition reaction to obtain a reaction liquid containing 1,1,1, 3-tetrachloropropane, the reaction liquid is subjected to high-speed centrifugal separation to produce a phase separation, and the metal complex catalyst is in a light phase and the 1,1,1, 3-tetrachloropropane is in a heavy phase. Separation of catalystThe separation ensures that the reaction product does not generate side reaction in the distillation process, thereby ensuring the high purity of the reaction product. Reacting 0.55mol iron and 0.1mol dimethylacetamide relative to 100mol carbon tetrachloride at 130 deg.C and 0.6MPa while continuously adding dimethylacetamide for 2.5hr until the total amount is 0.636mol, and continuing reaction for 5hr, CCl4The conversion was 94% and the product selectivity 98%.
The prior art improves the conversion rate of raw materials, the selectivity of products and the operability of a device through catalyst improvement and post-treatment process change, but does not fundamentally solve the problem of generating a colloidal oily substance in the reaction.
Disclosure of Invention
Aiming at the problem that the gum oil-like substance is generated in the process of preparing 1,1,1, 3-tetrachloropropane by reacting carbon tetrachloride and ethylene in the prior art, the invention reduces the generation amount of the gum oil-like substance by improving the reaction device.
The reaction formula for preparing 1,1,1, 3-tetrachloropropane by reacting carbon tetrachloride with ethylene is as follows:
since ethylene is easily polymerized at high temperature and high pressure, in addition to the above main reaction, there are also a series of side reactions, which produce gum oil-like by-products:
in the same catalyst, excessive ethylene or higher ethylene concentration is the main cause of side reaction, and the reduction of ethylene concentration or ethylene pressure in the reaction system is the key to reduce the side reaction.
The invention provides a device for preparing 1,1,1, 3-tetrachloropropane by reacting carbon tetrachloride and ethylene, which comprises a reaction kettle, wherein an ethylene circulating system is arranged outside the reaction kettle, a gas distributor is arranged at the bottom in the reaction kettle, the ethylene circulating system comprises an ethylene extracting pipe arranged at the upper part of the reaction kettle, an ethylene pressing pipe arranged at the lower part of the reaction kettle, and an ethylene compressor arranged between the ethylene extracting pipe and the pressing pipe, and the ethylene pressing pipe is communicated with the gas distributor; the reaction kettle is also provided with carbon tetrachloride, a catalyst feeding port and a reaction liquid discharging port; and an ethylene feed inlet is arranged on the ethylene extraction pipe.
Preferably, the length-diameter ratio of the reaction kettle is 1.5-60, and further preferably 2-15; the too little fat type reation kettle of slenderness ratio, gas-liquid phase contact time is short, is unfavorable for the gas-liquid reaction, otherwise, too big slenderness ratio, and the bubble takes place the gathering at long distance rising in-process, makes the gas-liquid area of contact reduce, has reduced reaction efficiency.
Preferably, the gas distributor is made of sintered metal porous materials, and further preferably, the gas distributor is a sintered metal porous screen plate, the area of the screen plate is 30-90% of the cross section area of the reaction kettle, so that the uniform distribution of gas is ensured, and reaction liquid can be sufficiently circulated in the reaction kettle;
the reaction kettle can fully stir the liquid phase through the ethylene bubbling from the gas distributor without an additional stirring device, can avoid the safety risk caused by the high-speed dynamic friction of the stirring device, can also avoid the collision of the metal catalyst and the reaction kettle wall caused by stirring, and greatly reduces the manufacturing cost of the reaction kettle.
Preferably, the ethylene compressor is an oil-free compressor, so as to prevent lubricating oil from causing adverse effects on the reaction; the pressure difference between the exhaust port and the air suction port of the ethylene compressor is 0.1-3.0 MPa, and the exhaust volume is 0.4-18 Nm/cubic meter of the volume of the reaction kettle3Min; the ethylene compressor can circulate the ethylene in the reaction kettle only by providing pressure for overcoming the liquid level difference in the reaction kettle, and the required power is very small; the discharge capacity of the ethylene compressor is the expression of the ethylene circulation capacity, too small a discharge capacity cannot provide enough ethylene to contact and react with the liquid phase, and too large a discharge capacity causes excessive boiling of the liquid phase, so that the reaction system is unstable.
The external ethylene circulating system ensures that ethylene is fully exchanged between a gas phase and a liquid phase, and even if the ethylene pressure in the reaction kettle is lower, the ethylene amount dissolved into the reaction liquid or contacted with the reaction liquid can be ensured, thereby ensuring the smooth reaction of carbon tetrachloride and ethylene.
The process for preparing 1,1,1, 3-tetrachloropropane by using the reaction device for preparing 1,1,1, 3-tetrachloropropane comprises the following steps: firstly discharging air from a reaction kettle, then adding a catalyst and carbon tetrachloride, introducing ethylene, starting an ethylene compressor, pumping the ethylene out of the upper part of the reaction kettle, pressurizing the ethylene by the ethylene compressor, pressing the ethylene into the reaction kettle from the lower part of the reaction kettle, distributing the ethylene pressed into the reaction kettle by a gas distributor, then introducing the ethylene into a reaction system, controlling the ethylene pressure in the reaction kettle to be 0.15-0.50 MPa, heating to 80-130 ℃ for reaction, and stopping the reaction when the conversion rate of the carbon tetrachloride in a reaction solution is 60-85%.
The catalyst is conventional carbon tetrachloride and ethylene telomerization catalyst. The catalyst can be selected from ferric chloride, ferrous chloride, cuprous chloride, etc., and the cocatalyst can be selected from tripropyl phosphite, tributyl phosphite, etc.
Compared with the prior art, the invention has the following advantages: 1. the generation amount of the gum oil-shaped by-products in the process of preparing the 1,1,1, 3-tetrachloropropane by reacting carbon tetrachloride and ethylene is reduced; 2. the selectivity of the main product 1,1,1, 3-tetrachloropropane is improved; 3. the reaction kettle does not need a stirring device; 4. the pressure of ethylene in the reactor was reduced at similar reaction rates.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing 1,1,1, 3-tetrachloropropane according to the present invention.
In figure 1,1 is a reaction kettle, 2 is carbon tetrachloride and a catalyst charging port, 3 is an ethylene extraction pipe, 4 is an ethylene charging port, 5 is an ethylene compressor, 6 is an ethylene pressing pipe, 7 is a discharging port, and 8 is a gas distributor
Detailed Description
As shown in figure 1, the device for preparing 1,1,1, 3-tetrachloropropane comprises a reaction kettle, wherein an ethylene circulating system is arranged outside the reaction kettle, and a gas distributor is arranged at the bottom of the reaction kettle; the ethylene circulating system comprises an ethylene extraction pipe 3 arranged at the upper part of the reaction kettle 1, an ethylene press-in pipe 6 arranged at the lower part of the reaction kettle 1, and an ethylene compressor 5 arranged between the ethylene extraction pipe 3 and the press-in pipe 6, wherein the ethylene press-in pipe is communicated with a gas distributor 8; the upper part of the reaction kettle is provided with a carbon tetrachloride and catalyst feed inlet 2, the lower part of the reaction kettle is provided with a reaction liquid discharge port 7, and an ethylene draw-out pipe is provided with an ethylene feed inlet 4; the reactor is made of stainless steel, the gas distributor is a multi-layer sintered metal mesh plate, the average pore diameter is 0.3-50 mu m, the porosity is 25% -45%, the area of the gas distributor is 30% -90% of the cross section area of the reactor, the ethylene compressor is an oil-free ethylene compressor, and the pressure difference between an exhaust port and an air inlet is 0.1-3.0 MPa.
The present invention will be further illustrated by using the reaction apparatus described below in conjunction with examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1
A 5000L reaction kettle made of stainless steel has a length-diameter ratio of 3, discharges air, adds 5kg of catalyst ferric chloride, 32kg of reduced iron powder, 25kg of cocatalyst tributyl phosphite and 3750kg of carbon tetrachloride, and leads ethylene to enter from an ethylene charging port, so that the ethylene pressure in the reaction kettle reaches 0.20 MPa; starting the oil-free ethylene compressor, the pressure difference between the exhaust port and the air inlet is less than or equal to 1.2MPa, and the exhaust volume of the ethylene compressor is 17.5Nm3The ethylene is pumped out from the upper part of the reaction kettle, is pressurized by an ethylene compressor, is pressed into the reaction kettle from the lower part of the reaction kettle, and is distributed into a reaction system by a gas distributor, wherein the gas distributor is a multi-layer sintered metal mesh plate, the average pore diameter is 0.45 mu m, the porosity is 38 percent, and the area of the gas distributor is 65 percent of the cross-sectional area of the reaction kettle; heating to 95 ℃ for reaction, supplementing ethylene, controlling the pressure of the ethylene in the reaction kettle to be 0.18-0.22 MPa, reacting for 7.5 hours, sampling for gas chromatographic analysis, wherein the conversion rate of 1,1,1, 3-tetrachloropropane is 73.4 percent, the selectivity of 1,1,1, 3-tetrachloropropane is 99.5 percent, and the reaction is stopped, and the secondary addition by-product is 0.4 percent, 1,1, 3-tetrachloropropane is 76.2 percent, carbon tetrachloride is 23.4 percent, and the secondary addition by-product is 0.4 percent.
Example 2
The ethylene pressure in the reaction kettle is controlled to be 0.46-0.50 MPa, other steps are the same as those in example 1, and gas chromatography analysis is performed on a sample, wherein 85.4% of 1,1,1, 3-tetrachloropropane, 13.9% of carbon tetrachloride, 0.7% of secondary addition by-products, 84.0% of conversion rate of reduced carbon tetrachloride and 99.3% of selectivity of 1,1,1, 3-tetrachloropropane are obtained.
Comparative example 1
The reaction kettle is not provided with an ethylene circulating system, reaction liquid is stirred by a mechanical stirring device, the ethylene pressure in the reaction kettle is controlled to be 0.78-0.82 MPa, the reaction time is 11 hours, other steps are the same as those in the embodiment 1, samples are taken for gas chromatography, and 75.9% of 1,1,1, 3-tetrachloropropane, 21.2% of carbon tetrachloride, 2.4% of secondary addition byproducts and other 0.5% are obtained, the conversion rate of the tetrachloro carbon is 79.0%, and the selectivity of the 1,1,1, 3-tetrachloropropane is 96.3%.
Claims (9)
1. The device for preparing the 1,1,1, 3-tetrachloropropane comprises a reaction kettle and is characterized in that an ethylene circulating system is arranged outside the reaction kettle, a gas distributor is arranged at the bottom in the reaction kettle, the ethylene circulating system comprises an ethylene extracting pipe arranged at the upper part of the reaction kettle, an ethylene pressing pipe arranged at the lower part of the reaction kettle, and an ethylene compressor arranged between the ethylene extracting pipe and the ethylene pressing pipe, and the ethylene pressing pipe is communicated with the gas distributor.
2. The apparatus for preparing 1,1,1, 3-tetrachloropropane according to claim 1, wherein the length-diameter ratio of the reaction kettle is 1.5-60.
3. The apparatus for preparing 1,1,1, 3-tetrachloropropane according to claim 2, wherein the length-diameter ratio of the reaction kettle is 2-15.
4. The apparatus for preparing 1,1,1, 3-tetrachloropropane according to claim 1, wherein the gas distributor is made of sintered metal porous material.
5. The apparatus for preparing 1,1,1, 3-tetrachloropropane according to claim 1, wherein the gas distributor is a sintered metal porous mesh plate, and the area of the mesh plate is 30-90% of the internal cross-sectional area of the reaction vessel.
6. The apparatus for preparing 1,1,1, 3-tetrachloropropane according to claim 1, wherein the ethylene compressor is an oil-free compressor.
7. The apparatus for preparing 1,1,1, 3-tetrachloropropane according to claim 1 or 6, wherein the pressure difference between the exhaust port and the suction port of the ethylene compressor is 0.1-3.0 MPa, and the exhaust amount is 0.4-18 Nm/m of the volume of the reaction kettle3/min。
8. A process for preparing 1,1,1, 3-tetrachloropropane, comprising: the device for preparing 1,1,1, 3-tetrachloropropane according to any one of claims 1 to 7 is adopted, firstly, the reaction kettle is discharged with air, then catalyst and carbon tetrachloride are added, after ethylene is introduced, an ethylene compressor is started, ethylene is pumped out from an ethylene extraction pipe at the upper part of the reaction kettle, after being pressurized by the ethylene compressor, ethylene is pressed into the reaction kettle from an ethylene pressing pipe at the lower part of the reaction kettle, and the ethylene pressed into the reaction kettle is distributed by a gas distributor and then enters a reaction system; and stopping the reaction when the conversion rate of carbon tetrachloride in the reaction system is 60-85%.
9. The process of claim 8, wherein the gas phase pressure at the upper part of the reaction kettle is 0.15-0.50 MPa, and the reaction temperature is 80-130 ℃.
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| CN114835554A (en) * | 2021-02-02 | 2022-08-02 | 中国科学院宁波材料技术与工程研究所 | Preparation method of 1,1,1, 3-tetrachloropropane |
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