CN117886665A - Full-flow continuous process for synthesizing 1, 3-pentafluoropropane - Google Patents
Full-flow continuous process for synthesizing 1, 3-pentafluoropropane Download PDFInfo
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- CN117886665A CN117886665A CN202311695921.XA CN202311695921A CN117886665A CN 117886665 A CN117886665 A CN 117886665A CN 202311695921 A CN202311695921 A CN 202311695921A CN 117886665 A CN117886665 A CN 117886665A
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- 238000010924 continuous production Methods 0.000 title claims abstract description 30
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 150
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 117
- 239000000463 material Substances 0.000 claims abstract description 109
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 74
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 59
- 239000003054 catalyst Substances 0.000 claims abstract description 44
- 239000000047 product Substances 0.000 claims abstract description 42
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 37
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000460 chlorine Substances 0.000 claims abstract description 32
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 32
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000005086 pumping Methods 0.000 claims abstract description 11
- MSSNHSVIGIHOJA-UHFFFAOYSA-N pentafluoropropane Chemical compound FC(F)CC(F)(F)F MSSNHSVIGIHOJA-UHFFFAOYSA-N 0.000 claims description 35
- 238000000926 separation method Methods 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 22
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 claims description 11
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- -1 alkyl phosphate Chemical compound 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims description 5
- 229960002089 ferrous chloride Drugs 0.000 claims description 5
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 5
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 3
- 229940045803 cuprous chloride Drugs 0.000 claims description 3
- 229960003284 iron Drugs 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000003426 co-catalyst Substances 0.000 claims 1
- 230000003797 telogen phase Effects 0.000 claims 1
- 238000004334 fluoridation Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 6
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- 125000004122 cyclic group Chemical group 0.000 description 5
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- ATADHKWKHYVBTJ-UHFFFAOYSA-N hydron;4-[1-hydroxy-2-(methylamino)ethyl]benzene-1,2-diol;chloride Chemical compound Cl.CNCC(O)C1=CC=C(O)C(O)=C1 ATADHKWKHYVBTJ-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000003507 refrigerant Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000001273 butane Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- PGJHURKAWUJHLJ-UHFFFAOYSA-N 1,1,2,3-tetrafluoroprop-1-ene Chemical compound FCC(F)=C(F)F PGJHURKAWUJHLJ-UHFFFAOYSA-N 0.000 description 1
- LDTMPQQAWUMPKS-UHFFFAOYSA-N 1-chloro-3,3,3-trifluoroprop-1-ene Chemical compound FC(F)(F)C=CCl LDTMPQQAWUMPKS-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Classifications
-
- 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
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- 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
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/20—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms
- C07C17/202—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms two or more compounds being involved in the reaction
- C07C17/204—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms two or more compounds being involved in the reaction the other compound being a halogen
-
- 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
- C07C17/278—Preparation of halogenated hydrocarbons by reactions involving an increase in the number of carbon atoms in the skeleton by addition reactions of only halogenated hydrocarbons
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application discloses a full-flow continuous process for synthesizing 1, 3-pentafluoropropane, which comprises telomerization: adding vinyl chloride, carbon tetrachloride, a catalyst I and a cocatalyst into a pre-kettle mixer for premixing to obtain a mixture I, pumping the mixture I into a reactor system for telomerization to obtain a telomerization material, continuously pumping out and separating the telomerization material to obtain R240fa, and returning the separated vinyl chloride, carbon tetrachloride, the catalyst I, the cocatalyst and the non-separated R240fa to the pre-kettle mixer for continuous reaction; fluorination reaction: continuously introducing R240fa, chlorine and anhydrous hydrogen fluoride obtained by telomerization into a fluorination reaction kettle containing an activated catalyst II for carrying out fluorination reaction to obtain a fluorination reaction product, separating the fluoridation reaction product to obtain 1, 3-pentafluoropropane, and returning the residual product after the 1, 3-pentafluoropropane is separated to a fluorination reaction kettle for continuous reaction.
Description
Technical Field
The application relates to the technical field of 1, 3-pentafluoropropane, in particular to a full-flow continuous process for synthesizing 1, 3-pentafluoropropane.
Background
At present, the current time of the process, the industrial production of 1, 3-pentafluoropropane mainly uses 1, 3-pentachloro propane (R240 fa) is used as a raw material and undergoes two main types of liquid-phase fluorination method or gas-phase fluorination method, for example, patent CN101913983B discloses a method for preparing R245fa by liquid phase fluorination, and patent CN103214342B discloses a method for synthesizing R245fa by two-step gas phase fluorination under the action of a chromium-based catalyst.
With the continuous technical improvement of various production enterprises, the preparation process of the R245fa is mature, but other first-generation, second-generation and third-generation refrigerant impurities including R11, R12, R13, R114, R115, R113, 244fa and the like still exist in unavoidable products. The generation of the impurities mainly originates from the fluorination reaction of the substance R240fa, and some impurities originate from the raw material R240fa, such as the impurity hexachloroethane, are generated in the production process of R240fa, but the impurities are difficult to separate by conventional rectification due to the close boiling point of the impurities and inevitably affect the quality of the product. Although the content of the impurities is mostly kept between tens and hundreds of ppm, with the continuous implementation of related international agreements, the product quality of R245fa has higher standards, the content requirements of related impurities are more and more severe, the current partial-use products have zero detection requirements on the impurities of the first-generation refrigerants, and the future requirements on the impurity contents of the second-generation and third-generation refrigerants in the products can be expected to be improved. In view of the above problems, there are still many efforts to be considered and studied to optimize and perfect the production process of high quality R245 fa.
Disclosure of Invention
The full-flow continuous process for synthesizing the 1, 3-pentafluoropropane has the advantages of high reaction yield, high product quality, good production safety, less pollution emission and capability of realizing full-flow continuous production and automatic control.
The technical scheme adopted for solving the technical problems is as follows: provides a full-flow continuous process for synthesizing 1, 3-pentafluoropropane, the synthetic route is as follows,
the synthesis process specifically comprises the following steps:
telomerization: vinyl chloride, carbon tetrachloride, a catalyst I and a cocatalyst are mixed according to the molar ratio: 1:0.8-3: adding 0.01-0.1:0.01-0.2 into a pre-kettle mixer for premixing to obtain a mixture I, pumping the mixture I into a reactor system at 600-2000kg/h, carrying out telomerization at the reaction pressure of 0.3-1.0MPa and the reaction temperature of 60-150 ℃ to obtain telomerization materials, continuously pumping out and separating the telomerization materials to obtain R240fa, and returning separated vinyl chloride, carbon tetrachloride, catalyst I, cocatalyst and non-separated R240fa to the pre-kettle mixer for continuous reaction when separating the R240fa;
fluorination reaction: the liquid phase fluorination method is adopted, and the molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by the telomerization reaction is as follows: 1:0.0001-0.0005:5-6 continuously feeding a fluorination reaction vessel containing a catalyst II activated according to a known technique, wherein the molar ratio of the feed amount of R240fa per hour to the amounts of hydrogen fluoride in the catalyst II and the fluorination reaction vessel is 1:0.1-5:10-100, carrying out fluorination reaction at the reaction pressure of 0.4-1.0MPa and the reaction temperature of 60-150 ℃ to obtain a fluorination reaction product, separating the fluorination reaction product to obtain 1, 3-pentafluoropropane, when separating 1, 3-pentafluoropropane, and (3) returning the residual product after the 1, 3-pentafluoropropane is separated from the fluorination reaction product to a fluorination reaction kettle for continuous reaction.
In the full-flow continuous process for synthesizing the 1, 3-pentafluoropropane, hydrogen fluoride is used for activating a catalyst, and simultaneously, the hydrogen fluoride also serves as a fluorination reagent and a solvent to play a role in dissolving the fluorination catalyst, so that certain requirements are met on the feeding amount of R240fa in unit time in a fluorination reaction kettle and the ratio of the fluorination catalyst to the hydrogen fluoride in the kettle, the ratio is too large, the production capacity is limited, the ratio is too small, the catalyst cannot be fully dissolved, and the reaction efficiency is also influenced. Thus, the molar ratio of the feed amount of R240fa per hour to the amount of hydrogen fluoride in the catalyst II and fluorination reaction vessel in the present invention is 1:0.1-5:10-100;
the main function of the chlorine is to maintain the catalytic activity of the fluorination catalyst, but because the one-step continuous liquid phase fluorination method adopted by the invention produces a small amount of olefin intermediates including trifluorochloropropene, tetrafluoropropene and the like in the process, if the content of the chlorine is too high, side reaction impurities can be generated with the olefins, and the content is too low, the activity of the catalyst cannot be maintained, so that the continuous feeding chlorine feeding amount needs to be strictly controlled in order to ensure that the fluorination reaction obtains high-quality fluorinated products, and the molar ratio of R240fa, the chlorine and anhydrous hydrogen fluoride in the invention is as follows: 1:0.0001-0.0005:5-6 continuously introducing the catalyst II into a fluorination reaction kettle containing the activated catalyst II.
The boiling point of the chlorine is-34 ℃, the boiling point of the chlorine is close to that of an olefin intermediate product, the consumption of the chlorine is small, the separation difficulty by a rectification technology is high, the accumulation of the chlorine content in a circulating light component material can be increased, and the product quality is reduced; or to ensure complete separation of chlorine, resulting in limited separation capacity of the fluorination continuous separation system, affecting the throughput of the overall continuous process. In view of the above, the invention is provided with the continuous water washing and alkali washing tower for removing chlorine before the light components are returned to the reaction system, thereby realizing an efficient continuous separation process.
Preferably, in telomerization, the reactor system is CSTR, the material of telomerization is pumped into a light component tower of the 240 continuous separation system by adopting the 240 continuous separation system to separate vinyl chloride and carbon tetrachloride when separating R240fa, the separated vinyl chloride and carbon tetrachloride return to a pre-kettle mixer to continue reaction, the tower bottom material of the light component tower enters a 240 tower of the 240 continuous separation system to carry out rectification separation, R240fa is separated from the top of the 240 tower, and the vinyl chloride, carbon tetrachloride, catalyst I, cocatalyst and non-separated R240fa at the bottom of the 240 tower return to the pre-kettle mixer to continue reaction.
Preferably, in telomerization, the 240 continuous separation system further comprises a heavy component tower, the heavy component tower is connected with the 240 tower, R240fa is separated from the top of the heavy component tower, and the heavy component tower is used for separating butane high-boiling substances possibly accumulated in long-time continuous reaction and deactivated catalyst and cocatalyst.
Preferably, in the fluorination reaction, when 1, 3-pentafluoropropane is separated, introducing a fluorination reaction product into a hydrogen chloride tower, separating hydrogen chloride from the tower top of the hydrogen chloride tower, introducing tower bottom materials of the hydrogen chloride tower into the hydrogen fluoride tower, separating light components containing R245fa from the tower top of the hydrogen fluoride tower, sequentially entering a water washing tower and an alkaline washing tower, returning the tower bottom materials of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, after hydrogen fluoride and chlorine in the light group containing R245fa are removed by an alkaline washing tower, introducing the product into a dehydrogenation tower, separating out the light component containing R1234ze from the top of the dehydrogenation tower, returning the light component to a fluorination reaction kettle for continuous reaction, introducing tower kettle materials of the dehydrogenation tower into a 245 tower for rectification, introducing the top product of the 245 tower into a drying tower, drying the product by the drying tower to obtain 1, 3-pentafluoropropane, and returning the tower kettle materials of the 245 tower to the fluorination reaction kettle for continuous reaction.
Preferably, the CSTR comprises three serially connected telomerization kettles, the capacity of the telomerization kettle is 2000-5000L, the material of the telomerization kettle has no special requirement, and the CSTR is made of common steel lining enamel material.
Preferably, the first catalyst is at least one of iron, zinc, ferrous chloride or cuprous chloride.
Preferably, the cocatalyst is an alkyl phosphate or an alkyl phosphite.
Preferably, the reaction temperature of telomerization is 80-140 ℃ and the reaction pressure is 0.4-0.8MPa.
Preferably, the reaction temperature of the fluorination reaction is 80-120 ℃ and the reaction pressure is 0.5-0.8MPa.
Preferably, the second catalyst is one of antimony trichloride, antimony pentachloride, tin tetrachloride or titanium tetrachloride.
The essential effects of the application are:
1. the full-flow continuous process for synthesizing the 1, 3-pentafluoropropane realizes synchronous and efficient mass and heat transfer in radial and circumferential directions through a CSTR technology, has more excellent mass and heat transfer effect compared with the traditional synthesis technology, and has the advantages of short residence time of reaction materials in a reaction stage, few reaction byproducts, simple product separation, high product quality and good product yield due to the CSTR technology;
2. compared with the traditional kettle type production, the full-flow continuous process for synthesizing the 1, 3-pentafluoropropane realizes mass transfer and heat transfer by stirring materials in a reaction kettle, reaction heat generated in the moment of contact of vinyl chloride and carbon tetrachloride is difficult to effectively remove, the situation that local materials in the kettle are overheated far beyond the process temperature occurs, and excessive reaction temperature can lead to the reaction to generate a larger amount of byproducts and more types, so that more complex equipment and more severe separation conditions are required for obtaining high-purity products. The CSTR technology adopts the design of continuous multistage serial stirring kettles, and synchronously realizes radial heat and material transfer in a material transmission pipeline besides circumferential mass and heat transfer of materials in the reaction kettle. Meanwhile, the continuous multistage kettles are arranged under the same production capacity, smaller reaction kettles can be selected, the influence of amplification effect is reduced, purer reaction products are obtained, and the subsequent separation difficulty is reduced;
3. the full-flow continuous process for synthesizing the 1, 3-pentafluoropropane realizes the full-flow continuous production process of feeding, reacting and separating products from raw materials, the full flow can realize automatic control, the production cost is greatly reduced, the productivity is greatly improved, the reaction process is safe and reliable, the pollution emission is less, and the method is environment-friendly.
Drawings
FIG. 1 is a schematic illustration of the process flow of the full-flow continuous process for synthesizing 1, 3-pentafluoropropane herein.
Detailed Description
As shown in fig. 1, the full-flow continuous process for synthesizing 1, 3-pentafluoropropane according to the present application comprises:
telomerization: vinyl chloride, carbon tetrachloride, a catalyst I and a cocatalyst are mixed according to the molar ratio: 1:0.8-3:0.01-0.1:0.01-0.2 is added into a pre-kettle mixer for premixing to obtain a mixture I, the catalyst I is at least one of iron, zinc, ferrous chloride or cuprous chloride, the catalyst I is alkyl phosphate or alkyl phosphite, the catalyst promoter is 600-2000kg/h of the mixture I is pumped into three serially connected telomerization kettles with the capacity of 2000-5000L, the telomerization is carried out at the reaction pressure of 0.3-1.0MPa and the reaction temperature of 60-150 ℃ to obtain a telomerization material, the telomerization material is pumped and separated continuously to obtain R240fa, the telomerization material is pumped into a light component tower of a 240 continuous separation system by a 240 continuous separation system to separate vinyl chloride and carbon tetrachloride when the R240fa is separated, the separated vinyl chloride and carbon tetrachloride return to the mixer in front of the kettle to continue the reaction, the tower bottom material of the light component tower enters a 240 tower of a 240 continuous separation system to carry out rectification separation, R240fa is separated from the tower top of the 240 tower, the vinyl chloride, the carbon tetrachloride, the catalyst I, the cocatalyst and the unseparated R240fa at the tower bottom of the 240 tower return to the mixer in front of the kettle to continue the reaction, the 240 continuous separation system also comprises a heavy component tower, and the heavy component tower is connected with the 240 tower to be used for separating butane high-boiling matters which are possibly accumulated in long-time continuous reaction and deactivated catalyst and cocatalyst, and R240fa is separated from the tower top of the heavy component tower;
fluorination reaction: the liquid phase fluorination method is adopted, and the molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by the telomerization reaction is as follows: 1:0.0001-0.0005:5-6 continuously introducing into a fluorination reaction kettle containing an activated catalyst II, wherein the catalyst II is one of antimony trichloride, antimony pentachloride, tin tetrachloride or titanium tetrachloride, and the molar ratio of the feeding amount of R240fa per hour to the hydrogen fluoride in the catalyst II and the fluorination reaction kettle is 1:0.1-5:10-100, carrying out fluorination reaction at the reaction pressure of 0.4-1.0MPa and the reaction temperature of 60-150 ℃ to obtain a fluorination reaction product, separating the fluorination reaction product to obtain 1, 3-pentafluoropropane, introducing the fluorination reaction product into a hydrogen chloride tower when separating the 1, 3-pentafluoropropane, hydrogen chloride is separated from the top of the hydrogen chloride tower, tower kettle materials of the hydrogen chloride tower are introduced into the hydrogen fluoride tower, light components containing R245fa are separated from the top of the hydrogen fluoride tower and sequentially enter a water washing tower and an alkaline washing tower, returning tower bottom materials of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, removing hydrogen fluoride and chlorine in light components containing R245fa by an alkaline washing tower, introducing the products into a dehydrogenation tower, separating light components containing R1234ze from the tower top of the dehydrogenation tower, returning the light components to the fluorination reaction kettle for continuous reaction, introducing tower bottom materials of the dehydrogenation tower to a 245 tower for rectification, introducing tower top products of the 245 tower to a drying tower, drying the products by the drying tower to obtain 1, 3-pentafluoropropane, and returning the tower bottom materials of the 245 tower to the fluorination reaction kettle for continuous reaction.
The technical scheme of the present application is further specifically described below through specific embodiments.
Example 1
A full-flow continuous process for synthesizing 1, 3-pentafluoropropane, comprising:
telomerization: carbon tetrachloride, chloroethylene, iron powder and tributyl phosphate in the mass ratio of 300:50:1:6, after premixing in a mixer in front of the kettle, pumping the mixture into a CSTR reaction system, wherein the total feeding flow is 1800kg/h, the size of a telomerization reaction kettle adopts 5000L specification, the reaction temperature is 90-100 ℃, and the reaction pressure is 0.6+/-0.1 MPa. After the materials are reacted by a CSTR reaction system, the materials are continuously pumped out to a 240 continuous separation system, light components such as chloroethylene, carbon tetrachloride and the like are separated by a light component tower and returned to a pre-kettle mixer for continuous reaction, tower kettle materials are distilled and separated by a 240 tower, R240fa at the top of the tower is used for fluoridation, and the tower kettle heavy components comprise a small amount of mixture of unseparated R240fa, iron powder and tributyl phosphate which is pumped back to the pre-kettle mixer for cyclic reaction. After the material is fed for about 12 hours, the flow rates of the circulating material, the R240fa extracted material and the like are stable, at the moment, the flow rate of the R240fa in the fluorination reaction is about 860kg/h, the feeding material is adjusted to 620kg/h of carbon tetrachloride and 250kg/h of vinyl chloride, and the dynamic balance of the materials in the whole system is kept;
fluorination reaction: 1000kg of antimony trichloride as a catalyst is put into a fluorination reaction kettle, 5000kg of anhydrous hydrogen fluoride is pumped, after the antimony trichloride is preactivated, the temperature is kept at 80-90 ℃ and the discharge of telomerization reaction is waited for carrying out the fluorination reaction. The molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by telomerization reaction is as follows: 1:0.0001-0.0005:5-6 are introduced into a fluorination reaction kettle, after the telomerization reaction is carried out, the feeding flow of each material is R240fa860kg/h, chlorine gas is 0.1kg/h, anhydrous hydrogen fluoride is 470kg/h, and the reaction pressure of the fluorination reaction kettle is controlled to be 0.6+/-0.1 MPa. And (3) extracting a fluorination reaction product from the top of the reaction kettle, separating hydrogen chloride through the top of the hydrogen chloride tower, and removing the hydrogen fluoride tower from the materials in the tower kettle. Returning the materials at the bottom of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, separating the light components containing R245fa at the top of the tower, removing hydrogen fluoride and chlorine in the light components by washing the water washing tower and the alkaline washing tower, removing the light components, separating a small amount of R1234ze and other light components, returning the light components to the fluorination reaction kettle for continuous reaction, removing the materials at the bottom of the light components tower to the 245 tower for rectification, drying to obtain high-quality R245fa, and returning the materials at the bottom of the 245 tower to the fluorination reaction kettle for continuous reaction. After R240fa is stably fed for about 10 hours, the R245fa finished product is discharged, the flow rate of circulating materials is stable, and the discharge flow rate of the finished product R245fa is about 525kg/h.
Summary of data: this example takes about 22 hours from start of telomerization to steady discharge of the fluorination station. Starting timing after the whole flow is stabilized, and stably operating for 300 hours, and summarizing the results as follows: 75t of chloroethylene, 186t of carbon tetrachloride, 30kg of chlorine and 141t of anhydrous hydrogen fluoride are consumed together to obtain 157.5t of R245fa finished product, the yield is 97.9%, and the purity is more than or equal to 99.9%.
Example 2
A full-flow continuous process for synthesizing 1, 3-pentafluoropropane, comprising:
telomerization: carbon tetrachloride, chloroethylene, iron powder and tributyl phosphate in the mass ratio of 300:50:1:6, after premixing in a mixer in front of the kettle, pumping the mixture into a CSTR reaction system, wherein the total feeding flow is 1800kg/h, the size of a telomerization reaction kettle adopts 5000L specification, the reaction temperature is 80-90 ℃, and the reaction pressure is 0.5+/-0.1 MPa. After the materials are reacted by a CSTR reaction system, the materials are continuously pumped out to a 240 continuous separation system, light components such as chloroethylene, carbon tetrachloride and the like are separated by a light component tower and returned to a mixer in front of a kettle for continuous reaction, the materials in the kettle are distilled and separated by a 240 tower, R240fa at the top of the tower is defluorinated, and the heavy components in the kettle comprise a small amount of mixture of unseparated R240fa, iron powder and tributyl phosphate which is pumped back to the mixer in front of the kettle for cyclic reaction. After the material is fed for about 12 hours, the flow rates of the circulating material, the R240fa extracted material and the like are stable, at the moment, the flow rate of the R240fa in the fluorination reaction is about 830kg/h, the feeding material is regulated to be carbon tetrachloride 600kg/h and vinyl chloride 240kg/h, and the dynamic balance of the whole system material is kept.
Fluorination reaction: 1000kg of antimony pentachloride as a catalyst is put into a fluorination reaction kettle, 5000kg of anhydrous hydrogen fluoride is pumped, after the antimony pentachloride is preactivated, the temperature is kept at 90-100 ℃ and the discharge of telomerization reaction is waited for carrying out the fluorination reaction. The molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by telomerization reaction is as follows: 1:0.0001-0.0005:5-6 are introduced into a fluorination reaction kettle, after the telomerization reaction is carried out and stable discharging is carried out, the feeding flow of each material is R240fa830kg/h, chlorine gas 0.1kg/h and anhydrous hydrogen fluoride 425kg/h, and the reaction pressure of the fluorination reaction kettle is controlled to be 0.6+/-0.1 MPa. And (3) extracting a fluorination reaction product from the top of the reaction kettle, separating hydrogen chloride through the top of the hydrogen chloride tower, and removing the hydrogen fluoride tower from the materials in the tower kettle. Returning the materials at the bottom of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, separating the light components containing R245fa at the top of the tower, removing hydrogen fluoride and chlorine in the light components by washing the water washing tower and the alkaline washing tower, removing the light components, separating a small amount of R1234ze and other light components, returning the light components to the fluorination reaction kettle for continuous reaction, removing the materials at the bottom of the light components tower to the 245 tower for rectification, drying to obtain high-quality R245fa, and returning the materials at the bottom of the 245 tower to the fluorination reaction kettle for continuous reaction. After R240fa is stably fed for about 10 hours, the R245fa finished product is discharged, the flow rate of circulating materials is stable, and the discharge flow rate of the finished product R245fa is about 505kg/h.
Summary of data: this example takes about 22 hours from start of telomerization to steady discharge of the fluorination station. Starting timing after the whole flow is stabilized, and stably operating for 300 hours, and summarizing the results as follows: the total consumption of 72t of chloroethylene, 180t of carbon tetrachloride, 30kg of chlorine and 127.5t of anhydrous hydrogen fluoride, and the yield of the R245fa finished product is 151.5t, and the purity is more than or equal to 99.9 percent.
Example 3
A full-flow continuous process for synthesizing 1, 3-pentafluoropropane, comprising:
telomerization: carbon tetrachloride, chloroethylene, iron powder and tributyl phosphate in the mass ratio of 300:50:1:6, after premixing in a mixer in front of the kettle, pumping the mixture into a CSTR reaction system, wherein the total feeding flow is 1000kg/h, the size of a telomerization reaction kettle adopts 3000L specification, the reaction temperature is 90-100 ℃, and the reaction pressure is 0.6+/-0.1 MPa. After the materials are reacted by a CSTR reaction system, the materials are continuously pumped out to a 240 continuous separation system, light components such as chloroethylene, carbon tetrachloride and the like are separated by a light component tower and returned to a mixer in front of a kettle for continuous reaction, the materials in the kettle are distilled and separated by a 240 tower, R240fa at the top of the tower is defluorinated, and the heavy components in the kettle comprise a small amount of mixture of unseparated R240fa, iron powder and tributyl phosphate which is pumped back to the mixer in front of the kettle for cyclic reaction. After the material is fed for about 12 hours, the flow rates of the circulating material, the R240fa extracted material and the like are stable, at the moment, the flow rate of the R240fa in the fluorination reaction is about 450kg/h, the feeding material is adjusted to be carbon tetrachloride 323kg/h and vinyl chloride is adjusted to be 130kg/h, and the dynamic balance of the materials in the whole system is kept.
Fluorination reaction: 800kg of antimony pentachloride as a catalyst is put into a fluorination reaction kettle, 4000kg of anhydrous hydrogen fluoride is pumped into the reaction kettle, after the antimony pentachloride is preactivated, the temperature is kept at 90-100 ℃, and the reaction kettle waits for telomerization reaction discharge to carry out fluorination reaction. The molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by telomerization reaction is as follows: 1:0.0001-0.0005:5-6 are introduced into a fluorination reaction kettle, after the telomerization reaction is carried out and stable discharging is carried out, the feeding flow of each material is R240fa450kg/h, chlorine gas is 0.05kg/h, anhydrous hydrogen fluoride is 230kg/h, and the reaction pressure of the fluorination reaction kettle is controlled to be 0.6+/-0.1 MPa. And (3) extracting a fluorination reaction product from the top of the reaction kettle, separating hydrogen chloride through the top of the hydrogen chloride tower, and removing the hydrogen fluoride tower from the materials in the tower kettle. Returning the materials at the bottom of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, separating the light components containing R245fa at the top of the tower, removing hydrogen fluoride and chlorine in the light components by washing the water washing tower and the alkaline washing tower, removing the light components, separating a small amount of R1234ze and other light components, returning the light components to the fluorination reaction kettle for continuous reaction, removing the materials at the bottom of the light components tower to the 245 tower for rectification, drying to obtain high-quality R245fa, and returning the materials at the bottom of the 245 tower to the fluorination reaction kettle for continuous reaction. After R240fa is stably fed for about 18 hours, the R245fa finished product is discharged, the flow rate of circulating materials is stable, and the discharge flow rate of the finished product R245fa is about 270kg/h.
Summary of data: this example takes about 30 hours from the start of the telomerization reaction to the start of the fluorination station to adjust the steady discharge. Starting timing after the whole flow is stabilized, and stably operating for 300 hours, and summarizing the results as follows: the total consumption of 39t of chloroethylene, 96.9t of carbon tetrachloride, 15kg of chlorine and 69t of anhydrous hydrogen fluoride is carried out, so that the R245fa finished product 81t is obtained, the yield is 96.8%, and the purity is more than or equal to 99.9%.
Example 4
A full-flow continuous process for synthesizing 1, 3-pentafluoropropane, comprising:
telomerization: carbon tetrachloride, chloroethylene, iron powder and triethyl phosphate in a mass ratio of 300:50:1:4, after premixing in a mixer in front of the kettle, pumping the mixture into a CSTR reaction system, wherein the total feeding flow is 1800kg/h, the size of a telomerization reaction kettle adopts 5000L specification, the reaction temperature is 90-100 ℃, and the reaction pressure is 0.6+/-0.1 MPa. After the materials are reacted by a CSTR reaction system, the materials are continuously pumped out to a 240 continuous separation system, light components such as chloroethylene, carbon tetrachloride and the like are separated by a light component tower and returned to a mixer in front of a kettle for continuous reaction, the materials in the kettle are distilled and separated by a 240 tower, R240fa at the top of the tower is defluorinated, and the heavy components in the kettle comprise a small amount of mixture of unseparated R240fa, iron powder and triethyl phosphate which is pumped back to the mixer in front of the kettle for cyclic reaction. After the material is fed for about 12 hours, the flow rates of the circulating material, the R240fa extracted material and the like are stable, at the moment, the flow rate of the R240fa in the fluorination reaction is about 857kg/h, the feeding material is adjusted to be 620kg/h of carbon tetrachloride and 250kg/h of vinyl chloride, and the dynamic balance of the whole system material is kept.
Fluorination reaction: 1000kg of antimony pentachloride as a catalyst is put into a fluorination reaction kettle, 5000kg of anhydrous hydrogen fluoride is pumped, after the antimony pentachloride is preactivated, the temperature is kept at 90-100 ℃ and the discharge of telomerization reaction is waited for carrying out the fluorination reaction. The molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by telomerization reaction is as follows: 1:0.0001-0.0005:5-6 are introduced into a fluorination reaction kettle, after the telomerization reaction is carried out, the feeding flow of each material is R240fa857kg/h, chlorine gas is 0.03kg/h, anhydrous hydrogen fluoride is 470kg/h, and the reaction pressure of the fluorination reaction kettle is controlled to be 0.6+/-0.1 MPa. And (3) extracting a fluorination reaction product from the top of the reaction kettle, separating hydrogen chloride through the top of the hydrogen chloride tower, and removing the hydrogen fluoride tower from the materials in the tower kettle. Returning the materials at the bottom of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, separating the light components containing R245fa at the top of the tower, removing hydrogen fluoride and chlorine in the light components by washing the water washing tower and the alkaline washing tower, removing the light components, separating a small amount of R1234ze and other light components, returning the light components to the fluorination reaction kettle for continuous reaction, removing the materials at the bottom of the light components tower to the 245 tower for rectification, drying to obtain high-quality R245fa, and returning the materials at the bottom of the 245 tower to the fluorination reaction kettle for continuous reaction. After R240fa is stably fed for about 10 hours, the R245fa finished product is discharged, the flow rate of circulating materials is stable, and the discharge flow rate of the finished product R245fa is about 523kg/h.
Summary of data: this example takes about 22 hours from start of telomerization to steady discharge of the fluorination station. Starting timing after the whole flow is stabilized, and stably operating for 300 hours, and summarizing the results as follows: 75t of chloroethylene, 186t of carbon tetrachloride, 9kg of chlorine and 141t of anhydrous hydrogen fluoride are consumed together to obtain 156.9t of R245fa finished product, the yield is 97.5%, and the purity is more than or equal to 99.9%.
Example 5
A full-flow continuous process for synthesizing 1, 3-pentafluoropropane, comprising:
telomerization: carbon tetrachloride, chloroethylene, ferrous chloride and triethyl phosphate in a mass ratio of 300:50:1:4, after premixing in a mixer in front of the kettle, pumping the mixture into a CSTR reaction system, wherein the total feeding flow is 1800kg/h, the size of a telomerization reaction kettle adopts 5000L specification, the reaction temperature is 70-80 ℃, and the reaction pressure is 0.45+/-0.1 MPa. After the materials are reacted by a CSTR reaction system, the materials are continuously pumped out to a 240 continuous separation system, light components such as chloroethylene, carbon tetrachloride and the like are separated by a light component tower and returned to a mixer in front of a kettle for continuous reaction, the materials in the kettle are distilled and separated by a 240 tower, R240fa at the top of the tower is defluorinated, and the heavy components in the kettle comprise a small amount of mixture of unseparated R240fa, ferrous chloride and triethyl phosphate which is pumped back to the mixer in front of the kettle for cyclic reaction. After the material is fed for about 12 hours, the flow rates of the circulating material, the R240fa extracted material and the like are stable, at the moment, the flow rate of the R240fa in the fluorination reaction is about 796kg/h, the feeding material is regulated to be carbon tetrachloride 575kg/h and vinyl chloride 230kg/h, and the dynamic balance of the whole system material is kept.
Fluorination reaction: 1000kg of antimony pentachloride as a catalyst is put into a fluorination reaction kettle, 5000kg of anhydrous hydrogen fluoride is pumped, after the antimony pentachloride is preactivated, the temperature is kept at 100-110 ℃ and the discharge of telomerization reaction is waited for carrying out the fluorination reaction. The molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by telomerization reaction is as follows: 1:0.0001-0.0005:5-6 are introduced into a fluorination reaction kettle, after the telomerization reaction is carried out, the feeding flow of each material is R240fa796kg/h, chlorine gas is 0.1kg/h, anhydrous hydrogen fluoride is 440kg/h, and the reaction pressure of the fluorination reaction kettle is controlled to be 0.6+/-0.1 MPa. And (3) extracting a fluorination reaction product from the top of the reaction kettle, separating hydrogen chloride through the top of the hydrogen chloride tower, and removing the hydrogen fluoride tower from the materials in the tower kettle. Returning the materials at the bottom of the hydrogen fluoride tower to the fluorination reaction kettle for re-reaction, separating the light components containing R245fa at the top of the tower, removing hydrogen fluoride and chlorine in the light components by washing the water washing tower and the alkaline washing tower, removing the light components, separating a small amount of R1234ze and other light components, returning the light components to the fluorination reaction kettle for continuous reaction, removing the materials at the bottom of the light components tower to the 245 tower for rectification, drying to obtain high-quality R245fa, and returning the materials at the bottom of the 245 tower to the fluorination reaction kettle for continuous reaction. After R240fa is stably fed for about 10 hours, the R245fa finished product is discharged, the flow rate of circulating materials is stable, and the discharge flow rate of the finished product R245fa is about 480kg/h.
Summary of data: this example takes about 22 hours from start of telomerization to steady discharge of the fluorination station. Starting timing after the whole flow is stabilized, and stably operating for 300 hours, and summarizing the results as follows: the total consumption of 69t of vinyl chloride, 172.5t of carbon tetrachloride, 30kg of chlorine and 132t of anhydrous hydrogen fluoride, and the yield of the R245fa finished product is 97.3 percent, and the purity is more than or equal to 99.9 percent.
A comprehensive analysis of the above-described embodiments is available,
1. comparative example 1 and example 2 have different telomerization temperatures which affect the product yield of R240fa per unit time of intermediate product, and more R240fa per unit time can be obtained at 90-100℃than at 80-90℃under the same feed conditions.
2. In comparative example 1 and example 3, the application effect of the telomerization CSTR technology has a certain influence on the size of the reaction equipment, compared with a 5000L reaction kettle, more R240fa can be obtained per unit time unit volume of 3000L reaction kettle, the main reasons are that the reaction rate is faster, the reaction rapidly releases heat, a large amount of reaction heat is generated in the reaction moment between materials, although the reaction materials are mixed in the circumferential direction of the reaction kettle and are conveyed in radial synchronization with a pipeline by the application of the CSTR technology, the efficient mass transfer and heat transfer are realized, the larger reaction kettle still has the phenomenon that the materials are locally overheated due to the fact that the reaction kettle with the excessively large volume is not obvious, the generated side reaction products are relatively more, and the final product yield is influenced, so that the selection of a reactor with a proper size is also extremely critical under the condition of meeting the capacity requirement.
3. Comparative example 1 and example 4, example 5, the choice of catalyst and cocatalyst also has an effect on the yield of telomerization, and catalyst choice, feed ratio of materials, reaction temperature are also very critical control indicators for fluorination reactions.
The above embodiment is only a preferred embodiment of the present application, and is not limited in any way to the present application, but other variations and modifications can be made without departing from the technical solutions described in the claims.
Claims (10)
1. A full-flow continuous process for synthesizing 1, 3-pentafluoropropane, comprising:
telomerization: vinyl chloride, carbon tetrachloride, a catalyst I and a cocatalyst are mixed according to the molar ratio: 1:0.8-3: adding 0.01-0.1:0.01-0.2 into a pre-kettle mixer for premixing to obtain a mixture I, pumping the mixture I into a reactor system at 600-2000kg/h, carrying out telomerization at the reaction pressure of 0.3-1.0MPa and the reaction temperature of 60-150 ℃ to obtain telomerization materials, continuously pumping out and separating the telomerization materials to obtain R240fa, and returning separated vinyl chloride, carbon tetrachloride, catalyst I, cocatalyst and non-separated R240fa to the pre-kettle mixer for continuous reaction when separating the R240fa;
fluorination reaction: the liquid phase fluorination method is adopted, and the molar ratio of R240fa, chlorine and anhydrous hydrogen fluoride obtained by the telomerization reaction is as follows: 1:0.0001-0.0005:5-6 continuously feeding a fluorination reaction kettle containing an activated catalyst II, wherein the molar ratio of the feeding amount of R240fa per hour to the hydrogen fluoride in the catalyst II and the fluorination reaction kettle is 1:0.1-5:10-100, carrying out fluorination reaction at the reaction pressure of 0.4-1.0MPa and the reaction temperature of 60-150 ℃ to obtain a fluorination reaction product, separating the fluorination reaction product to obtain 1, 3-pentafluoropropane, when separating 1, 3-pentafluoropropane, and (3) returning the residual product after the 1, 3-pentafluoropropane is separated from the fluorination reaction product to a fluorination reaction kettle for continuous reaction.
2. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as defined in claim 1, wherein in telomerization, a reactor system is a CSTR, a 240 continuous separation system is adopted to pump materials of telomerization into a light component tower of the 240 continuous separation system to separate vinyl chloride and carbon tetrachloride, the separated vinyl chloride and carbon tetrachloride return to a pre-kettle mixer to continue reaction, tower bottom materials of the light component tower enter a 240 tower of the 240 continuous separation system to carry out rectification separation, R240fa is separated from the top of the 240 tower, and vinyl chloride, carbon tetrachloride, catalyst I, cocatalyst and unseparated R240fa at the bottom of the 240 tower return to the pre-kettle mixer to continue reaction.
3. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1 or 2, wherein the 240 continuous separation system further comprises a heavies column connected to 240 column, and wherein R240fa is separated from the top of the heavies column.
4. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1, wherein during the fluorination reaction, the product of the fluorination reaction is introduced into a hydrogen chloride column from which hydrogen chloride is separated at the top of the hydrogen chloride column, introducing tower kettle materials of the hydrogen chloride tower into the hydrogen fluoride tower, separating light components containing R245fa from the tower top of the hydrogen fluoride tower, sequentially entering a water washing tower and an alkaline washing tower, returning tower kettle materials of the hydrogen fluoride tower to a fluorination reaction kettle for re-reaction, after hydrogen fluoride and chlorine in the light group containing R245fa are removed by an alkaline washing tower, introducing the product into a dehydrogenation tower, separating out the light component containing R1234ze from the top of the dehydrogenation tower, returning the light component to a fluorination reaction kettle for continuous reaction, introducing tower kettle materials of the dehydrogenation tower into a 245 tower for rectification, introducing the top product of the 245 tower into a drying tower, drying the product by the drying tower to obtain 1, 3-pentafluoropropane, and returning the tower kettle materials of the 245 tower to the fluorination reaction kettle for continuous reaction.
5. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 2, wherein the CSTR comprises three serially connected telogens having a capacity of 2000-5000L.
6. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1, wherein said catalyst one is at least one of iron, zinc, ferrous chloride, or cuprous chloride.
7. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1, wherein said co-catalyst is an alkyl phosphate or an alkyl phosphite.
8. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1, wherein the telomerization reaction is carried out at a reaction temperature of 80-140 ℃ and a reaction pressure of 0.4-0.8MPa.
9. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1, wherein the reaction temperature of the fluorination reaction is 80-120 ℃ and the reaction pressure is 0.5-0.8MPa.
10. The full-flow continuous process for synthesizing 1, 3-pentafluoropropane as claimed in claim 1, wherein said catalyst two is one of antimony trichloride, antimony pentachloride, tin tetrachloride or titanium tetrachloride.
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