135results about "Preparation by halogen replacement" patented technology

The invention relates to the technical field of preparation of hydrofluoroolefin, in particular to a method for preparing 2, 3, 3, 3-tetrafluoropropene, which comprises the following steps: carrying out fluorination reaction on 3, 3, 3-trifluoro-2-chloropropene and excessive hydrogen fluoride under the action of a catalyst to generate a first mixture flow containing 1, 1, 1, 2, 2-pentafluoropropane (245cb), and separating the first mixture flow from the first mixture flow to obtain the 2, 3, 3, 3, 3-tetrafluoropropene. Then directly introducing the first mixture flow into a dehydrofluorination reactor for gas phase dehydrofluorination reaction to generate a second mixture flow containing 2, 3, 3, 3-tetrafluoropropene, hydrogen fluoride and unreacted raw materials, finally condensing the second mixture to remove hydrogen chloride, condensing and recycling hydrogen fluoride to obtain a third mixture flow, and rectifying the third mixture flow to obtain 2, 3, 3, 3-tetrafluoropropene. And 3, 3, 3, 3-tetrafluoropropene. According to the invention, unavoidable process wastes in the prior art are converted into recyclable reaction raw materials, the environmental protection and economic pressure of by-product treatment in the prior art is eliminated, meanwhile, the purpose of continuous flow reaction is effectively realized, and the process control difficulty and the process cost are reduced.

Systems and methods for the preparation of (Z)-1, 1, 1, 4, 4, 4-hexafluoro-2-butene are provided. Compositions prepared according to one or more of the systems and methods described herein and methods of using these compositions are also provided.

The invention relates to an improved process for the manufacture of a fluorinated organic compound, wherein the process comprises a fluorination reaction of an organic precursor compound having at least one chlorine substituent and / or at least one double bond, and said organic precursor compound is reacted in liquid phase in HF (hydrogen fluoride) serving as solvent and fluorinating agent in the presence of a fluorinating catalyst, and wherein the fluorination reaction is performed in liquid phase in a SiC block chemical reactor, and wherein the reaction mixture is withdrawn from SiC block chemical reactor, and wherein the process comprises optionally isolating and / or purifying the targeted fluorinated organic compound.

The application discloses a continuous production process and equipment for a trifluoromethylbenzene tower, and belongs to the field of organic fluorine chemistry. The production process comprises the following steps: S1: continuously feeding trichloromethylbenzene and hydrogen fluoride into a tower reactor connected with a heat exchanger circulating cooling system in a reverse direction, so that a three-stage continuous fluorination reaction occurs in the tower reactor to obtain crude trifluoromethylbenzene, and unreacted hydrogen fluoride is separated into liquid at the top of the tower and then flows back into the tower reactor; S2: the crude trifluoromethylbenzene obtained in the reaction is subjected to nitrogen bubbling in a bubble tower, and then is continuously distilled in a rectifying tower to obtain finished trifluoromethylbenzene; and S3: byproduct hydrogen chloride generated in the fluorination reaction is introduced into a hydrochloric acid tank to obtain hydrochloric acid, and the content of hydrofluoric acid in the hydrochloric acid is less than 1000 ppm. The method can greatly improve the utilization rate of raw material hydrogen fluoride, improve the purity of byproduct hydrochloric acid, reduce the generation amount of waste acid, avoid the sharp change of pressure in the reaction process, and realize large-scale, continuous, stable and safe production of trifluoromethylbenzene.

The present invention provides a method for the co-production of 1,1-difluoroethane and vinyl chloride, including: (a) vaporizing dichloroethane and hydrogen fluoride, and delivering the vaporized dichloroethane and hydrogen fluoride into a reactor for a catalytic reaction under the action of a catalyst to obtain a reaction product; (b) delivering the reaction product into a first rectifying tower for separation to obtain an overhead product from the first rectifying tower and a bottom product from the first rectifying tower; (c) delivering the overhead product from the first rectifying tower into a second rectifying tower for separation to obtain hydrogen chloride and a bottom product from the second rectifying tower; (d) delivering the bottom product from the second rectifying tower into a purifying tower for purification to obtain an overhead product from the purifying tower; (e) simultaneously delivering the overhead product from the purifying tower and a saturated organic solvent into a third rectifying tower for separation to obtain a 1,1-difluoroethane product and a bottom product from the third rectifying tower; and (f) delivering the bottom product from the third rectifying tower into a fourth rectifying tower for separation to obtain a vinyl chloride product and a bottom stream from the fourth rectifying tower. The present invention has the advantages of simple process, high conversion rate, and good product quality.

The invention relates to bio-based vinylidene difluoride. The invention also relates to processes for preparing bio-based vinylidene difluoride from various renewable raw materials. The invention further relates to vinylidene difluoride homopolymers obtained by polymerization of said monomer, as well as copolymers obtained by copolymerization of said monomer with one or more compatible co-monomers. Finally, the invention relates to the use of said homopolymers or copolymers in applications such as chemical engineering or electronics, particularly consumer electronic devices.

A method for producing a hydrofluorocarbon (HFC) is provided, the method being excellent in terms of the conversion of a chlorofluorocarbon and reduced in the formation of by-products.　This method for producing an HFC comprises reacting a chlorofluorocarbon (1A) with hydrogen in the presence of a catalyst to produce a hydrofluorocarbon (2A) in which one or two of the chlorine atoms of the chlorofluorocarbon (1A) have each been replaced with a hydrogen atom, the reaction being conducted using a reactive mixture comprising the chlorofluorocarbon (1A), hydrogen, and hydrogen chloride and having a hydrogen chloride concentration of 100-10,000 mass ppm of the chlorofluorocarbon (1A).

The invention provides a fluorination catalyst composition, a preparation method and application thereof, and a method for catalyzing 1, 1, 1, 3, 3-pentachloropropane to generate E-1-chloro-3, 3, 3-trifluoropropene, and belongs to the field of materials. The fluorination catalyst composition comprises a main catalyst and a third metal element loaded on the main catalyst, wherein the main catalyst is biomass charcoal simultaneously modified by a first metal element and a second metal element; wherein the first metal element comprises at least one of rare earth metal elements; the second metal element comprises at least one of Zr, Nb, Mo, V, Fe, Mn, Ti, Hf, Ga, In and Sn; the third metal element comprises at least one of Mg, Ca, Ba and Sr. The fluorination catalyst composition provided by the invention can efficiently catalyze 1, 1, 1, 3, 3-pentachloropropane to generate a gas phase fluorination reaction to generate E-1-chloro-3, 3, 3-trifluoropropene, has the advantages of high conversion rate, strong selectivity, long service life and the like, and is suitable for wide application.

Minimum-boiling, heterogeneous azeotropic and azeotrope-like compositions including 1,1,2,2,3-pentachloropropane (HCC-240aa) and hydrogen fluoride (HF), as well as methods for using these azeotropic or azeotrope-like compositions in the production of trifluorochloropropenes.

A method of synthesizing 3,3,3-trifluoropropene including contacting 1,1,1,3-tetrachloropropane, in the vapor phase, at a temperature sufficient to effect dehydrochlorination to form 1,1,3-trichloro-1-propene. The 1,1,3-trichloro-1-propene is isolated and subsequently contacted, in the vapor phase, with hydrogen fluoride in the presence of a fluorination catalyst at a temperature sufficient to effect formation of 3,3,3-trifluoropropene.

The invention discloses a preparation method of 2-bromo-1, 1, 1, 3, 3, 3-hexafluoropropane, and belongs to the technical field of synthesis of fluorine-containing intermediates. According to the preparation method, perfluoro-2-methyl-2-pentene and hypobromite are used as raw materials, 2-bromo-1, 1, 1, 3, 3, 3-hexafluoropropane is prepared under the action of an aprotic polar solvent under the low-temperature condition, the preparation method is low in cost and easy to obtain, the steps are simple and convenient, the reaction conditions are mild and rapid, and the method is suitable for industrial production. And a stable and reliable intermediate source is provided for downstream fields of fluorine-containing medicines, electronic chemicals and the like.

A process is provided which includes contacting a haloalkane reactant with a fluorination agent in the liquid phase, in the presence of a catalyst, under conditions which are free of or substantially free of a superacid, to produce a product stream including a haloalkane product, preferably a hydro(chloro)fluorocarbon.

There is provided a method for producing chlorofluorobutane (CFB) by forming chlorinated butadiene by dimerizing trichloroethylene (TCE) and fluorinating hydrogen atoms of the chlorinated butadiene. Trichloroethylene (TCE) is dimerized by using a dimer represented by the following formula (1) as a solvent and in the presence of a free radical generating agent at a temperature of 100° C. or higher. Hexachlorobutadiene (C4Cl6) is produced from the above dimer by chlorination and dehydrochlorination reaction, and further, the chlorofluorobutane (CFB) is produced by fluorinating the hexachlorobutadiene.

Processes for producing at least one of 2-chloro-3,3,3-trifluoropropene (HCFO-1233xf) or 2,3-dichloro-3,3-difluoropropene (HCFO-1232xf) from 1,1,2,3-tetrachloro-1-propene (HCO-1230xa), in the absence of a catalyst, are provided.

The invention provides a regeneration method and application of a chromium fluoride-based catalyst, and relates to the technical field of fluorine-containing olefin preparation. The regeneration method of the chromium fluoride-based catalyst comprises the following steps: A1, forcibly inactivating or collecting the inactivated chromium fluoride-based catalyst in industrial production; a2, a step of oxidizing and decarbonizing the inactivated chromium fluoride-based catalyst; and A3, treating the oxidized chromium fluoride-based catalyst in mixed gas of carbon monoxide and inert gas. The regenerated chromium fluoride-based catalyst can be used for reactions such as preparation of trans-1-chloro-3, 3, 3-trifluoropropene from 1, 1, 1, 3, 3-pentachloropropane, preparation of 2-chloro-3, 3, 3-trifluoropropene from 1, 1, 1, 2, 3-pentachloropropane and the like, and the selectivity of a target product is obviously improved.

A system may include a pre-pressurized canister filled with one or more polymeric materials and one or more low global warming potential (GWP) propellants. The one or more low GWP propellants may include at least one of carbon dioxide, nitrogen, or trans-1-Chloro-3,3,3-trifluoropropene. The system may include a valve sub-system including a dispensing valve configured to couple to the pre-pressurized canister and a valve control mechanism configured to regulate a pressure of the pre-pressurized canister to cause the pre-pressurized canister to release the one or more polymeric materials. The system may include a dispensing sub-system configured to fluidically couple the pre-pressurized canister to the valve sub-system. The dispensing sub-system may include a dispensing hose coupled to the dispensing valve and a dispensing member coupled to the dispensing hose. The dispensing member may be configured to dispense the one or more polymeric materials contained within the pre-pressurized canister.

The invention discloses a gas-phase one-step preparation method of 2, 2, 2, 3-tetrafluoropropene, and belongs to the technical field of fluorine chemical industry. The method aims at solving the problems that in the prior art, the technological process is complex, selectivity is poor and cost is high. The method is characterized in that gas-phase 1, 1, 2, 3-tetrachloropropene and / or 1, 1, 1, 2, 3-pentachloropropane and gas-phase hydrogen fluoride are mixed and preheated, and the mixture is introduced into a reactor filled with a specific catalyst for a one-step fluorination reaction. By optimizing parameters such as a raw material molar ratio and reaction pressure and cooperating with separation and purification processes including removal of HCl by a light component tower, refining by a heavy component tower and water alkali washing, high conversion rate of the raw materials and high selectivity of the reaction are realized.

To provide a method for producing chlorofluorobutane (CFB) by dimerizing trichloroethylene (TCE) to generate chlorinated butadiene and fluorinating the hydrogen atoms of this chlorinated butadiene.　Trichloroethylene (TCE) is dimerized at a temperature of 100°C or more in the presence of a free radical generator using a dimer represented by formula (1) from TCE as a solvent. Hexachlorobutadiene (C4Cl6) is produced by chlorination and dehydrochlorination from the dimer, and the hexachlorobutadiene is fluorinated to produce chlorofluorobutane (CFB).

The present invention discloses a method for co-producing 3,3,3-trifluoropropene and 2,3,3,3-tetrafluoropropene, introducing 1,1,1,3-tetrachloropropane, 1,1,1,2,3-pentachloropropane and hydrogen fluoride into a first reactor to have a reaction in the presence of a first catalyst to obtain a reaction product of the first reactor; distilling the reaction product of the first reactor to obtain a 3,3,3-trifluoropropene product and a column bottom product, mixing the column bottom product with the hydrogen fluoride, and feeding a resulting mixture into a second reactor to have a reaction in the presence of a second catalyst to obtain a reaction product of the second reactor; and separating hydrogen chloride from the reaction product of the second reactor, and then carrying out water washing, alkali washing and drying to obtain a 2,3,3,3-tetrafluoropropene product. The present invention has the advantages of simple process, high efficiency, high operation flexibility, small investment and low energy consumption.

This invention discloses a method for preparing phosphorus pentafluoride and co-producing difluorochloromethane. The method includes the following steps: 1) vaporizing PCl and reacting it with CHF3 and Cl2 in a reaction tube equipped with a supported catalyst to undergo a fluorine-chlorine exchange reaction, yielding a mixed gas containing products such as PF5 and CHClF2; 2) fractionating the mixed gas in a distillation column, collecting the product PF5 and unreacted CHF3 mixture from the top of the condenser. This mixture is then directly reacted with a LiF carbonate solution to convert it into a high-value-added lithium hexafluorophosphate solution; another product, CHClF2, is collected from the body of the distillation column. This invention utilizes CHF3, a high-temperature-effect, long-life fluorine chemical byproduct, as a fluorine source and PCl3 as a phosphorus source. Through the fluorine-chlorine exchange reaction of CF3H, PCl3, and Cl2, it converts into high-value-added PF5 gas, which is further converted into LiPF6, while simultaneously co-producing CHClF2, thus realizing the resource utilization of fluorine and possessing significant economic and social benefits.

The invention discloses a preparation method of 1, 1, 2-trifluoroethane, and belongs to the field of fluorine-containing alkane preparation. According to the method, 1, 1-difluoro-2-chloroethane and anhydrous hydrogen fluoride are used as raw materials, iron powder is creatively used as a catalyst, and the pollution problem of a traditional chromium-based catalyst is solved by optimizing reaction conditions. The method is characterized in that the iron powder catalyst is subjected to organic solvent washing, vacuum drying and reduction activation pretreatment in the hydrogen atmosphere, and the catalytic efficiency is remarkably improved. Through a system purification process and a raw material circulation mechanism, the effects that the highest conversion rate of R142 is 75.28% and the highest selectivity of R143 is 91.83% are achieved, the method has the outstanding advantages of being environmentally friendly, low in cost and easy to industrialize, and a reliable scheme is provided for clean production of 1, 1, 2-trifluoroethane.

The invention belongs to the technical field of fluorine chemical industry, and particularly relates to a preparation method of cis-1, 1, 1, 4, 4, 4-hexafluoro-2-butene. Comprising the following steps: I, under an illumination condition, enabling 3, 3, 3-trifluoropropene to react with carbon tetrachloride, optionally in the presence of a first catalyst, so as to obtain 1, 1, 1, 3-tetrachloro-4, 4, 4-trifluorobutane; and II, the obtained 1, 1, 1, 3-tetrachloro-4, 4, 4-trifluorobutane and hydrogen fluoride are subjected to a reaction under the action of a second catalyst, and cis-1, 1, 1, 4, 4, 4-hexafluoro-2-butene is obtained. According to the method, in the first step, the addition reaction is driven by illumination, the production cost can be greatly reduced by a photocatalysis mode, and the reaction efficiency can be improved by matching with a special catalyst; the fluorination reaction in the second step is matched with an exclusive catalyst, so that the conversion rate of reactants and the selectivity of a target product can be effectively improved, and the high efficiency of the whole preparation process is guaranteed.

The invention discloses a 2, 6-diethyl-4-methyl bromobenzene full-continuous flow synthesis process and a reaction device thereof, and relates to the technical field of compound synthesis. A reaction substrate and a sodium nitrite solution mixed with a catalyst are respectively input into a full-continuous flow shear reaction device through a feed port; after flowing through the temperature zone 1, the mixture is mixed with hydrobromic acid and enters a temperature zone 2 to complete a diazotization reaction, a diazotization reaction solution is obtained, the diazotization reaction solution flows out of the temperature zone 2, enters the bromination unit, reacts with a bromination reagent in the bromination unit, sequentially flows through a temperature zone 3 and is output from a discharge port, and a final product 2 is obtained after extraction, water washing, desolvation and distillation. The catalyst is 2, 6-diethyl-4-methyl bromobenzene. A continuous process is adopted, so that the difficulty of industrial application is greatly reduced; and during industrial amplification, the required production scale can be obtained through one-time amplification without tedious and complex multi-time step-by-step amplification and adjustment and optimization of process conditions and parameters, so that manpower, material resources and project development time are greatly saved.

The invention relates to the technical field of protein electrophoretic separation, and particularly discloses a capillary electrophoretic separation gel material as well as a preparation method and application thereof. In the capillary electrophoresis separation gel material 12-n fluorododecyl lithium sulfate provided by the invention, n is equal to 1, 2 or 3. When being used in gel electrophoresis, the polymer is more stable than SDS under a high-temperature condition. Meanwhile, the 12-n fluorododecyl lithium sulfate capillary gel electrophoresis separation gel provided by the invention has good migration time consistency during long-time operation, and methodological detection shows that the gel has good repeatability. The capillary gel electrophoresis separation gel has very good repeatability, precision, linearity and accuracy indexes when being used for separating the polysaccharylation site fusion protein.

This specification provides one or more embodiments of a high-purity hexafluoroethane production apparatus, including a main body, a reaction chamber installed outside the main body, and a separation tube for separating hexafluoroethane and hydrogen chloride, with the separation tube located inside the main body. Heating equipment is matched within the main body, and a storage chamber is provided within the reaction chamber outside the main body. The storage chamber has a mesh structure around its periphery to allow the reactants to contact the internal solid particles and to provide heating during the internal reaction. After passing through the reaction chamber and the corresponding separation chamber, the reactants can enter the separation chamber for separation processing. During separation, the pressure and water flow are controlled to ensure that the reaction product, hydrogen chloride, is completely dissolved in water, significantly improving the purity of the final product, hexafluoroethane. The entire reaction process and effect are completed within the equipment, reducing the requirements of traditional equipment processing in terms of large amounts of equipment and space, and significantly improving the purity of the product during re-separation.

A process for preparing a fluorinating reagent from a calcium-containing compound is disclosed. The process bypasses the requirement to form hydrofluoric acid. The fluorinating reagent can be used to prepare high-value fluorochemicals.

The invention provides a method for co-producing HFO-1234yf and HFO-1234ze. The method comprises the following steps: (1) reacting dichloroethylene with trifluoromethane under the action of a first catalyst to prepare trifluorodichloropropane; (2) carrying out gas-phase dehydrochlorination reaction on the trifluorodichloropropane under the action of a second catalyst to generate trifluorochloropropene; and (3) the trifluorochloropropene and anhydrous hydrogen fluoride are subjected to a gas phase fluorination reaction under the action of a third catalyst, and HFO-1234yf and HFO-1234ze are generated. By optimizing a reaction path and a catalyst system, efficient co-production of HFO-1234yf and HFO-1234ze is realized, and the method has the advantages of mild reaction conditions, high product selectivity and the like, and is suitable for industrial production.

A delivery pipe I (4) of a liquid chlorine steel cylinder (1) and a delivery pipe II (5) of a dichloromethane storage tank (2) form one path and then are communicated with a dichloromethane multi-stage pump (8) through a mixer (6), and a hydrogen fluoride storage tank (3) is communicated with a shield pump (10). The dichloromethane multi-stage pump (8) and the shield pump (10) are respectively communicated with the fluorination reactor (12) through a mixed feeding pipeline I (11) and a mixed feeding pipeline II (13), and the fluorination reactor (12) is communicated with the difluoromethane finished product storage tank (15) through a finished product delivery pump (14). According to the preparation method disclosed by the invention, the difluoromethane and the hydrogen fluoride react in proportion under the action of the antimony pentachloride to prepare the difluoromethane, and the liquid chlorine is introduced through the liquid chlorine steel cylinder to be uniformly mixed with the difluoromethane. The service life of the catalyst is prolonged, corrosion to reaction equipment is reduced, and the reaction is fully carried out.

This invention discloses a method for preparing 2,3,3,3-tetrafluoropropylene, comprising reacting carbon tetrachloride with ethylene in the presence of a catalyst containing reduced iron powder and a co-catalyst, separating and purifying the reactants to obtain HCC-250fb; subjecting HCC-250fb to dehydrochlorination to generate HCC-1240za; reacting HCC-250fb with chlorine in a liquid-phase or gas-phase chlorination reaction to obtain HCC-240db; reacting HCC-240db with hydrogen fluoride in a gas-phase fluorination reaction to generate HCFO-1233xf; and reacting HCFO-1233xf with hydrogen fluoride in a gas-phase fluorination reaction in the presence of a supported or unsupported chromium oxide catalyst to generate HFO-1234yf. The method of this invention uses readily available raw materials, has low cost, and allows unreacted raw materials to be recycled for further reactions, resulting in minimal waste emissions.