104results about "Preparation by halogen addition" patented technology

The invention relates to production equipment and a production method of 1, 1, 1, 2, 3-pentachloropropane, and belongs to the technical field of preparation of chemical intermediates. According to the invention, 1, 1, 1, 3-tetrachloropropane is adopted as an initial raw material, 1, 1, 1, 2, 3-pentachloropropane is produced through dehydrochlorination and chlorination in the serial tower reactor, and compared with a traditional two-step synthesis process of 1, 1, 1, 2, 3-pentachloropropane, after dehydrochlorination of 1, 1, 1, 3-tetrachloropropane and a 1, 1, 3-trichloropropene chlorination system are coupled, the process flow is shortened; compared with the existing one-pot synthesis process, the reaction is easier to control; a fixed bed catalyst system is adopted, the problems that traditional anhydrous ferric chloride catalyst powder is not easy to add, poor in dispersity and frequent to add are solved, saponification salt-containing wastewater is not discharged, the process is green and environmentally friendly, and the application prospect is wide.

The present invention discloses a method and system for producing hexafluorobutadiene, which includes the following steps: In step (1), an organic solution of bromotrifluoroethylene and zinc powder are respectively introduced into a first reactor containing an initiator, zinc powder, and an organic solvent, followed by a second reactor, and reacted to obtain a trifluorovinylzinc bromide solution. The reaction solution is then introduced into a precipitator to separate excess zinc powder, resulting in a zinc-free trifluorovinylzinc bromide solution. The excess zinc powder is then filtered and reused. In step (2), the trifluorovinylzinc bromide solution obtained above and a pre-prepared composite catalyst solution are introduced into a third reactor and subjected to a coupling reaction to obtain crude hexafluorobutadiene. In step (3), the crude hexafluorobutadiene obtained above is purified to obtain a product with a purity of ≥ 99.9%.

To provide a new method for producing a fluorinated organic compound in which removal or separation of an auxiliary is easy and which is advantageous in production cost.SOLUTION: A compound represented by the following formula (1): wherein R1, R2 and n are as defined in the description. The method comprises reacting the compound represented by the formula (1) with (A) at least one fluorine source selected from hydrogen fluoride, a hydrogen fluoride salt and a fluoride salt, (B) at least one iodine source selected from iodine and ammonium iodide, and (C) a compound having at least one fluorinated quaternary nitrogen atom in the molecule. A step of difluorinating the compound represented by the formula (1), wherein the amount of the iodine source (B) used is less than 1.0 mol per 1 mol of the compound represented by the formula (1).SELECTED DRAWING: None

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.

The present invention relates to a process for preparing 1,1,1-trifluoro-2,3-dichloropropane which comprises contacting chlorine with 3,3,3-trifluoropropene in the presence of a catalyst to form 1,1,1-trifluoro-2,3-dichloropropane, wherein the catalyst comprises at least one metal halide, where the metal is a metal from Group 13, 14 or 15 of the periodic table or a transition metal or combination thereof.

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.

To provide a composition including 1,1,1-trifluoro-2,3-dichloropropane.SOLUTION: A composition includes 1,1,1-trifluoro-2,3-dichloropropane, 3,3,3-trifluoropropene, a chlorine gas, a catalyst, and 1,1,1-trifluoro-3-chloropropylene. The catalyst includes at least one metal chloride. The metal is nickel, iron, chromium, or a combination of them. The at least one metal chloride is supported on activated carbon. The molar ratio of 3,3,3-trifluoropropene to the chlorine gas ranges from 1: 0.02 to 1: 1.SELECTED DRAWING: None

The invention relates to a method for resource utilization of 1, 1, 2-trichloropropane, and the method comprises the following steps: (1) carrying out high-temperature cracking on a material flow containing 1, 1, 2-trichloropropane to obtain a material flow containing 3, 3-dichloropropene; and (2) carrying out chlorination on the material flow containing 3, 3-dichloropropene to obtain a material flow containing 1, 1, 2, 3-tetrachloropropane. According to the method disclosed by the invention, the propylene chlorination by-product 1, 1, 2-trichloropropane can be subjected to high-temperature cracking to obtain 3, 3-dichloropropene, and 1, 1, 2, 3-tetrachloropropane is obtained after the 3, 3-dichloropropene is chlorinated. The byproduct 1, 1, 2-trichloropropane is fundamentally solved, the process route is simple, the flow is short, the reaction conversion rate is high, the selectivity is good, and industrial implementation is facilitated.

The invention relates to a device and a method for producing partially chlorinated alkanes by means of a direct chlorination of alkenes. In particular, the invention relates to a device and a method for producing 1,2-dichloroethane by means of a direct chlorination of ethene (synonym: ethylene). The invention is characterized in that a loop reactor is used for the direct chlorination, wherein the outlet for the produced partially chlorinated alkane is provided on a vertical position of the loop reactor (in the operating state) on a lateral wall of the loop reactor, the vertical position being situated below half the height of the loop reactor.

The invention relates to the technical field of electronic-grade fluorine-containing special gas synthesis, in particular to an electronic-grade hexafluoroethane directional synthesis process based on a composite catalyst, which comprises the following steps: S1, carrying out reflux treatment on activated carbon by hydrofluoric acid-nitric acid mixed liquor, sequentially loading aluminum trichloride, cesium fluoride, lanthanum oxide and graphene quantum dots, and roasting in a nitrogen atmosphere to prepare the composite catalyst; s2, mixing tetrafluoroethylene and hydrogen fluoride in proportion, dehydrating through a molecular sieve, and removing impurities through a nano-zinc oxide coating purification tower; s3, introducing the raw materials into a fixed bed with a guide plate, and carrying out segmented temperature control reaction under the adjustment of a composite catalyst and perfluorohexane; and S4, condensing, alkali-washing and drying the reaction product, and rectifying in a rectifying tower to obtain the electronic-grade hexafluoroethane. And S5, adsorbing the rectification tail gas by a composite adsorbent, and resolving and recycling the raw materials for pretreatment. The process improves the selectivity and purity of hexafluoroethane, prolongs the service life of the catalyst, is good in regeneration effect, reduces energy consumption and raw material loss, reduces wastewater discharge, and meets the requirements of the semiconductor industry.

The utility model relates to the technical field of preparation of dichloroethane through chlorination, in particular to a high-temperature chlorination reactor for ethylene chlorine. Comprising a circulating part, a separating part and a washing part which are sequentially connected, the circulating part is a U-shaped bent pipe, the separating part is a horizontal tank, the washing part is a spraying pipe, two outlets are formed in the two U-shaped ends of the top of the U-shaped bent pipe and communicated with the bottom of the horizontal tank, and the lower end of the spraying pipe is communicated with the top of the horizontal tank; the high-temperature chlorination reactor disclosed by the utility model is influenced by chlorine dissolution, the chlorine dissolution effect can be obviously improved by increasing the circulation volume, the axial flow pump is arranged to control the static mixer arranged above the distribution pipe to ensure that chlorine is fully dissolved, the reaction conversion rate and the product yield are effectively improved, entrainment and a catalyst entrained in gas can be effectively removed by the washing part, and the product quality is improved. The liquid and the catalyst are recovered to prevent the liquid and the catalyst from being taken out from the top of the reactor.

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.

The present invention provides a method for preparing a supported carbon catalyst, the method comprises at least the following steps: (1) contacting a gas containing an organic silicon source with a silicon oxide-based material to obtain a precursor; (2) contacting the precursor with a gas containing an organic carbon source to obtain the supported carbon catalyst. The temperature and energy consumption of the chemical vapor deposition of heteroatom-containing carbon material on silica-based materials can be greatly reduced in this method, and the cost of the catalyst can be effectively reduced.

Alkyne compounds are produced by contacting a 1-alkene with chlorine, optionally in the presence of a halide salt, to form a 1,2-dichloroalkane compound, then optionally contacting the 1,2-dichloroalkane compound with a catalyst to form a chloroalkene compound, and then contacting the 1,2-dichloroalkane compound and / or the chloroalkene compound with a base and a phase transfer catalyst to form a reaction mixture comprising a 1-alkyne and / or a 2-alkyne. Representative alkynes that can be produced using this process include 1-hexyne, 2-hexyne, 2-heptyne, and the like.

The invention provides a method for catalyzing free radical-nucleophilic addition halogenation-functionalization of alkene through a visible light induced iron-based material, and belongs to the technical field of organic chemistry. According to the method, olefin is taken as a reaction substrate, inorganic halide MXn is taken as a halogen source, in the presence of a nucleophilic reagent Nu, a halogen functionalization reaction of olefin is efficiently and highly selectively realized through co-catalysis of an iron-based material and visible light, C-X (X = Cl, Br) and C-Y (Y = X, O, S) are constructed at the same time, and a halogen-functionalization product is prepared. According to the method, halide ions are used for replacing traditional halogen simple substances, and olefin which is low in price and easy to obtain is directly converted into the halide which contains a plurality of functional groups and has a high additional value and subsequent derivation potential through free radical-nucleophilic addition under a mild condition. The method has the advantages of environment friendliness, high selectivity, low energy consumption and the like, and has important theoretical significance and practical application value.

The invention provides a preparation method of hexafluorobutadiene, which comprises the following steps: 1) carrying out electrophilic addition reaction on chlorotrifluoroethylene and liquid bromine at normal temperature and normal pressure to generate 1, 2-dibromo-1-chloro-1, 2, 2-trifluoroethane; 2) mixing zinc powder, 1, 2-dibromo-1-chloro-1, 2, 2-trifluoroethane and an aprotic polar solvent, and carrying out a reaction so as to obtain a zinc reagent containing 1-chloro-2-bromo-1, 2, 2-trifluoroethyl zinc bromide and 1, 2-dibromo-1, 2, 2-trifluoroethyl zinc chloride; 3) adding a catalyst and a zinc reagent, and carrying out a self-coupling reaction to generate an intermediate product containing 1, 4-dibromo-2, 3-dichloro-1, 1, 2, 3, 4, 4-hexafluorobutane and 1, 2, 3, 4-tetrabromo-1, 1, 2, 3, 4, 4-hexafluorobutane; 4) dehalogenating the intermediate product to generate hexafluorobutadiene; the method has the effects of simple reaction process, relatively low risk, relatively mild reaction conditions and relatively high yield.

The invention discloses a preparation method of a fluidized bed catalyst and a method for preparing 1, 2-dichloroethane by directly chlorinating ethylene. Comprising the following steps: (1) preparing a modified carrier; al2O3 and Sc2O3 are mixed and ground, and a modified carrier A is prepared; (2) preparing active components; compounding a copper compound, a potassium compound and a noble metal simple substance mixture, and dissolving in acid to prepare an active component B; (3) active component loading; and mixing and dipping the active component B solution in the step (2) and the modified carrier A in the step (1) to obtain a mixture C containing the catalyst. Special elements are introduced to improve the carrier, so that the adsorption performance and reaction activity of the catalyst are enhanced; and the catalyst is suitable for wear requirements of the fluidized bed. A third reaction medium is introduced to weaken side reaction. The ethylene full-gas-phase direct chlorination is realized to synthesize the 1, 2-dichloroethane.

This invention discloses a method for iodine recovery and reuse during the preparation of tetrachlorohexafluorobutane, comprising the following steps: S1, preparing trifluorodichloroiodoethane using refined iodine and trifluorochloroethylene as raw materials, and preparing a tetrachlorohexafluorobutane reaction solution using trifluorodichloroiodoethane as raw material; S2, adding water to the tetrachlorohexafluorobutane reaction solution to obtain a soluble solution, oxidizing, filtering, and refining the aqueous phase to obtain refined iodine, and distilling the organic phase to obtain refined tetrachlorohexafluorobutane, an organic solvent containing iodine and zinc iodide, and an organic iodide; S3, washing the organic solvent containing iodine and zinc iodide with an absorbent to obtain an iodide ion aqueous solution, which is then oxidized, filtered, and refined to obtain refined iodine; the organic iodide is catalytically chlorinated to obtain iodine chloride, which is used to prepare trifluorodichloroiodoethane. The entire process of this invention is rapid, environmentally friendly, and has a high iodine recovery rate, making it suitable for large-scale industrial production.

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).

Disclosed is a method for producing 1,4-dibromo-2,3-dichlorohexafluorobutane (Br-CF2-CFCl-CFCl-CF2-Br), in which, through the photoreaction of 1,2-dibromo-1-chlorotrifluoroethane (Br-CF2-CFCl-Br) with a CTFE (CF2=CFCl) gas mixed with a diluent gas, 1,4-dibromo-2,3-dichlorohexafluorobutane is produced. According to an embodiment of the present disclosure, an intermediate for producing hexafluoro-1,3-butadiene (C4F6) can be produced with high production yield.

The application provides a preparation method of hexafluorobutadiene, 1) under normal temperature and pressure, chlorotrifluoroethylene and liquid bromine are subjected to an electrophilic addition reaction to generate 1,2-dibromo-1-chloro-1,2,2-trifluoroethane; 2) zinc powder and 1,2-dibromo-1-chloro-1,2,2-trifluoroethane are mixed with an aprotic polar solvent to generate a zinc reagent containing 1-chloro-2-bromo-1,2,2-trifluoroethane zinc bromide and 1,2-dibromo-1,2,2-trifluoroethane zinc chloride; 3) a catalyst is added, and the zinc reagent is subjected to a self-coupling reaction to generate an intermediate product containing 1,4-dibromo-2,3-dichloro-1,1,2,3,4,4-hexafluorobutane and 1,2,3,4-tetrabromo-1,1,2,3,4,4-hexafluorobutane; 4) the intermediate product is subjected to dehalogenation to generate hexafluorobutadiene; and the method has the effects of simple reaction process, low danger, relatively mild reaction conditions and high yield.

The present application relates to processes of preparing (E)-1,1,1,4,5,5,5-heptafluoro-4-(trifluoromethyl)pent-2-ene.

The present disclosure provides a method for more efficiently obtaining HFO-1132(E) and / or HFO-1132(Z) than in conventional methods. The present disclosure specifically provides a method for producing a composition comprising trans-1,2-difluoroethylene (HFO-1132(E)) and / or cis-1,2-difluoroethylene (HFO-1132(Z)), the method comprising: (x) supplying a starting material gas comprising 1,1,2-trifluoroethane (HFC-143), HFO-1132(E) and / or HFO-1132(Z), and a diluent gas to a reactor containing a catalyst to perform a dehydrofluorination reaction of HFC-143 and an isomerization reaction between HFO-1132(E) and HFO-1132(Z), thereby obtaining a reaction product comprising HFO-1132(E) and HFO-1132(Z), wherein the content of the diluent gas in the starting material gas is 1 to 80 mol%.

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.

A process for producing E-1,1,1,4,4,4-hexafluorobut-2-ene comprises contacting 1,1,2,4,4-pentachlorobuta-1,3-diene with hydrogen fluoride in the vapor phase in the presence of a fluorination catalyst. A process for producing Z-1,1,1,4,4,4-hexafluorobut-2-ene further comprises contacting E-1,1,1,4,4,4-hexafluoro-2-butene with chlorine in the presence of a catalyst to produce 2,3-dichloro-1,1,1,4,4,4-hexafluorobutane, followed by reaction with base to produce 1,1,1,4,4,4-hexafluoro-2-butyne, and subsequently hydrogenating hexafluoro-2-butyne to produce Z-1,1,1,4,4,4-hexafluoro-2-butene.

The invention relates to the field of fluorine-containing fine chemicals, and particularly provides a preparation method of 1, 1-difluoro-2-vinyl iodide, which comprises the following steps: taking elemental iodine and vinylidene fluoride as raw materials, carrying out photocatalysis to obtain an intermediate product, and adding an alkali metal catalyst to obtain the 1, 1-difluoro-2-vinyl iodide. The method has the characteristics of simple process, low cost, high yield and the like.

The utility model relates to the technical field of preparation of dichloroethane by chlorination, in particular to a production device for producing dichloroethane by combining high-temperature and low-temperature chlorination of ethylene and chlorine. Comprising a high-temperature chlorination reactor, a product tower, a heavy component removal tower and a light component removal tower, a first chlorine gas inlet and an ethylene gas inlet are formed in the high-temperature chlorination reactor, and a crude dichloroethane gas phase outlet is formed in the top of the high-temperature chlorination reactor; a coarse dichloroethane gas phase inlet and a product tower material outlet are formed in the tower bottom of the product tower, a product tower gas phase outlet is formed in the tower top of the product tower, and a fine dichloroethane side line extraction port and a product tower liquid phase inlet are formed in the middle of the product tower; according to the device, on the basis of reducing the consumption of steam and circulating water, reaction tail gas is utilized to react with chlorine again to generate dichloroethane, so that the output of waste gas is reduced, the conversion rate of raw materials is improved, the production cost is reduced, the production efficiency is improved, and the production cost is reduced. And the utilization rate of the raw material ethylene is increased from 77% to 95%.

The present disclosure features methods for modulating the production of a small halogenated organic compound from a microalgae, as well as related compositions and methods thereof.