166results about "Preparation by halogen addition" patented technology

The invention belongs to the technical field of fluoride preparation, and particularly relates to a method for preparing hexafluoroethane at low temperature. The method comprises the following steps: S1, liquefying tetrafluoroethylene: vacuumizing a reaction kettle, introducing tetrafluoroethylene, and cooling the reaction kettle with liquid nitrogen until tetrafluoroethylene is completely liquefied; s2, preparing hexafluoroethane through reaction of fluorine-nitrogen mixed gas and tetrafluoroethylene: introducing the fluorine-nitrogen mixed gas into the tetrafluoroethylene liquefied in the step S1 in a bubbling manner, stirring and reacting, and continuously stirring and reacting after the introduction of the fluorine-nitrogen mixed gas is finished, so as to obtain the hexafluoroethane; and S3, gas purification: after the reaction is finished, purging the gas phase space of the reaction kettle with nitrogen to remove residual gas in the reaction kettle, then heating the reaction kettle until the hexafluoroethane is gasified, and carrying out alkali washing, drying and rectification to obtain the high-purity hexafluoroethane. In the preparation method disclosed by the invention, the reaction is safer and easier to control under a low-temperature condition, and the preparation method disclosed by the invention is simple in process, high in reaction speed, high in yield, few in product impurity, easy to purify and suitable for industrial production.

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 %.

The invention relates to a preparation method of octafluorocyclobutane, which comprises the following steps: mixing hexafluorocyclobutene with preheated nitrogen trifluoride, carrying out addition reaction on the mixed gas, and condensing and collecting the octafluorocyclobutane after the reaction is completed. According to the method, octafluorocyclobutane is prepared by using nitrogen trifluoride, continuous production of octafluorocyclobutane with the purity being 99 wt% or above can be achieved, the preparation method has the advantages of being low in raw material cost, simple in process, low in energy consumption, simple in product separation, good in selectivity and convenient to purify, and amplified continuous production can be achieved easily.

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 invention discloses a method for preparing 3, 3, 3-trifluoro-1-propyne through a two-step method, the 3, 3, 3-trifluoro-1-propyne is prepared through a production system and collected through a material collecting system, and the preparation steps of the production system comprise: (1) in a first solvent, carrying out an addition reaction on 3, 3, 3-trifluoro-1-propylene and ICl to obtain 2-iodo-1-chloro-3, 3, 3-trifluoropropane; (2) in a second solvent, enabling the 2-iodine-1-chloro-3, 3, 3-trifluoropropane to react with alkali to eliminate bimolecular hydrogen halide so as to obtain 3, 3, 3-trifluoro-1-propyne; the temperature of the material receiving system is-196 to-60 DEG C, and the pressure of the material receiving system is-0.03 MPa to normal pressure. The 3, 3, 3-trifluoro-1-propyne is prepared by taking trifluoropropene as a raw material through two-step reaction, and the method has the advantages of simple preparation steps, high reaction yield, small amount of three wastes, low production cost and the like, and is very suitable for industrial production.

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%.

The invention relates to the technical field of pesticide production, in particular to a method and a device for continuously preparing octachlorocyclopentene, and the method at least comprises the following steps: by taking dicyclopentadiene and chlorine as raw materials, cracking dicyclopentadiene to obtain cyclopentadiene, gasifying the cyclopentadiene to obtain gasified cyclopentadiene, and separating the gasified cyclopentadiene from the chlorine to obtain the octachlorocyclopentadiene. According to the method, gasified cyclopentadiene reacts with chlorine in a reactor to prepare tetrachlorocyclopentane, tetrachlorocyclopentane is transferred to a chlorination kettle, chlorine continues to be introduced, and octachlorocyclopentene is prepared through staged cooling, the method does not need to add a diluent, operation is easy and convenient, side reactions are few, the yield is high, and meanwhile the continuous process can shorten the reaction time, improve the productivity and facilitate industrialization.

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 disclosure provides an integrated process for producing trifluoroiodomethane (CF3I), in three steps: a) reacting a first reactant stream comprising hydrogen (H2) and iodine (I2) in the presence of a first catalyst to produce a first product stream comprising hydrogen iodide (HI); (b) reacting the first product stream with a second reactant stream comprising trifluoroacetyl chloride (TFAC) in the presence of a second catalyst to produce an intermediate product stream comprising trifluoroacetyl iodide (TFAI); and (c) reacting the intermediate product stream to produce a final product stream comprising trifluoroiodomethane. (CF3I).

To provide a process for making 2,3,3,3-tetrafluoropropene (HFO-1234yf) from a composition including 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb).SOLUTION: A method includes providing a composition including 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) to a reactor including a heater surface at a surface temperature greater than about 850°F (454°C), and then bringing the composition into contact with the heater surface for a contact time of less than 10 seconds to dehydrochlorinate a portion of the HCFC-244bb to make HFO-1234yf.SELECTED DRAWING: Figure 1

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.

The present invention relates to a method for producing terephthaloyl chloride, and the purity of hexachloroparaxylene, which is an intermediate raw material, can be improved by adopting a photochlorination method instead of a radical initiator, and by controlling a light amount of light irradiation to less than 2000 LUX, the advantages of a low occurrence of side reactions of hexachloroparaxylene and a high yield are provided. In addition, the present invention provides a method for producing terephthaloyl chloride in which, by adopting a circulation system, chlorine gas is not discharged to the outside.

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 present invention discloses a preparation method of bromochlorides or bromoazides. Using 1,3-conjugated diene compounds as raw materials and NBS as the bromine positive reagent, they are respectively combined with TMSCl or TMSN 3 to achieve the selective bromochlorination and bromoazidation reactions of 1,3-conjugated dienes, and a series of bromochlorides and bromoazides with wide applications are successfully obtained. The present invention adopts a one-step method with mild conditions, without any metals and additives, simple operation, high reaction efficiency, wide substrate scope, and high yields, regioselectivities and stereoselectivities of the products. The present invention provides a new means for synthesizing various bromochlorides and bromoazides, with strong economic practicability and industrial application prospects. In addition, a series of derivatization reactions indicate that the above products have important synthetic application values.

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.

The present invention relates to a process for producing dimethyl ether (DME) and hydrogen (H2) from methane, comprising the steps of: a) providing a gaseous feed stream comprising methane; b) reacting said gaseous feed stream with at least one halogen reactant (X2), under reaction conditions effective to produce an effluent stream comprising methyl halide (MeX), and hydrogen halide (HX); c) separating from the effluent stream obtained in step b): (i) a methyl halide (MeX) stream; and, (ii) a hydrogen halide (HX) stream; d) reacting the methyl halide (MeX) stream separated in step c) with a solid metal oxide (MO(s)) under reaction conditions effective to produce metal halide (MX) and dimethyl ether (DME); and e) decomposing by means of electrolysis said hydrogen halide (HX) stream separated in step c) under conditions effective to produce a gaseous hydrogen (H2) stream and a stream comprising halogen reactant (X2).

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.

A method of producing carbon tetrachloride includes providing a chloromethanes stream, combining the chloromethanes stream with chlorine and additional carbon tetrachloride to form a reaction mixture, wherein the reaction mixture includes at least stoichiometric levels of chlorine, introducing electromagnetic radiation to the reaction mixture and subjecting the reaction mixture to suitable reaction conditions to form product carbon tetrachloride, and collecting a product stream including the product carbon tetrachloride.

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 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%.

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.