387 results about "Fluoridation reaction" patented technology

One or more materials selected from 1,1,1,3,3-pentachloropropane, 1,1,3,3-tetrachloropropene and 1,3,3,3-tetrachloropropene are used as the specific materials described above. Before submitting the materials and HF to a fluorination reaction, almost all water is removed from them.To continuously manufacture useful intended products efficiently as well as to prevent deactivation of the catalyst and the accumulation of organic substances with high boiling points when manufacturing said useful 1,1,1,3,3-pentafluoropropane and/or 1-chloro-3,3,3-trifluoropropene, by fluorinating the specific materials with HF in the presence of a catalyst.

The invention relates to the field of lithium batteries and lithium capacitors, in particular to a preparation method for difluorosulfimide lithium salt and application of the difluorosulfimide lithium salt. The preparation method for the difluorosulfimide lithium salt, provided by the invention, comprises the following steps: (1) performing fluorination reaction: synthetizing midbody difluorosulfimide from dichlorosulfimide and hydrogen fluoride under the action of a catalyst; (2) performing reaction between the difluorosulfimide obtained in the step 1 and alkaline lithium, and performing solid-liquid separation after the reaction to obtain an LiFSI product. The preparation method for the difluorosulfimide lithium salt, provided by the invention, is low in cost, few in by-product and simple in post-treatment, and the quality and the purity of the product are ensured, therefore the preparation method which is capable of obtaining the high-quality and high-purity product and is economic and practical is provided; the preparation method is suitable for industrial production.

The present invention provides a preparation method of lithium bis(fluorosulfonyl)amide. The method comprises the following steps: A) reacting chlorosulfuric acid with ammonia in the presence of an organic base to obtain organic alkali salt of bis(fluorosulfonyl)amide; B) mixing the bis(fluorosulfonyl)amide obtained in the step A) with HF for a fluorinated reaction to obtain an organic alkali salt of bis(fluorosulfonyl)amide; C) mixing the organic alkali salt of bis(fluorosulfonyl)amide obtained in the step B) with an alkaline substance for a neutralization reaction to obtain a bis(fluorosulfonyl)amid metal salt crude product; D) purifying the bis(fluorosulfonyl)amid metal salt crude product obtained in the step C) to obtain bis(fluorosulfonyl)amid metal salt; and E) mixing the bis(fluorosulfonyl)amid metal salt obtained in the step D) with a lithium reagent for a replacement reaction, so as to obtain lithium bis(fluorosulfonyl)amide. The preparation method provided by the invention has the characteristics of low raw material cost, low impurity content in the product and high yield of lithium bis(fluorosulfonyl)amide.

The invention discloses high-fluoride-content graphite fluoride and a preparation method thereof. The method comprises the following steps: preparing aqueous dispersion liquid of graphite oxide with a conventional improved Hummers method, then freezing the aqueous dispersion liquid of graphite oxide in liquid nitrogen to be completely frozen into solid, and freezing and drying to obtain cellular graphite oxide; under a mixed atmosphere of inert gas and fluoride, warming the cellular graphite oxide for fluoridation, and cooling to room temperature. The fluoride content of the prepared high-fluoride-content graphite fluoride is 55-70 percent, fluorine atoms are bonded with carbon atoms in a covalent bond mode, weightlessness peak temperature is larger than 470 DEG C, the heat stability is good, and the resistance is larger than 1012 omega. The prepared graphite fluoride has the advantages of high fluoride content, good heat resistance of fluorine-containing groups, low cost, simple process, lower reaction temperature, high safety and energy saving, is suitable for mass production, and has a better application prospect.

The invention discloses a preparation method of difluoro-sulfonyl imide lithium. The preparation method comprises the following steps: 1) under a protective atmosphere, adding a fluorizating agent into difluoro-sulfonyl imide to perform a fluorination reaction so as to obtain a mixture, wherein the fluorizating agent is one of or a combination of fluorine, a fluorine-containing mixed gas, anhydrous hydrogen fluoride, potassium fluoride, antimonic fluoride and rubidium fluoride; 2) performing reduced pressure distillation on the obtained mixture to obtain a di(fluoro-sulfonyl) imide intermediate; and 3) under a protective atmosphere, performing synthetic reaction on the obtained di(fluoro-sulfonyl) imide intermediate and a lithium source, and performing solid-liquid separation to obtain difluoro-sulfonyl imide lithium. According to the preparation method disclosed by the invention, the fluorination reaction does not need a solvent or other auxiliary agent, is less in types of adopted reagents, does not introduce a new impurity, is simple in operation, and is easy to control; the method is less in side reaction, good in fluorination effect and low in fluorination cost; and the purity and the yield of the product namely difluoro-sulfonyl imide lithium obtained by a subsequent synthetic reaction are improved on the whole, and the method has good economic and environmental benefits.

The invention discloses a preparation method of difluorosulfimide salt. The preparation method comprises the following steps: (1) adding dichlorosulfimide and a nitrogen-containing hydrogen fluoride complex which are used as reaction raw materials into an organic solvent for reaction at 0-100 DEG C, and after reaction, distilling to remove the organic solvent to obtain a difluorosulfimide and nitrogen-containing ion compound; (2) adding the ion compound obtained in the step (1) into a water solution of metal alkali or salt, neutralizing until the solution is neutral, distilling, drying, re-crystallizing by using the organic solvent, and purifying to obtain difluorosulfimide salt. According to the preparation method, the nitrogen-containing hydrogen fluoride complex is adopted as a fluorating agent, so that the whole reaction is carried out in a homogeneous system, the fluorating reaction is relatively safe, the efficiency is relatively high, and the product yield is more than 98%; a process route is simple, the yield is high, and the production cost is relatively low.

The invention relates to the field of organic synthesis, specifically to a preparation method for 3,5,-dichloro-2,4,-difluoroaniline and application thereof. The preparation method for 3,5,-dichloro-2,4,-difluoroaniline provided by the invention comprises the following steps: 1) nitration reaction; 2) reduction reaction; 3) diazotization reaction; 4) nitration reaction; 5) fluorination reaction; and 6) reduction reaction. The preparation method for 3,5,-dichloro-2,4,-difluoroaniline provided by the invention has the following beneficial effects: 1) the method has mild reaction conditions, is stable and controllable, has less active sites, is insusceptible to side reaction, and has good yield and quality in the whole line; and 2) raw materials are cheap and easily available, so cost can be effectively reduced, and energy is saved; meanwhile, the use of chlorine gas is avoided, so the method is environment-friendly.

The invention discloses a preparation method 2,4,5-trifluorophenylacetic acid. The method is characterized by consisting of four reaction steps of: A, reaction of 2,4,5-trifluoronitrobenzene (I) and diethyl malonate which are condensed to prepare 2,5-difloro-4-nitrobenzophenone diethyl malonate; B, hydrolysis, acidification and decarboxylic reaction of dibasic ester; C, reduction reaction of nitryl; and D, diazotization fluoridation of amino. The four reaction steps can be sequentially carried out according to A, B, C and D, or A, C, B and D, or A, C, D and B. According to the preparation method provided by the invention, condensation of 2,4,5-trifluoronitrobenzene (I) and diethyl malonate is easy to realize by means of high substituting activity of nitryl p-fluorine, and the raw material 2,4,5-trifluoronitrobenzene (I) is low in cost and easy to obtain and can be easily prepared by nitration and fluorination of 2,4-dichlor fluorbenzene. Compared with the prior art, the preparation method provided by the invention has the characteristics of low-cost and easily obtained raw materials, mild reaction condition, high total yield, low production cost and the like, and is comparatively suitable for industrialized production.

To produce a catalyst having an enhanced fluorination activity in the catalyst used for a fluorination reaction using hydrogen fluoride as a fluorinating agent, and to provide a fluorination method using the catalyst. This catalyst for the fluorination reaction is characterized in that a porous support comprising calcium fluoride or magnesium fluoride is carried with an antimony halogenated substance represented by formula (1): SbFnCl(5-n) (wherein (n) represents a number of 0-5).

The invention relates to a preparation method of imidodisulfuryl fluoride lithium salt. The preparation method comprises the following steps: (1) performing a fluorination reaction of imidodisulfuryl chloride by taking a hydrogen fluoride complex salt as a fluorinating agent in the presence of a solvent, the fluorinating agent and an initiator, performing filter pressing separation at the end of the reaction, distilling filtrate under a reduced pressure to remove the solvent, and rectifying under a reduced pressure to obtain imidodisulfuryl fluoride; (2) reacting the imidodisulfuryl fluoride with a lithium compound at the temperature of 80 to 110 DEG C to obtain a crude imidodisulfuryl fluoride lithium salt. The preparation method provided by the invention has the advantages of easiness in operation of a fluorinating process route, mild conditions, high operability and easiness in implementation of industrial production; the prepared imidodisulfuryl fluoride lithium salt is 99 percent or more in purity, and is suitable for lithium batteries.

The invention provides a fluorinated graphene, and a preparation method and an application thereof. The preparation method of the fluorinated graphene is characterized in that reduced graphene oxide and a fluorinating agent undergo a fluorination reaction at 280-550 DEG C; and the fluorinating agent is a mixed gas of F2 and an inert gas, and the volume concentration of fluorine in the mixed gas is1-10%, preferably 3-10%, more preferably 3-8% and best preferably 3-5%. The reduced graphene oxide is fluorinated and modified with the mixed gas of F2 and the inert gas, so the safety, the stabilityand the controllability of the process are improved, the corrosion of high-purity F2 to a fluorination device is effectively reduced, and the problems of high cost and low fluorination quality in theprior art are solved.

The invention relates to a method for preparing potassium borofluoride through fluorine-containing wastewater. The method is characterized by comprising the following steps: (1) utilizing water to regulate the hydrogen fluoride content of the fluorine-containing wastewater until the mass content of hydrogen fluoride is 12%-17%; (2) completely mixing the wastewater after treatment in the step (1) with potassium chloride saturated solution according to a mass ratio of (3-5):1 so as to fluorate; (3) mixing borax with the wastewater after treatment in the step (1) according to a mass ratio of 1: (3-5), and stirring so as to completely dissolve the borax; mixing solution in the step 2 with solution in the step 3 according to a mass ratio of (0.8-1.2):1, stirring to react, and continuously separating potassium fluoborate out in a reaction process so as to prepare potassium fluoborate suspension; and (5) solid-liquid separating, washing and drying the potassium fluoborate suspension in the step (4) so as to obtain a potassium fluoborate product. The potassium fluoborate product prepared by the method can satisfy the requirements of potassium fluoborate use factories.

Synthesis of 2-chlorine-5-trifluopyridine is carried out by taking 2-chlorine-5-chloromethyl pyridine as raw material, chlorination reacting at 60<=t<80íÒC with azodiisobutyronitrile, phosphorus trichloride and light radiation of iodo-tungsten light as evocator, carbon tetrachloride as organic solvent and below distilling purification 160íÒC and fluoridation reacting. It can be used for pesticide and medicine. Its advantages include simple raw material, low cost, high conversion efficiency, better reaction selectivity and more output.

The invention discloses a fluorinated graphene lubricant additive and a preparing method thereof and a fluorinated graphene lubricant composite material, and relates to the technical field of lubricating materials. The preparing method of the lubricant additive comprises the step of conducting a fluorination reaction after absorbing moisture from graphene oxide. Through the fluorination process ofin-situ catalysis of graphene oxide by the moisture medium in graphene oxide, it is achieved that under the room temperature and the low fluorine gas concentration, fluorinated graphene with low oxygen content, high fluorine content and large interlayer spacing is prepared. The fluorinated graphene lubricant additive is simply mixed with lubricating oil, and does not easily get agglomerated in the lubricating oil, and the fluorinated graphene lubricant composite material with high dispersing stability is prepared. Compared with an original compound material, the friction coefficient is lowered by 52.3%, and the wearing ratio is lowered by 92.5%.

The invention relates to the field of chemical industry, and particularly relates to a method for recycling fluorides in a preparation process of a silicon-containing compound. The method comprises the steps of: mixing a silicon-containing substance with fluoride to generate fluoridation to obtain silicon tetrafluoride gas and oxides of cations in the fluoride; carrying out pyrohydrolysis on the silicon tetrafluoride gas to obtain nanoscale silicon dioxide and hydrogen fluoride gas; reacting the hydrogen fluoride gas with the oxides of cations in the fluoride to obtain fluorides again. In the method for recycling the fluorides, during the whole reaction, fluorine element basically does not have any loss; as reactants, the fluorides are obtained again in the final reaction; and in the preparation of the silicon-containing compound, the fluorides are recycled.

The invention discloses a synthesis method of 3, 4, 5, 6-tetrafluorophthalic acid, comprising the following steps: (1) adding phthalylhydrazine into mixed liquid of fuming sulfuric acid and diluted hydrochloric acid, then adding a catalyst I into the mixed liquid and stirring the mixture, controlling the filling of chlorine, and carrying out a thermal reaction; (2) adding potassium fluoride into a reaction device containing methyl alcohol, methylbenzene and a solvent I, heating up and then stirring the mixture, and carrying out atmospheric distillation on reaction liquid to recover the methyl alcohol and the methylbenzene; after that, under the protection of nitrogen, adding the tetrachloro phthalylhydrazine prepared in the step (1) and a catalyst II into the product, heating up to 120-200 DEG C and carrying out a fluoridation reaction; (3) adding the tetrachloro phthalylhydrazine and sodium peroxide which are prepared in the step (2) into water, carrying out a hydrolysis reaction for 2-8 hours at the temperature of 10-50 DEG C, then adjusting the acidity of the obtained reaction liquid until the pH value of the reaction liquid is equal to 1-4, carrying out suction filtration and drying to obtain the tetrafluorophthalic acid.

The invention relates to the field of chemical industry and specifically relates to a preparation method of nano-scale silicon dioxide. The preparation method comprises the following steps: mixing a silicon-containing substance and a fluoride, and then performing fluorination reaction to obtain gas-phase silicon tetrafluoride; performing high-temperature hydrolysis on the silicon tetrafluoride to obtain the nano-scale silicon dioxide; and performing quenching crystallization on the silicon dioxide to obtain particulate silicon dioxide, wherein the silicon-containing substance comprises mineral containing a silicon metal oxide or waste material containing the silicon dioxide. A reactant adopted in the preparation method provided by the invention is the silicon-containing substance, namely the mineral containing the silicon metal oxide or the waste material containing the silicon dioxide, and the raw material can be bound everywhere and further has the advantages of wide sources, convenience in taking the material and relatively low cost; and furthermore, as silicon is a fluorophilic substance, the silicon is in contact with fluorine to react firstly to generate the gas-phase silicon tetrafluoride, the high-temperature hydrolysis is performed on the silicon tetrafluoride to perform intermolecular reaction to obtain the nano-scale silicon dioxide, and then the quenching crystallization is performed to agglomerate to form the particulate silicon dioxide for collection.

The present invention belongs to fluorination catalyst technology. The catalyst is applied in the haloarene replacing fluorination between the haloarene and fluorinating agent inside sulfolane solution. The present invention features the catalyst being calixarene or its derivative, consumption of 0.01-1 mol and using temperature 80-230 deg.c. Using the catalyst in haloarene replacing fluorination can simplify the technological process, lower the product cost, raise the product yield and purity and simplify post-treatment. The present invention is suitable for industrial production.

A method for preparing a carbon fluoride/fluorinated metal composite material comprises the steps of: carbonizing at least one of the group consisting of copper-based, iron-based, cobalt-based, nickel-based, and manganese-based metal organic framework materials at a high temperature in an inert gas atmosphere, then cooling the organic framework material to room temperature to obtain a composite material precursor; drying the composite material precursor in a reaction vessel, then introducing a mixed gas composed of a fluorine gas and a nitrogen gas, performing a fluorination under a heating condition, and performing vacuum drying to obtain the carbon fluoride/fluorinated metal composite material as a final product. The method is low in raw material cost, easy to operate and liable to industrial production. The fluorinated metal and carbon fluoride composite materials are prepared by an in-situ method. The two materials have high recombination degree, and the composite material has richinner pores and high specific surface area. The fluorinated metal and carbon fluoride composite materials have good chemical stability, high discharge specific capacity and high discharge voltage platform, and can be applied to lithium ion batteries and the like, and have very good application prospects.

The invention discloses a preparation method of trans-1, 2-dichloro-3, 3, 3-trifluoropropene. The method comprises the following steps: a, 1,1,1,2,2,3-hexachloropropane and/or 1,1,1,2,3,3-hexachloropropane are reacted with the existence of diluent gas and a catalyst, a gas-phase reaction is carried out for removing hydrogen chloride, and 1,1,2,3,3-pentachloropropene is produced; b. a liquid phase fluoridation reaction is carried out between 1,1,2,3,3-pentachloropropene and hydrogen fluoride with the existence of a liquid phase fluorination catalyst, or a gas phase fluorination reaction is carried out between 1,1,2,3,3-pentachloropropene and hydrogen fluoride with the existence of a gas phase fluorination catalyst; c. washing, alkali washing and drying are carried out for reaction products in the step b, and trans-1, 2-dichloro-3, 3, 3-trifluoropropene is obtained by rectification in a condition with normal pressure. The method has the characteristics of high reaction selectivity, high conversion rate and high stereoselectivity, and is mainly used for preparing trans-1, 2-dichloro-3, 3, 3-trifluoropropene.

The invention discloses a method for preparing high-purity graphite fluoride according a catalytic method. The method comprises the following steps: pretreatment, fluoridation, off-gas treatment, product collection, graphite fluoride purification and catalyst recovery. Through the addition of metal fluoride as a catalyst, the activation energy of graphite and fluoride reaction is reduced, so that the reaction temperature is greatly reduced. The method disclosed by the invention has the advantages that the reaction temperature is low, the production cost is low, the process is simple, the safety is high, and the fluorine content of the prepared high-purity graphite fluoride can be flexibly changed through adjustment of reaction temperature, pressure and time, so that large-scale industrialized production of graphite fluoride is realized. The metal fluoride catalyst is insoluble in water, and can be separated from graphite fluoride according to a water-deposition method, so that the catalyst is recycled, and the production cost is greatly reduced.

The invention concerns a method for producing 2,3,3,3-tetrafluoropropene comprising: a fluoridation reaction of a halopropane and/or halopropene into 2,3,3,3-tetrafluoropropene by means of hydrogen fluoride; the recovery of a gas stream resulting from the reaction; the cooling and partial condensation of the gas stream resulting from the reaction into a partially condensed stream; the separation of the partially condensed stream into a gas fraction and a liquid fraction; the compression of the gas fraction into a compressed gas fraction; the compression of the liquid fraction into a compressed liquid fraction; the distillation of the compressed gas fraction and compressed liquid fraction in order to provide a stream of 2,3,3,3-tetrafluoropropene, a stream of hydrochloric acid, and a stream of unreacted hydrogen fluoride. The invention also concerns an installation suitable for implementing said method.