72 results about "Hexafluoroacetone" patented technology

The present invention relates to a novel fluorine-containing cyclic compound that is derived from a norbornadiene and hexafluoroacetone and has an oxacyclopentane or oxacyclobutane structure. This compound may be represented by the following formula (1) or (2). Furthermore, the present invention relates to a fluorine-containing high-molecular compound prepared by a polymerization or copolymerization using this fluorine-containing cyclic compound or its derivative. By using such fluorine-containing high-molecular compound, it is possible to provide a superior resist material and a fine pattern forming process using the same.

The invention relates to a biological mineralization method of tussah silk fibroin for promoting cell growth. No existing biological mineralization method capable of preparing the tussah silk fibroin with high biocompatibility is easy to operate and quick. The method sequentially comprises the following steps: pulverizing tussah cocoon, and adding into a Na2CO3 water solution for degumming, thereby obtaining the tussah silk fibroin fiber; adding the tussah silk fibroin fiber into an LiSCN water solution, dissolving, dialyzing, freezing, drying to obtain tussah silk fibroin powder, and dissolving the tussah silk fibroin powder in hexafluoroacetone to obtain a tussah silk fibroin solution; dropwisely adding the tussah silk fibroin solution onto a plastic board, and drying in air to obtain a tussah silk fibroin film; and impregnating the tussah silk fibroin film in a CaCl2 water solution, cleaning with water and acetone, drying in air, and impregnating in an Na2HPO4 water solution, cleaning with water and acetone, drying in air, and repeating the operation 20-35 times, thereby obtaining the finished product. The invention has the advantages of simple technique and short preparation period; and the prepared biological material does not have cytotoxicity.

The present invention relates to a novel fluorine-containing cyclic compound that is derived from a norbornadiene and hexafluoroacetone and has an oxacyclopentane structure. This compound may be represented by the following formula (1) or (2). Furthermore, the present invention relates to a fluorine-containing polymer compound prepared by a polymerization or copolymerization using this fluorine-containing cyclic compound or its derivative. By using such fluorine-containing polymer compound, it is possible to provide a superior resist material and a fine pattern forming process using the same.

The present invention is catalyst for isomerization process of preparing hexafloroacetone and its preparation and application. The catalyst consists of main catalyst component Cr2O3 and / or AlF3, the first co-catalyst component TiO2 and the second co-catalyst component graphite or metal powder. The catalyst is prepared through mechanical mixing, drying and programmed heating to activate. By means of the catalyst, the isomerization process of preparing hexafloroacetone may be completed under normal temperature and normal pressure, can complete rearrangement instantaneously and has no need of inert gas for diluting material. The catalyst has facile material, simple preparation process, high catalytic activity, high operation stability and capacity of preparing high purity hexafloroacetone.

A continuous process for producing hexafluoroisopropanol is provided which comprises contacting hexafluoroacetone with hexafluoroisopropanol and hydrogen to produce a liquid feed stream; introducing the liquid feed stream to a reactor containing an immobilized hydrogenation catalyst to convert the hexafluoroacetone to hexafluoroisopropanol and provide a product stream; and recovering at least a portion of the hexafluoroisopropanol from the product stream. Preferably a portion of the product stream is recycled. The reactor can be a packed bed or stirred tank reactor.

An analytical technique for the accurate and precise measurement of trace water in chemical reagents, comprising the steps of combining a chemical reagent comprising ≦5 ppm water, with hexafluoroacetone (HFA), to form a sample mixture comprising at least the chemical reagent and a water derivative of hexafluoroacetone; and measuring the concentration of the water derivative of hexafluoroacetone by gas chromatography.

The invention discloses a hydrogenation catalyst and a preparation method thereof. The preparation method of the catalyst comprises the following steps: (1) first, preparing a gamma-Al2O3 carrier; (2)loading the gamma-Al2O3 carrier by a Co metal component and a F-containing assistant component, and performing drying and roasting; and (3) performing impregnation on the carrier obtained in the step(2) by adopting a solution containing a Ni-containing compound and a W-containing and / or Mo-containing compound, and performing drying and roasting to obtain the catalyst. The catalyst is prepared byloading the gamma-Al2O3 with active components of Co, Ni and W / Mo, and simultaneously the F-containing compound is used as an auxiliary agent, wherein the F-containing compound is at least one selected from a group consisting of tetrabutylammonium fluoride, trifluoroacetic acid, hexafluoroacetone and hexafluoroisopropanol. The catalyst can be used for hydrofining of light distillate oil such as gasoline fraction, kerosene fraction and diesel fraction, has high hydrogenation desulfurization activity and aromatic saturation activity.

The invention discloses a method for preparing 1,1,1,3,3,3-hexafluoroacetone by gas phase fluorination. The method comprises that 1,1,1,3,3,3-hexachloroacetone as a raw material undergoes a one-step gas phase fluorination reaction in the presence of a fluorination catalyst at a reaction temperature of 300 DEG C to produce 1,1,1,3,3,3-hexafluoroacetone, wherein a mole ratio of hydrogen fluoride to the organic matter is 10: 1 and contact time is 10s. The fluorination catalyst is a ferric compound-loaded catalyst. A preparation method of the fluorination catalyst comprises utilizing alumina, magnesium oxide or calcium oxide as carriers, dipping the carriers in an iron soluble salt and one of soluble salts of metal cocatalysts such as copper, manganese, zinc, nickel, cobalt and lanthanum to obtain a catalyst precursor with a mass ratio of iron to the carriers of 2-20% and cocatalyst content of 0.5-2wt%, and carrying out drying, roasting and HF fluorination. The prepared fluorination catalyst has the characteristics of environment-friendliness, low price, good catalytic activity, good stability and regeneration easiness. The method realizes high-selectivity synthesis of the 1,1,1,3,3,3-hexafluoroacetone.

The invention belongs to the technical field of electronic chemical materials, and more specifically relates to a preparation method for bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The preparationmethod for the bis(3-amino-4-hydroxyphenyl)hexafluoropropane disclosed by the invention comprises the following steps: step 1, introducing hexafluoroacetone into a reactant (I) in the presence of a catalyst for a reaction so as to obtain a compound (II); step 2, allowing the compound (II) obtained in the step 1 with nitric acid and sulfuric acid so as to obtain a compound (III); step 3, adding thecompound (III) obtained in the step 2 into inorganic base for a reaction so as to obtain a compound (IV); and step 4, carrying out catalytic hydrogenation on the compound (IV) obtained in the step 3so as to obtain the bis(3-amino-4-hydroxyphenyl)hexafluoropropane.

The invention discloses a method used for preparing 2,2-bis(3,4-dimethylphenyl)hexafluoropropane. According to the method, 2,2-bis(3,4-dimethylphenyl)hexafluoropropane is obtained via liquid phase reaction of o-xylene with hexafluoroacetone monohydrate under the action of hydrogen fluoride. The raw materials of the method are low in toxicity; reaction pressure is low; operation is convenient; reaction selectivity and yield are high; and the method is suitable for industrialized production. 2,2-bis(3,4-dimethylphenyl)hexafluoropropane prepared via the method can be taken as an intermediate to synthesize fluorine-containing polyimide.

The invention discloses a method for improving mechanical properties of a silk protein membrane by virtue of biological mineralization. The method is realized by the following steps of dissolving an aqueous solution of silk protein or silk protein powder in organic solvents such as hexafluoroacetone, hexafluoroisopropanol and formic acid to obtain a silk protein solution, then dropwises adding the aqueous solution of silk protein or the silk protein solution to a plastic plate and drying to obtain the silk protein membrane. By adopting the method disclosed by the invention. The mechanical properties of the silk protein membrane are significantly improved and the time is greatly saved and the method has the advantages of short production period, simple and efficient extraction process and no complicated and tedious mineralization process and is simple to operate.

The invention discloses a low-toxicity synthesis method of a siloxane gas-sensitive material, which takes liquid 2-ethylenic alkyl hexafluoride isopropyl alcohol as a raw material at the normal temperature, and the siloxane gas-sensitive material can be prepared by the addition reaction between the raw material and hydrogen-containing siloxane under the catalysis of divinyl tetramethyl disiloxaneplatinum coordination, so that hexafluoroacetone which is high in toxicity and is gaseous at the normal temperature can be avoided. The preparation method is simple in method, easy to operate, mild in reaction condition, lower in requirements for experimental facilities and lower in material toxicity, and can simply, practically and efficiently introduce hexafluoro-isopropanol substituent group into silicon hydrogen bond of the hydrogen-containing siloxane.

The invention provides a method for preparing 1,1,1,3,3,3-hexafluoroacetone through gas-phase catalysis, relating to the field of organic synthesis. The method comprises the following reaction steps: (1) introducing 1,1,3,3-tetrafluoro-1,3-dichloroacetone gas and hydrogen fluoride gas into a fixed bed type reactor with a supported catalyst, and reacting; and (2) rectifying the gas discharged from the fixed bed type reactor to obtain the 1,1,1,3,3,3-hexafluoroacetone. According to the method for preparing 1,1,1,3,3,3-hexafluoroacetone through gas-phase catalysis, the tetrafluorodichloroacetone is used as the raw material; and the process is simple and environment-friendly, low in cost and high in yield.

The invention discloses a method for detecting hydrogen by a palladium nanoparticle discrete film. The method comprises the following steps that: palladium hexafluoroacetone (II), formalin, a quartz glass substrate, high-purity nitrogen and a carbon-supporting film are firstly prepared; under a vacuum environment, palladium hexafluoroacetone (II) is introduced into a reaction chamber as a precursor, and chemical absorption and chemical reaction are generated by the precursor of palladium hexafluoroacetone (II) and the surface of the quartz glass substrate; the formalin as a precursor generateschemical reaction with palladium hexafluoroacetone (II) as the precursor combined with the substrate. The method disclosed by the invention has the beneficial effects that the response rate of a sensing film to the hydrogen can be effectively increased, the phase change phenomenon caused by pure palladium in the high-concentration hydrogen can be effectively avoided, the accuracy of detection canbe ensured, and the problems that a palladium-yttrium alloy film in the existing optical-fiber hydrogen sensor is easily poisoned by oxygen in the air to cause foaming and cracking and the like of the film to further cause zero drift and influence the accuracy of hydrogen detection are solved.

The invention discloses a greasy dirt cleansing agent and a preparation method thereof. The greasy dirt cleansing agent is prepared from the following components in parts by weight: 30-55 parts of butyl acetate, 5-7 parts of dimethyl formamide, 4-8 parts of isopropanol, 4-6 parts of bisphenol hexafluoroacetone diglycidyl ether, 1-2.5 parts of adipic acid dihydrazide, 0.5-1 part of 4-vinyl-1-cyclohexene bicyclo-oxide and 80-120 parts of water. The invention also provides a preparation method of the greasy dirt cleansing agent.

An analytical technique for the accurate and precise measurement of trace water in chemical reagents, comprising the steps of combining a chemical reagent comprising ≦5 ppm water, with hexafluoroacetone (HFA), to form a sample mixture comprising at least the chemical reagent and a water derivative of hexafluoroacetone; and measuring the concentration of the water derivative of hexafluoroacetone by gas chromatography.

The invention discloses a synthetic method of perfluoroisobutyronitrile. The synthetic method comprises the following steps of: (1) taking hexafluoropropylene oxide and hexafluoroacetone as raw materials to react to prepare perfluoroepoxyisobutane; (2) carrying out catalytic isomerization on the perfluoroepoxyisobutane to obtain heptafluoroisobutyryl fluoride; (3) carrying out esterification reaction on heptafluoroisobutyryl fluoride and alcohol to obtain heptafluoroisobutyrate; and (4) reacting heptafluoroisobutyrate with ammonia, and performing dehydrating to obtain perfluoroisobutyronitrile. The synthesis method has the advantages of easily available raw materials, low raw material cost, few byproduct, mild reaction conditions, high reaction conversion rate and yield, short synthesis route, simple and safe process and easy industrial production.

The invention relates to a biological mineralization method of tussah silk fibroin for promoting cell growth. No existing biological mineralization method capable of preparing the tussah silk fibroin with high biocompatibility is easy to operate and quick. The method sequentially comprises the following steps: pulverizing tussah cocoon, and adding into a Na2CO3 water solution for degumming, thereby obtaining the tussah silk fibroin fiber; adding the tussah silk fibroin fiber into an LiSCN water solution, dissolving, dialyzing, freezing, drying to obtain tussah silk fibroin powder, and dissolving the tussah silk fibroin powder in hexafluoroacetone to obtain a tussah silk fibroin solution; dropwisely adding the tussah silk fibroin solution onto a plastic board, and drying in air to obtain a tussah silk fibroin film; and impregnating the tussah silk fibroin film in a CaCl2 water solution, cleaning with water and acetone, drying in air, and impregnating in an Na2HPO4 water solution, cleaning with water and acetone, drying in air, and repeating the operation 20-35 times, thereby obtaining the finished product. The invention has the advantages of simple technique and short preparation period; and the prepared biological material does not have cytotoxicity.

The invention discloses a method for improving mechanical properties of a silk protein membrane by virtue of biological mineralization. The method is realized by the following steps of dissolving an aqueous solution of silk protein or silk protein powder in organic solvents such as hexafluoroacetone, hexafluoroisopropanol and formic acid to obtain a silk protein solution, then dropwises adding the aqueous solution of silk protein or the silk protein solution to a plastic plate and drying to obtain the silk protein membrane. By adopting the method disclosed by the invention. The mechanical properties of the silk protein membrane are significantly improved and the time is greatly saved and the method has the advantages of short production period, simple and efficient extraction process and no complicated and tedious mineralization process and is simple to operate.

The invention relates to a preparation method for preparing a novel fluorine-containing bisphenol compound, namely 2, 2-bis (4-(2, 4-diaminophenoxy) phenyl) hexafluoropropane. The preparation method comprises the following steps of lithiating m-dibromobenzene to prepare m-phenyl dilithium salt; performing addition reaction on the m-phenyl dilithium salt and hexafluoroacetone to prepare 1, 3-bis (2-hydroxy-hexafluoropropylidene) benzene; and performing condensation reaction on the 1, 3-bis (2-hydroxy-hexafluoropropylidene) benzene and phenol to prepare 1, 3-bis (1-(4-hydroxyphenyl)-hexafluoropropylidene) benzene. The preparation method provided by the invention has the advantages of simplicity in operation and low cost, the purity of the obtained product is more than 99%, and the preparation method is suitable for industrial production.

The invention discloses a preparation method of 1,1,1,3,3,3-hexafluoro-2-(4-styrene)propanol. According to the preparation method, phenylethenyl magnesium chloride Grignard reagent is reacted with hexafluoroacetone at a low temperature, and an obtained product is subjected to washing and refining so as to obtain a finished product with a content of 99.0% or higher. Cheaper raw materials are adopted in the preparation method, the raw materials are safer for storage, transportation, and using, and requirement on operator protection and equipment is low; the preparation method is more reasonable, safe, simple, low in energy consumption, high in yield, and low in environmental pollution; the finished product is a high-activity organic intermediate with a fluorine double bond structure, augmented products of the finished product are more, application range is extremely wide, and market prospect is promising; an obtained three wastes byproduct is magnesium chloride which is an excellent flame-resistant material in the field of building material, and can be recycled; and three wastes processing of chlorine-containing waste water is convenient, and less pollution on the environment is caused.

The invention relates to a chiral rare earth-nitroxyl radical single-chain magnet and a preparation method thereof. A chemical reaction of the single-chain magnet is [Dy(hfac)3((1R)-(-)-Myrtenal-NIT)]n, wherein n is a natural number from 1 to positive infinity. The preparation method comprises the following steps: a hexane solution of hexafluoroacetone dysprosium is backflowed for 2 hours, a dichloromethane solution of (1R)-(-)-Myrtenal-NIT is added for a reaction for several minutes, and room-temperature volatilization is carried out to obtain a target product. A simple chemical synthesis iscarried out to prepare a chiral rare earth-nitroxyl radical complex, the complex presents zero-field slow-magnetic relaxation behavior, and hysteresis loop is realized. The chiral single-chain magnetmaterial has latent application value on high-density information storage, a quantum computer and a spin-electron device, and correlation and mutual influence between chirality and magnetic phenomenoncan be understood for people.

Disclosed is a method for producing a hexafluoroisopropanol, including the steps of (a) purifying a mixture containing hexafluoroacetone and at least 1,1,1-trifluoro-2,2-dichloroethane as an impurity, thereby obtaining a purified hexafluoroacetone containing 120 ppm or lower of the 1,1,1-trifluoro-2,2-dichloroethane; and (b) bringing hydrogen (H2) into contact with the purified hexafluoroacetone in the presence of a catalyst, thereby hydrogenating the hexafluoroacetone into the hexafluoroisopropanol. It is possible by this method to produce the hexafluoroisopropanol with a short reaction time and a high conversion. Therefore, it is possible to particularly advantageously produce fluoromethyl hexafluoroisopropyl ether (sevoflurane) by using the hexafluoroisopropanol produced by the method.

The invention discloses a novel process for synthesizing hexafluoroacetone. The novel process comprises the following steps: reacting trifluoroacetic anhydride with a metal fluoride in a solvent to obtain trifluoroacetyl fluoride, adding an alkaline salt and trifluoroacetate, and carrying out a coupling reaction on trifluoroacetate and trifluoroacetyl fluoride to obtain the product hexafluoroacetone. The product yield is 95% or above, and the product purity is higher than 96%.

The invention belongs to the technical field of hexafluoroisopropanol, and particularly relates to a preparation method of hexafluoroisopropanol, which comprises the following steps: 1, proportionally pouring hexafluoroacetone water and hexafluoroisopropanol into a temperature stirring device, and heating the stirring device in the stirring process at the heating temperature of 90-150 DEG C; 2, mixing hexafluoroacetone water with hexafluoroisopropanol, then adding a catalyst into the temperature stirring equipment, and heating the interior of the temperature stirring equipment; 3, introducing a mixed gas of hydrogen and nitrogen into the temperature stirring equipment; and 4, carrying out pressure relief on the interior of the temperature stirring equipment, discharging internal gas after the internal gas passes through filtering equipment, and then introducing a liquid mixture in the temperature stirring equipment into the reaction equipment for reaction, so as to prepare hexafluoroisopropanol.

The invention discloses a method for preparing hexafluoroisobutene through environment-friendly visual light catalysis. The method comprises the steps that 1, a photocatalyst is added into a transparent container, oxygen inside the transparent container is removed and placed into a low-temperature dry ice bath, and under the vacuum state, hexafluoroacetone and ketene are added and stirred to be uniform; 2, under the stirring condition, visual light is used for irradiating a reactant in step 1; 3, the hexafluoroisobutene product is obtained through rectification separation refining. The initiator hexafluoroacetone is a commercialized product, and is easy to obtain and low in cost; photocatalysis is adopted for preparation, and environment-friendliness is achieved; due to one-step preparation, the technological process is simple; adopted raw materials and reactants are easy to separate, and purification is easy.

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of bis (3-amino-4-hydroxyphenyl) hexafluoropropane. The preparation method comprises the following specific steps: S1, in the presence of a catalyst A, reacting a general formula I with hexafluoroacetone to obtain a general formula II; s2, in the presence of a catalyst B, reacting the general formula II with the general formula III to obtain a product. The invention solves the problems that the production process of bis (3-amino-4-hydroxyphenyl) hexafluoropropane is strict and the actual yield of the product is low in the prior art, and realizes the industrial production method of bis (3-amino-4-hydroxyphenyl) hexafluoropropane, which is more environment-friendly and safer than the prior art. Bis (3-amino-4-hydroxyphenyl) hexafluoropropane which is high in yield and purity and easy to purify is obtained under mild reaction conditions, and the method can promote production of structural materials in the fields of precision machinery, aerospace materials and the like.

The invention discloses a method for analyzing and determining the content of hexafluoroacetone. Hexafluoroacetone is subjected to gas chromatographic analysis, the content of hexafluoroacetone is directly and quantitatively determined by an area normalization method, and chromatographic conditions during detection are as follows: a chromatographic column is a non-polar column; the temperature ofa chromatographic column is 40-200 DEG C; the temperature of a sample inlet is 60-140 DEG C; the temperature of a detector is 250 to 300 DEG C; the carrier gas is high-purity nitrogen; the flow rate of carrier gas is 0.8 mL / min to 1.5 mL / min; the split ratio is (30-100): 1; the operation time is 20 min, and the pre-column pressure is 13 Psi; and the sample size is 0.1 to 1.0 mL. And the detector is a hydrogen flame detector. The chromatographic analysis method for directly and quantitatively determining the purity of hexafluoroacetone in production has the advantages of reliable result, simpleoperation and low test price, is suitable for routine analysis of enterprises, has high practical value, and can be used for guiding the research and production process detection of hexafluoroacetone.

The invention discloses a method for preparing hexafluoroacetone by taking perfluoropropylene oxide as a raw material. The method comprises the following steps: adding the perfluoropropylene oxide, acatalyst and water into a reaction kettle according to a weight ratio of 1: (0.1-0.5): (1-5), carrying out isomerization reaction at 10-80 DEG C for 1-5 hours, and distilling and purifying to obtain the hexafluoroacetone, wherein by condensing substituted phenol and Merrifield resin, and mixing and compounding with a carrier, the catalyst is obtained. According to the method, the Merrifield resinloaded substituted phenol is used as the catalyst for the first time, and is applied to the method for preparing the hexafluoroacetone by taking the perfluoropropylene oxide as the raw material, so that a new preparation thought is provided, and particularly for fluorine chemical enterprises, self-produced intermediate products can be fully utilized. The raw materials of the catalyst are easy to obtain, the cost is low, and the economic benefit is good; the catalyst is simple in preparation process and mild in preparation condition. The yield of the hexafluoroacetone reaches 95% or above, theoperation is safe, and the catalyst can be continuously used.

The invention provides a method for preparing hexafluoroacetone by perfluoroisobutylene or alcohol absorption liquid of the perfluoroisobutylene. The method sequentially comprises the following steps: firstly, in a reaction medium, the alcohol absorption liquid of the perfluoroisobutylene is reacted with tertiary amines to form middle stable state tetraalkylammonium salt of alcohol hexafluoroisobutene; secondly, nitrite of alkali metal or alkaline earth metal is dispersed in the reaction medium; thirdly, the obtained middle stable state tetraalkylammonium salt of the alcohol hexafluoroisobutene is mixed with dispersion liquid of the nitrite of the alkali metal or the alkaline earth metal to react to form oxime hexafluoroacetone; and fourthly, the oxime hexafluoroacetone is reacted with inorganic acid to form the hexafluoroacetone.