52 results about "Caesium fluoride" patented technology

The invention relates to brazing aluminum steel and a cesium and rubidium containing brazing flux thereof and belongs to the field of brazing materials in non-metal materials. The brazing flux comprises, by a mole ratio, 0.01 mol to 0.56 mol of rubidium fluoride (RbF), 0.15 mol to 0.58 mol of cesium fluoride (CsF), 0.001 mol to 0.25 mol of aluminum oxide (Al2O3), 0.001 mol to 0.2 mol of potassium fluoride (KF), 0.002 mol to 0.05 mol of gallium fluoride (GaF3), 0.001 mol to 0.025 mol of lithium fluoride (LiF), 0.001 mol to 0.025 mol of boron fluoride (BF3), and the balance aluminum fluoride (AlF3). According to the brazing aluminum steel and a cesium and rubidium containing brazing flux thereof, brazing technical requirements of aluminum to aluminum, aluminum to copper, and aluminum to steel can be simultaneously met, and the high-activity novel soldering flux is achieved.

The invention discloses a caesium rubidium soldering flux containing gallium oxide, belonging to the brazing material field of non-metallic materials. The caesium rubidium soldering flux containing gallium oxide is characterized in that the caesium rubidium soldering flux containing gallium oxide comprises the following components in proportion in mole number: 0.12-0.5 mole of rubidium fluoride (RbF), 0.12-0.5 mole of cesium fluoride (CsF), 0.001-0.2 mole of aluminium oxide (Al2O3), 0.001-0.02 mole of potassium fluoride (KF), 0.0001-0.02 mole of gallium oxide (Ga2O3), and 0.159-0.479 mole of aluminium fluoride (AlF3). According to the caesium rubidium soldering flux containing the gallium oxide, the requirement on brazing the aluminium-copper, the aluminium-steel and the aluminium-aluminium can be satisfied simultaneously and the caesium rubidium soldering flux containing gallium oxide has high activity.

The invention discloses a self-brazing material for welding an aluminum-copper member. The self-brazing material comprises the following components: 12-15 percent of fluoride (30-80 percent of aluminum fluoride, 5-35 percent of caesium fluoride and the balance of potassium fluoride), 0.01-0.3 percent of hafnium, 0.01-0.8 percent of germanium, 0.05-2 percent of nickel, 0.8-3 percent of copper, 5-17 percent of silicon and the balance of aluminum. The self-brazing material is prepared through the following steps of: smelting and atomizing the raw materials of hafnium, the germanium, the nickel, the copper, the silicon and the aluminum in a vacuum furnace into fine powder; and then uniformly mixing with the fluoride, pressing into a composite ingot, directly extruding the composite ingot into a yarn or pipe, and winding the yarn into a coil or cutting the pipe into a ring to obtain the self-brazing material. The self-brazing material disclosed by the invention has the advantages that trace elements of Ge and Hf are introduced on the basis of the traditional Al-Si-Cu-Ni alloy system brazing material, so that the brazing material smelting temperature is lowered, the burning loss of an aluminum base material during welding is favorably avoided, the strength and plasticity of the brazing material are improved, the mechanical property of a brazing joint is favorably improved, and the improvement of the plasticity of the brazing material can ensure that the production efficiency is increased.

The invention discloses a synthesis method of 2,3-difluoro-5-chloropyridine, and the method comprises the following steps: in organic solvent, adopting 2,3,5-trichlopyridine and potassium fluoride asraw materials and tetraphenylphosphonium bromide or tetrabutylphosphonium bromide as phase transfer catalyst, keeping temperature at 180-190 DEG C for 5-10h under the protection of inert gas and keeping temperature at 200-210 DEG C for 10-15h to prepare 2,3-difluoro-5-chloropyridine. The synthesis method of 2,3-difluoro-5-chloropyridine of the invention adopts cheap and accessible potassium fluoride as fluorinating agent and adds phase transfer catalyst and controls the reaction temperature to prepare high yield 2,3-difluoro-5-chloropyridine, thus avoiding to use more expensive fluorinating agent such as caesium fluoride and the like and solving the defect that the yield of the reaction that potassium fluoride is directly used to perform fluorination is low. The method of the invention hassimple operation and is applicable to the large-scale production of 2,3-difluoro-5-chloropyridine.

The invention relates to the field of brazing materials, in particular to fluoride brazing flux for copper-aluminum dissimilar metal and a preparation method for the fluoride brazing flux. The fluoride brazing flux consists of cesium fluoride, aluminum trifluorid, potassium fluoride, copper difluoride and assistant. The preparation method comprises the following steps: mixing the cesium fluoride, the aluminum trifluorid, the potassium fluoride, the copper difluoride, zinc difluoride and lithium fluoride powder with zinc powder or ZnAl alloyed powder in proportion, adding a proper amount of deionized water and grinding in a mortar to form paste, and then, drying and grinding.

The invention relates to medium-temperature type anti-corrosion fluoroaluminate soldering flux and a preparation method thereof. The soldering flux takes lithium-settling mother liquor obtained by extracting lithium from Jiangxi lepidolite as a base solution; the base solution is subjected to impurity removal to obtain a solution rich in k, Rb and Cs as a raw material solution; one or more of aluminum fluoride, potassium fluoride, rubidium fluoride and cesium fluoride are dosed and added to prepare mixed type soldering flux; the added metal salts can be extracted from the lepidolite. The lepidolite is rich in rubidium and cesium, so that the production cost of the novel soldering flux is greatly reduced, and the Jiangxi lepidolite realizes resource maximum utilization. The medium-temperature type anti-corrosion fluoroaluminate soldering flux is suitable for welding aluminum alloy and high-magnesium alloy, and has special activity on alloy with high magnesium content.

The invention belongs to the technical field of fine chemicals and related chemistry, and provides an efficient preparation method of a 1-aryl-4-butene compound. The 1-aryl-4-butene compound can be obtained by taking halogen-containing methyl aromatic hydrocarbon and derivatives thereof as raw materials, taking cesium fluoride as an alkali in the presence of a palladium catalyst and a ligand and reacting with allyl boronic acid pinacol ester for 12 hours at the temperature of 80-100 DEG C under the condition of an anhydrous organic solvent. The method has the beneficial effects that the selectivity is high, the reaction conditions are mild, the operation is simple and convenient, the possibility of industrialization is realized, and the 1-aryl-4-butene compound is obtained at a relativelyhigh yield; the 1-aryl-4-butene compound synthesized by the method can be further functionalized to obtain various compounds, and is applied to development and research of natural products, functionalmaterials and fine chemicals.

The invention relates to a method for preparing chlorine fluorine cyclopentene isomeride in the formula (II) (please see the formula in the specification). The chlorine fluorine cyclopentene isomeride is obtained with chlorine fluorine cyclopentene in the formula (I) (please see the formula in the specification) as the raw material in solvent dimethylformamide, dimethyl sulfoxide or sulfolane by conducting an isomerization reaction in catalysts ammonium fluoride, ammonium bifluoride, potassium fluoride, lithium fluoride, sodium fluoride, rubidium fluoride or cesium fluoride. The technological method is little in raw material toxicity and mild in reaction conditions, the reaction is easy to control, the isomeride yield of chlorine fluorine cyclopentene is high, and industrialization is easy.

The invention relates to a method for preparing halogenated pentacyclic olefin by gas-phase isomerization reaction. The method comprises the following steps of: by adopting the halogenated pentacyclic olefin C5HxFyClz as a material, under the existence of an isomerization catalyst, generating the gas-phase isomerization reaction to obtain isomers of the halogenated pentacyclic olefin, wherein X is an integer from 0 to 2, Y is an integer from 4 to 7, Z is an integer from 0 to 4, the sum of X and Y and Z is 8, and the isomerization catalyst is prepared by adopting at least one of lithium fluoride, potassium fluoride, sodium fluoride, rubidium fluoride or cesium fluoride as an active component and loading the active component on at least one of carriers such as aluminium fluoride, magnesium fluoride, iron fluoride, chromium fluoride and zinc fluoride. The method has the advantages that the material is easy to obtain, the isomerization catalyst is low in price, the yield of the isomer is higher, and the method is applicable to large-scale preparation of the isomers of the halogenated pentacyclic olefin by gas-phase reaction.

The invention relates to a corrosion-free soldering flux used for braze welding aluminium and aluminium alloy. Counted by weight percentage, the soldering flux used for braze welding the aluminium and aluminium alloy comprises the following components: 32.0-34.0 percent of cesium fluoride, 44.0-46.5 percent of aluminium fluoride, 20.5-23.5 percent of potassium fluoride, 0.5-2.5 percent of one, two or three materials selected from tin fluoride, zinc fluoride and lithium fluoride. The corrosion-free soldering flux of the invention has low melting point and better soldering performance.

The invention discloses a synthesis method of 2,3-difluoro-5-chloropyridine, and the method comprises the following steps: in organic solvent, adopting 2,3,5-trichlopyridine and potassium fluoride as raw materials and tetraphenylphosphonium bromide or tetrabutylphosphonium bromide as phase transfer catalyst, keeping temperature at 180-190 DEG C for 5-10h under the protection of inert gas and keeping temperature at 200-210 DEG C for 10-15h to prepare 2,3-difluoro-5-chloropyridine. The synthesis method of 2,3-difluoro-5-chloropyridine of the invention adopts cheap and accessible potassium fluoride as fluorinating agent and adds phase transfer catalyst and controls the reaction temperature to prepare high yield 2,3-difluoro-5-chloropyridine, thus avoiding to use more expensive fluorinating agent such as caesium fluoride and the like and solving the defect that the yield of the reaction that potassium fluoride is directly used to perform fluorination is low. The method of the invention has simple operation and is applicable to the large-scale production of 2,3-difluoro-5-chloropyridine.

The invention provides a synthesis method of a triphenylene compound. By taking 2-(trimethylsilyl)phenyl trifluoromethane sulfonate as a benzyne precursor, cesium fluoride as an alkali and 18-crown-6-ether as a phase transfer catalyst, a reaction of the precursor with 9-fluorenone oxime under the condition of no additional metal catalyst is realized through a one-pot process reaction. The reactioncondition is mild and easy to realize, the reaction overcomes the defect that transition metal or noble metal catalysts are required to be added in the previous reaction, and a brand-new way is provided for developing the triphenylene compound.

The invention provides a ferrocenyl-containing arylamine compound and a synthesis method thereof. A trifluoromethanesulfonic acid-2-(trimethylsilyl) phenyl ester compound is used as a benzyne precursor, cesium fluoride is used as an alkali, 18-crown-6-ether is used as a phase transfer catalyst, and a ferrocenyl arylamine structural unit is efficiently constructed through a one-pot reaction under the condition of no additional metal catalyst. The reaction overcomes the defects that a transition metal or noble metal catalyst needs to be added in the conventional reaction, the requirements on a substrate and reaction conditions are harsh and the like, the reaction is simple in substrate synthesis, reagents are easy to obtain, target molecules are obtained simply and quickly with high atom economy, and a brand-new way is provided for developing the ferrocenyl-containing arylamine compound.

The invention relates to a synthesizing method for an N, N-double substitution-3-amino isoxazole-5-methanol compound, and mainly solves the technical problems of long procedure, rigorous reaction conditions, toxic reagent using and the like in the conventional synthesis method. The synthesizing method for N, N-double substitution-3-amino isoxazole-5-methanol compound in the invention comprises the steps as follows: under the action of cesium fluoride, 3-bromine isoxazole-5-methenol 1 and an amine compound 2 are directly subjected to substitution reaction on a solvent-free condition to generate the N, N-double substitution-3-amino isoxazole-5-methanol compound 3. The reaction formula is as follows: the amine compound in one of pyrrolidine, piperidine and 4-methylpiperidine.

The present invention discloses a synthesis process of (4R,6S,E)-2-{6-[2-[4-(4-fluorophenyl)-6-isopropyl-2-(N-methyl (methylsulfonyl) amino) pyrimidin-5-yl] ethenyl]-2,2-dimethyl-1,3-epoxyhexane-4-yl} acetate alkyl ester. With an aprotic polar solvent as solvent, 4-(4-fluorophenyl)-6-isopropyl-2-(N-methyl-N-methanesulfonyl amino)-5-pyrimidine methyl, n-butyl lithium, 2,2,6,6-tetramethyl piperidine or LDA react with trimethyl silicon chloride; and then the reaction products react with (4R-cis)-6-[(acetyloxy) methyl]-2,2-dimethyl-1,3-dioxo hexane-4-alkyl acetate under catalysis of cesium fluoride in an aprotic polar solvent to produce the target product. The process uses trimethyl silicon as a condensation agent, and does not use alkali; the cesium fluoride is directly used as a catalyst; and the usage amount and three wastes are less. Z type condensation ethylenic bond is less than 10%, which is much less than the triphenylphosphine process. The reaction process does not need low temperature, is easy to realize industrialization and has the advantages of easily available raw materials and low cost.

The invention relates to the field of brazing materials, in particular to a fluoride flux for copper-aluminum dissimilar metals and a preparation method thereof, which consists of cesium fluoride, aluminum trifluoride, potassium fluoride, copper difluoride and additives; Cesium fluoride, aluminum trifluoride, potassium fluoride, copper difluoride, zinc difluoride, lithium fluoride powder and zinc powder or ZnAl alloy powder are mixed in proportion, and an appropriate amount of deionized water is added and ground in a mortar until Paste, then dried and ground.

The invention provides a synthesis method of 1,1,2-trichloro-3-fluoropropylene, comprising the following step: in the presence of a polyalcohol solvent, carrying out a reaction on 1,1,2,3-tetrachloropropene and an alkali metal fluoride at 90-120 DEG C for 1.0-10h to obtain 1,1,2-trichloro-3-fluoropropylene. The molar ratio of the alkali metal fluoride to 1,1,2,3-tetrachloropropene is (1-5):1, wherein the alkali metal fluoride is sodium fluoride, potassium fluoride or cesium fluoride; and the polyalcohol is glycol, 1,2-propanediol, 1,3-propanediol, 2,3-butanediol, diethylene glycol, triethylene glycol, tetraethylene glycol or glycerol. The synthesis method provided by the invention is mainly applied to preparing 1,1,2-trichloro-3-fluoropropylene.

The invention discloses a low-melting-point high-transference-number electrolyte material for a fluorine ion thermal battery and a preparation method thereof.The preparation method comprises the steps that lithium fluoride, sodium fluoride and potassium fluoride are mixed in proportion and subjected to first calcination treatment for 4-6 h at the temperature of 500-600 DEG C, an obtained product is rapidly cooled, and powdery ternary fluoride eutectic salt is obtained; mixing cesium fluoride with the ternary fluoride eutectic salt in proportion, performing secondary calcination heat treatment for 4-6 hours at the temperature of 600-700 DEG C, and then quickly cooling to obtain powdery quaternary fluoride eutectic salt; and mixing the quaternary fluoride eutectic salt with magnesium oxide of which the mass is 0.8-1.2 times that of the quaternary fluoride eutectic salt, carrying out third calcination treatment at 400-600 DEG C for 3-5 hours, and then rapidly cooling and crushing. By adding the high-atomic-number cation salt, the fluorine ion transference number of the fused salt is improved, the multi-element eutectic salt is obtained, the salt melting point is reduced, the working temperature range of the fluorine ion thermal battery is widened, and the specific energy of the battery is improved.

The invention discloses a preparation method of (S)-2-(adamantane-1-yl)-2-aminoacetic acid hydrochloride, wherein, comprising the following steps: firstly, 1-adamantanecarboxaldehyde and (S) ‑(‑)‑tert-butyl sulfinamide was dissolved in methylene chloride, then slowly adding dehydrating agent and pyridine p-toluenesulfonate, and reacted for 16 hours at a temperature of 20 ° C to obtain tert-butyl sulfinyl imide ; tert-butyl sulfenimide is dissolved in dichloromethane and tetrahydrofuran, trimethylnitrile silane and cesium fluoride are added, and the reaction is carried out at a temperature of 20 ° C for 16 hours to obtain cyanide; use a hydrolysis reagent to hydrolyze cyanide, First react for 6 hours at a temperature of 15°C, and then react at a temperature of 110°C for 16 hours to obtain the final compound, namely (S)-2-(adamantan-1-yl)-2-aminoacetic acid hydrochloride Salt, mainly to solve the technical problem that there is no suitable industrial synthesis method at present.

The invention discloses a preparation method of a 1, 4 enyne compound, which comprises the following steps of in an inert gas atmosphere, adding allyl alcohol, acetylenic acid and a combined catalyst into an organic solvent, and stirring and reacting for 12-24 hours at the temperature of 80-100 DEG C to obtain a reaction solution, wherein the combined catalyst is prepared from organic palladium, villiaumite and cesium fluoride, and the villiaumite is bis (trifluoromethanesulfonimide) salt or bis (trifluoromethanesulfonate), and extracting the reaction solution by using water and ethyl acetate to remove part of the reaction solvent, drying and concentrating an organic phase, and purifying by using a petroleum ether / ethyl acetate developing solvent system through thin layer chromatography to obtain the 1, 4-eneyne compound. The preparation method is simple and convenient to operate, the obtained by-products only comprise water and carbon dioxide, and the method has the advantages of being high in atom economy and environmentally friendly; in addition, the preparation method is low in raw material price and wide in applicable substrate range.

This invention belongs to the field of organic synthesis, and specifically relates to a method for synthesizing 3-indolone. Using N-methylbenzylamine compounds of Formula 1 and methyl 2-fluorobenzoate compounds of Formula 2, in the presence of a strong base (lithium di(trimethylsilyl)amino) and a cesium salt additive (cesium fluoride), and mixed with an organic solvent (methyl tert-butyl ether), 3-indolone of Formula 3 is synthesized. The raw materials used in this invention are simple and readily available, and a one-pot method for synthesizing 3-indolone is constructed, which has advantages such as simple synthesis method, economic and environmental friendliness, and wide applicability.

The invention belongs to the field of fine chemicals and related chemical technologies, and provides a highly efficient preparation method of 1-aryl-4-butene compounds. Using halogen-containing methyl aromatic hydrocarbons and their derivatives as raw materials, in the presence of palladium catalysts and ligands, cesium fluoride as a base, under the condition of anhydrous organic solvents, and allylboronic acid pinacol ester at 80 ° C ~ 1-aryl-4-butene compound can be obtained by reacting at 100°C for 12 hours. The invention has the beneficial effects of high selectivity, mild reaction conditions, easy and convenient operation, the possibility of realizing industrialization, and obtaining 1-aryl-4-butene compounds in a relatively high yield; the 1-aryl-4-butene compound synthesized by the method is Aryl-4-butene compounds can be further functionalized to obtain various compounds, which are applied in the development and research of natural products, functional materials and fine chemicals.

The application discloses a high-activity aluminum brazing flux. The high-activity aluminum brazing flux is composed of 46.0-54.0% of cesium fluoride, 2.5-5.0% of nano aluminum hydroxide, 2.5-5.0% of nano aluminum oxide, 0.02-0.2% of nano rubidium fluoride, 0.0001-0.0002% of nano gallium fluoride, 0.0001-0.0002% of nano gallium oxide and the balance of aluminum fluoride. The spreading area of the brazing flux is increased by 200-280% compared with that of the existing commercially available cesium fluoroaluminate brazing flux, the spreading area of the brazing filler metal is increased by 100-140%, the high-activity aluminum brazing flux can meet the brazing requirements of 'aluminum-steel', 'aluminum-copper' and 'aluminum-aluminum' simultaneously.

The invention discloses a method for preparing 1,4 enyne compounds. In an inert gas atmosphere, allyl alcohol, alkynoic acid and a combined catalyst are added into an organic solvent, and the reaction is stirred at a temperature of 80-100° C. for 12-12 24h, a reaction solution was obtained; the combined catalyst was composed of organic palladium, fluoride salt and cesium fluoride, and the fluoride salt was bis-trifluoromethanesulfonimide salt or bis-trifluoromethanesulfonate; then the reaction solution was passed through water Extraction with ethyl acetate to remove part of the reaction solvent, drying and concentrating the organic phase, and purification by thin layer chromatography with petroleum ether / ethyl acetate developing solvent system to obtain 1,4-enyne compounds. The preparation method of the present invention is simple, the operation is convenient, the obtained by-products are only water and carbon dioxide, and has the characteristics of high atom economy and environmental protection; in addition, the preparation method of the present invention has low price of raw materials and a wide range of applicable substrates.

The application belongs to the field of organic synthesis, and particularly relates to a synthesis method of diaryl acetylene. A toluene compound shown in formula 1 and a methyl benzoate compound shown in formula 2 are mixed with an organic solvent (toluene or dimethyl tetrahydrofuran) in the presence of a strong base (lithium bis(trimethylsilyl)amide), a cesium salt additive (cesium fluoride), an amidine additive (DBU) and an activating agent (Nf-F), and then reacted to synthesize the diaryl acetylene shown in formula 3. The raw material used in the application is simple and easy to obtain, a one-pot synthesis method of the diaryl acetylene is constructed, and the application has the advantages of simple synthesis method, economy, environmental protection and wide application range.

The invention provides a synthesis method of 1,1,2-trichloro-3-fluoropropylene, comprising the following step: in the presence of a polyalcohol solvent, carrying out a reaction on 1,1,2,3-tetrachloropropene and an alkali metal fluoride at 90-120 DEG C for 1.0-10h to obtain 1,1,2-trichloro-3-fluoropropylene. The molar ratio of the alkali metal fluoride to 1,1,2,3-tetrachloropropene is (1-5):1, wherein the alkali metal fluoride is sodium fluoride, potassium fluoride or cesium fluoride; and the polyalcohol is glycol, 1,2-propanediol, 1,3-propanediol, 2,3-butanediol, diethylene glycol, triethylene glycol, tetraethylene glycol or glycerol. The synthesis method provided by the invention is mainly applied to preparing 1,1,2-trichloro-3-fluoropropylene.

The invention relates to the rust resistant method for aluminum coating of carbon steel part, aluminum soldering part and non aluminum soldering part, then installing aluminum part on the surface of the carbon steel part. Sending the assembled part into 200 deg.C-250deg.C drying oven, drying the compound soldering agent sufficiently, then taking into the controllable atmosphere oven for soldering and plating under the protection of the nitrogen, controlling the temperature within 570-615deg.C, soldering aluminum part on the surface of the carbon steel part, with the rest of the surface plated with aluminum, to finish the soldering and plating at one time, with the compound soldering material made of 30%-50% soldering material, 20%-40% soldering agent with the rest being ethandiol solution and the soldering material being Al. 85%-94%,Si: 15%-6%, the rest being microelement, the soldering material being aluminun fluoride 40-75%, and caesium fluoride 25-60%. It can be used to reduce the manufacturing cost.

The invention belongs to the field of catalysts, and particularly relates to a modified silicon dioxide mesoporous catalyst and a preparation method thereof. The preparation method comprises the following steps: (1) dissolving cetyl trimethyl ammonium bromide (CTAB) in distilled water, stirring for 30 minutes at room temperature, and then sequentially adding ammonia water and tetraethoxysilane (TEOS) to obtain a post-mixed solution; 2) adding a cesium fluoride solution and a silver nitrate solution into the mixed solution obtained in the step 1); stirring at room temperature; and 3) adding themixture obtained in the step 2) into a reaction kettle containing a polytetrafluoroethylene lining, crystallizing, taking out the sample, carrying out suction filtration, washing and drying, and carrying out high-temperature roasting in a muffle furnace. In the preparation process of the modified silicon dioxide mesoporous catalyst, due to the fact that one-step synthesis is adopted, cesium fluoride and silver oxide directly enter the skeleton structure of the catalyst carrier, and uniform distribution of cesium fluoride and silver oxide components is guaranteed.

The invention belongs to the technical field of ceramic materials, and in particular relates to a photocurable polysilazane and a preparation method thereof, SiCN ceramics and a preparation method thereof. In the present invention, by using 3-(trimethyloxysilyl)propyl methacrylate as a modifying agent, tetrabutylammonium fluoride, potassium fluoride and / or cesium fluoride are used as catalysts to Silazane is modified to activate the Si-H and N-H bonds of the branch chain under the condition of ensuring the polysilazane main chain is continuous, and then react with the modifier to introduce a photocurable group to obtain a photocurable polysilazane. Curing polysilazane, the photocurable polysilazane of the present invention can be combined with 3D photocuring molding to prepare complex shape embryos, and SiCN ceramics can be prepared after sintering.