178 results about "Trifluoride" patented technology

Novel substituted phenylsulfur trifluorides that act as fluorinating agents are disclosed. Also disclosed are methods for their preparation and methods for their use in introducing one or more fluorine atoms into target substrate compounds.

The present invention relates to one kind of antiseptic active cationic dye and its preparation process. The dye has matrix in anthraquinone structure, active group of sym-triazine monochloride or sym-triazine monofluoride, water soluble group of long carbon chain quaternary ammonium salt structure and the chemical structure as shown. The dye may be used in dyeing and antiseptic finishing of various kinds of fiber and has high antiseptic effect, high color fastness and lasting antiseptic performance. It is prepared through the following steps: dissolving anthraquinone A and sym-triazine trichloride or sym-triazine trifluoride in nitrobenzene solvent, heating, cooling and filtering to obtain intermediate B; dissolving the intermediate B in DMF solvent, adding tertiary amine, heating to react, evaporating DMF and vacuum drying to obtain intermediate D; dissolving the intermediate D in DMF solvent, adding alkyl halide, heating to react, washing with ethyl ether, re-crystallizing and drying.

A process for preparing the superfine particles of high-purity cerium trifluoride includes proportionally mixing Cyanex 923 with diluent chosen from hexane, pentane, octane, etc to obtain composite extractant, extracting the Ce and F contained RE sulfate solution, washing and back extracting by strip liquid chosen from hydrogen peroxide, hydrazine hydrate, hydroxyamine hydrochloride, etc. Its purity is 99.9-99.999%.

The invention discloses a method for preparing a chiral cylopropyl acetenyl tertiary alcohol compound.The steps of the method are as follows: (a) cylopropyl ethylnen or other derivatives react with a chiral induction reagent, a chirality auxiliary reagent and zinc halide in an organic solvent under the action of an alkaline reagent so as to obtain a zinc complex; (b) addition reaction is carried out between the obtained zinc complex and 5-chlorin-2-amino trifluoro-benzophenone; (c) (S)-2-amino-5-chlorin-alpha-cylopropyl ethylnen-alpha-benzyl alcohol trifluoride is collected from reaction liquid. Compared with butyl lithium and diethylzinc, the alkaline reagent adopted in the invention is safer; in addition, the cheap zinc halide is used as a ligand, which greatly reduces the cost. Therefore, the method is suitable for industrial production.

New methods for producing difluoromethylene-containing compounds with phenylsulfur trifluoride or a primary alkyl-substituted phenylsulfur trifluoride are disclosed. Also, new methods for producing trifluoromethyl-containing compounds with phenylsulfur trifluoride or primary alkyl-substituted phenylsulfur trifluoride are also disclosed.

The invention discloses a Ti<3+>:TiO2 / TiF3 composite semiconductor photocatalyst. According to the photocatalyst, the diameter of titanium dioxide is 10-20nm, the diameter of titanium fluoride is 100-150nm, a type II heterojunction is formed by titanium dioxide and titanium trifluoride, and the photocatalyst has low carrier recombination efficiency, contains lots of trivalent titanium, has high visible light absorption capacity and can be used for degrading organic pollutants. The invention also discloses a method for preparing the composite semiconductor photocatalyst. Elemental zinc serves as a reducing agent, titanium tetrachloride and titanium tetrafluoride serve as raw materials, and Ti<3+>:TiO2 / TiF3 with different ratios of titanium dioxide to titanium trifluoride can be prepared by changing the amount of elemental zinc in different reactions by utilizing alcohol-thermal method synthesis. The preparation method has the advantages of simplicity in operation, low cost and mild synthesis conditions and has high commercial application prospects.

The invention relates to a method for producing enriched boric-10 acid from a trifluoride-anisole complex and application thereof. The method comprises the following steps: reacting a boron trifluoride-anisole complex with excessive sodium methoxide methanol solution, operating in an ice bath for 5-25 minutes, carrying out thermostatic water bath, reacting for 40-60 hours while keeping the reaction temperature within the range of 40-60 DEG C, stopping heating, and carrying out centrifugal stratification; fractionating the centrifugated supernatant: heating the mixture, starting to collect the fraction when the temperature rises to 50 DEG C, and stopping collecting the fraction when the temperature rises to 60 DEG C; and carrying out salting-out stratification on the collected fraction, mixing with deionized water, carrying out vacuum filtration on the mixture to obtain a solid, and drying to obtain the boric acid. The enriched boric-10 acid is used in the field of production of 10B-isotope-enriched downstream boric acid products, nuclear-grade boric acids and other enriched boric-10 acids by an anisole chemical exchange fractionation process. The production raw materials are from a closed system; and the invention has the impurity removal link, so the product purity is higher, thereby lowering the difficulty of subsequent boric acid production.

The invention discloses a method for industrial production of a sorafenib tosylate polymorphic substance I. The method comprises the following steps: by adopting N-methyl-4-chloro-pyridine carboxamide and p-aminophenol as raw materials, adding a proper amount of alkali to obtain an intermediate 4-(4-aminophenoxy)-N-methyl-2-pyridine carboxamide by virtue of nucleophilic substitution reaction in an organic solvent, performing condensation on 4-(4-aminophenoxy)-N-methyl-2-pyridine carboxamide and 4-chloro-3-benzenyl trifluoride isocyanate to obtain free alkali of sorafenib, finally performing back-flow and salification with p-toluenesulfonic acid in a mixed solvent of acetone and acetonitrile, and cooling and crystallizing to obtain sorafenib tosylate of the polymorphic substance I. Compared with the prior art, the scheme of the method disclosed by the invention is simple and safe to operate, is mild in reaction condition, and does not need crystal form transformation steps; an obtained product is single and stable in crystal form and high in purity, and is suitable for large-scale industrial production.

This invention discloses the method for separating cerium and recovering fluorine and preparing ultramicro-powder cerium trifluoride. In this invention method, bastnasite ore or the mixture containing bastnasite ore and eremite ore is used as raw material mixed with sulfuric acid or nitric acid or the mixture containing both in optional ratio. The extractant is the mixture containing EXTR1 and EXTR2. Said EXTR1 is trialkyl phosphine oxide or dimethyl heptyl methyl-phosphonate or tritutyl phosphate; and said EXTR2 is di(2-ethylhexyl) phosphate, or mono 2-ethyl-hexyl 2-ethyl-hexyl-phosphonate, or di (2,4,4-trimethyl pentyl) phosphonate. The diluent is paraffine or sulfonated kerosene. The products of Ce3+ and cerium trifluoride are obtained after the loading organic phase is proceeded washing and back-extraction. The purity of the cerium trifluoride is 99.9-99.999%, and the grain size distribution is 40-300nm, the recovery rate of cerium is greater than 95%, and fluorine than 98%.

The invention discloses a preparation method of a biphenyl triphosphane ligand and an application thereof in hydroformylation reaction. The prepared biphenyl triphosphane ligand has the structure shown as a formula (I) or formula (II) described in the specification. In the formula (I), aryl substituent Ar is benzene, p-methyl benzene, m-benzenyl trifluoride, p-benzenyl trifluoride, 3, 5-dibenzenyl trifluoride, 3, 5-difluorobenzene, 3, 5-dimethyl benzene, 3, 5-di-tert-butyl benzene, 3, 5-di-tert-butyl-4-metoxybenzene, p-metoxybenzene, p-dimethylamino benzene, 2-pyridine, p-fluorobenzene or 2, 3, 4, 5, 6-pentafluoro benzene; in the formula (II), R is in a cyclic phosphonate structure. The biphenyl triphosphane ligand disclosed by the invention can be used as a linear hydroformylation reaction catalyst, so that the selectivity and reaction rate of hydroformylation reaction can be remarkably improved. The biphenyl triphosphane ligand is low in cost and has a huge practical value.

The invention relates to a matrix material for MALDI, in particular to application of fluoride nanometer materials as a matrix in MALDI-MS. The fluoride nanometer materials are nano-particles with various shapes of ytterbium trifluoride, lanthanum trifluoride, cerium trifluoride, praseodymium trifluoride, neodymium trifluoride, samarium trifluoride, europium trifluoride, gadolinium trifluoride, terbium trifluoride, dysprosium trifluoride, holmium trifluoride, erbium trifluoride, thulium trifluoride, ytterbium trifluoride or lutetium trifluoride, or nano-particles of trifluorides compounded byany two or more of ytterbium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium or lutetium in any proportion. The invention takes rare earth fluoride nanometer materials as the matrix of the MALDI-MS for the first time, develops the matrix of the MALDI-MS with simple and convenient operation and strong universality, and realizes the quick and accurate analysis of the MALDI-MS.

The process of preparing cerium trifluoride micro powder with neutral phosphorus extracting system adopts the material solution of RE sulfuric acid and / or nitric acid solution containing Ce(IV) and F and with acidity of 0.2-6.0 mol / L; extractant comprising Cyanex923 and one or several of TBP, P350, PBBP, DEHEHP, ODOP, Cyanex921, Cyanex925, Cyanex471 and TOEDPO in arbitrary proportion; diluting solvent of n-hexane, n-heptane, octane, noane, decane or sulfonated kerosene to constitute extracting composition together with the extractant; and the back extracting solution of hydrogen peroxide, hydrazine hydrate, hydroxylamine hydrochloride or their mixture with sulfuric acid and / or nitric acid. The extracted composition is washed and back extracted to obtain the cerium trifluoride micro powder with purity of 90-99.9999 % and granularity of 1-4000 nm.

The invention discloses a preparing method by using unactivated olefin hydrogen trifluoride methylation and application thereof. The method comprises the following steps: A, adding unactivated olefin I, sodium trifluoromethanesulfonate and a photocatalystIr[dF(CF3)ppy]2(dtbpy)PF6 into a Schlenk tube; B, vacuumizing, replacing argon, adding methyl alcohol; C, irradiating the Schlenk tube with a fluorescent lamp, and stirring to react; and D, after reaction is finished, adding water into the system to perform a quenching reaction, extracting with ethyl acetate, separating an organic phase, drying, filtering, performing rotary evaporation to remove a solvent, chromatographing the residue through an ethyl acetate / petroleum ether mixed solvent to obtain a target product II, wherein the proportion of the ethyl acetate / petroleum ether mixed solvent is selected according to different polarities of the product, and silica gel is adopted as a solid phase in column chromatography. The method applied to medicinal molecule synthesis is feasible, is simple and convenient to operate, and is used for implementing an unactivated olefin hydrogen trifluoride methylation reaction to prepare a series of trifluoromethyl-containing target compounds by selecting low-price trifluoromethyl reagent under a mild condition.

The invention provides an iron trifluoride composite material. The iron trifluoride composite material is composed of iron trifluoride and a multi-component conductive polymer doped and hybridized in iron trifluoride. The invention further provides a preparation method of the iron trifluoride composite material. The preparation method comprises the following steps of mixing and grinding multi-component conductive polymer powder and iron trifluoride powder, and then, thermally processing so as to obtain the iron trifluoride composite material. The conductive polymer is doped and hybridized in iron trifluoride nano-particles, such that a conductive polymer / iron trifluoride composite material is obtained; the electrochemical performance of the iron trifluoride composite material can be effectively improved; the stability, the capacity and the rate capability of a cathode material are improved; simultaneously, the problem that the iron trifluoride cathode material is low in electric conductivity can be solved well; furthermore, a one-step method provided in the invention is simple to operate and low in cost; furthermore, reaction is unnecessary to carry out in a solvent; and thus, the preparation method is more suitable for industrial mass production and application.

The invention provides a ferric fluoride / conducting polymer composite material. The ferric fluoride / conducting polymer composite material comprises ferric fluoride and a conducting polymer compounded to the surface of ferric fluoride. The invention further provides a preparation method of the ferric fluoride / conducting polymer composite material. The preparation method comprises the step of mixing ferric fluoride powder, a ferric trichloride solution, conducting polymer monomers, an anionic surfactant and an organic solvent to react, so as to obtain the ferric fluoride / conducting polymer composite material. Aiming at the problems that ferric trichloride has over-low electronic conductivity and expands along the polarization in charging and discharging processes, ferric trifluoride nanoparticles are coated with the conducting polymer by virtue of in situ polymerization and compounding, so that the polarization phenomenon of a ferric trifluoride material in the charging and discharging processes can be effectively overcome, the stability and capacity of the cathode material can be enhanced, meanwhile, the problem that the conductivity of a ferric trifluoride cathode material is too low can be well solved, and therefore, the electrochemical performance of the ferric trifluoride cathode material is improved.

The present invention relates to an erbium doped yttrium trifluoride upconversion luminescence hollow nanometer fiber preparation method, and belongs to the technical field of nanometer material preparation. The preparation method comprises the following four steps: (1) preparing a spinning solution; (2) adopting a uniaxial electrospinning technology to prepare PVP / [Y(NO3)3+Er(NO3)3] original composite fibers; (3) preparing Y2O3:Er<3+> hollow nanometer fibers, wherein the Y2O3:Er<3+> hollow nanometer fibers are obtained by carrying out a heat treatment on the original composite fibers; and (4) preparing YF3:Er<3+> hollow nanometer fibers, wherein a dual crucible method is adopted, ammonium bifluoride is adopted to carry out a fluorination treatment on the Y2O3:Er<3+> hollow nanometer fibers to obtain the YF3:Er<3+> hollow nanometer fibers, and the YF3:Er<3+> hollow nanometer fibers have excellent crystallinity, a diameter of 149-195 nm and a length of more than 30 mum. The hollow nanometer fibers are an important upconversion luminescence material. In addition, the preparation method has characteristics of simpleness, easy performing, mass production and broad application prospects.

The invention discloses a preparation method of thallous iodide, and belongs to the technical field of metal compounds. The preparation method is characterized in that ash slag of sulfuric acid, wastewater of sulfuric acid and iodide are used as raw materials to prepare; the ash slag of sulfuric acid is prepared from Fe2O3 (ferric oxide), Fe3O4 (ferroferric oxide), TlF (thallium fluoride) and TlF3 (thallium trifluoride); the sulfur acid waste water contains HF (hydrogen fluoride) and Tl<+>. The preparation method of the thallous iodide has the advantages that the production cost is reduced, and the purer product can be obtained.

The invention relates to a method and equipment for preparing long carbon chain olefins by use of natural alcohols or esters. The method comprises the following steps: by using one or a mixture of one or more of natural alcohols or esters as a reaction primer, carrying out a reaction in a reactor filled with a catalyst after gasification; and then separating the product to prepare the long carbon chain olefins, wherein the natural alcohols or esters are one or more of primary alcohols, secondary alcohols, primary esters or secondary esters with 6-18 carbon atoms; the catalyst is a mixture of a metal fluoride and an oxide, wherein the oxide accounts for 8-100wt% of the catalyst and the metal fluoride accounts for 0-90wt% of the catalyst; the metal fluoride is one or more of aluminum trifluoride, chromium trifluoride or gallium trifluoride and the oxide is one or more of aluminum oxide or silicon dioxide. The method and equipment for preparing long carbon chain olefins by natural alcohols or esters provided by the invention have the beneficial effects of being high in production efficiency, energy-saving and environment-friendly.

The invention discloses a method for synchronizing m-benzenyl trifluoride di-cyan acetonephenone which is an important intermediate for metaflumizone, a kind of efficient insecticide. The method includes utilizing 4-cyanobenzylchloride as raw materials to generate 4-cyano phenylacetonitrile to be reacted with methyl 3-benzoate in organic solvent for 5-8 hours. The yield of the intermediate of the metaflumizone produced by the method is higher than 90%, and content is higher than 89%. The method for synchronizing m-benzenyl trifluoride di-cyan acetonphenone is high in yield, low in cost and can be used for industrial production.

Production of 1,1,1,2-tetrafluoroethane and pentafluoethane simultaneously is carried out by taking chlorylene as raw material, reacting with Cl2 with anhydrous ferric chloride as catalyst to generate pentaline partly, reacting with HF with mixture of antimony chloride and anhydrous ferric chloride as catalyst to generate mixture of 1,1,1-trifluoride-2-chloroethane and 1,1,1,2-tetrafluoride-2-hydrochloric ether, reacting with HF at 200í½400íÒC and 0í½0.5Mpa with mixture of CrF3, AlF3, ZnF2 and MgF2 as catalyst to generate mixture of 1,1,1,2-tetrafluoroethane and pentafluoethane, separating, washing, alkali washing, dewatering, rectifying and drying to obtain 1,1,1,2-tetrafluoroethane and pentafluoethane.

The invention discloses a rare-earth-ion-doped cerium trifluoride / graphite-phase carbon nitride composite photocatalytic material, and a preparation method and application thereof. The preparation method comprises the following steps: putting g-C3N4 into deionized water for ultrasonic stripping to obtain a suspension solution, adding Ce(NO3)3. 6H2O, NH4F and Pr(NO3)3. 6 H2O into the suspension solution, adjusting the pH value of a formed system to 4-5, and carrying out magnetic stirring and uniform mixing; and then transferring a mixture obtained in the previous step into a high-pressure hydrothermal reaction kettle with a stainless steel jacket and a polytetrafluoroethylene liner, and carrying out a hydrothermal reaction in the hydrothermal reaction kettle at 160-180 DEG C for 10-16 hoursto obtain the rare-earth-ion-doped cerium trifluoride / graphite-phase carbon nitride up-conversion composite photocatalytic material. The material is applied to the field of photocatalytic degradationof dye wastewater, and the degradation rate of methylene blue reaches 93% after visible light illumination is performed for 60 min.

A process for preparing 2-aryl-5-(trifluoromethyl) pyrrole-3-nitrile includes such steps as reacting of alpha-arylamino acid on trifluoroacetic acid and acylchlorating reagent under existance of organic solvent to obtain the trifluoroacetyl derivative of alpha-arylamino acid, and reacting on 2-haloacrylonitrile under existance of alkali, organic solvent, and acylchlorating reagent or acid anhydride. Said alpha-aryl trifluoroacetylamino acid compound is prepared from trifluoroacetic acid and acylchlorating reagent through acetylation under existance of organic solvent.

The invention discloses a method for preparing 2-bromine-5-fluoro-benzo-trifluoride, and belongs to the field of organic synthesis. The method comprises the following steps: firstly, mixing sulfuric acid with fluorobenzotrifluoride, and further adding bromated into the obtained mixture at 0-80 DEG C to react, thereby obtaining 2-bromine-5-fluorobenzotrifluoride. Through the adoption of the method, the yield can be greater than 90.0%, the purity is greater than 99.0%, the raw materials are easy to obtain, and the reaction condition is mild and easy to control.

The invention discloses a method for preparing 2-bromine-5-fluoro-benzo-trifluoride, and belongs to the field of organic synthesis. The method comprises the following steps: firstly, mixing sulfuric acid with fluorobenzotrifluoride, and further adding bromated into the obtained mixture at 0-80 DEG C to react, thereby obtaining 2-bromine-5-fluorobenzotrifluoride. Through the adoption of the method, the yield can be greater than 90.0%, the purity is greater than 99.0%, the raw materials are easy to obtain, and the reaction condition is mild and easy to control.

The invention discloses a nanometer FeF3 / C composite positive electrode material, a preparation method thereof and a lithium ion battery. The method comprises the following steps: (1) putting reaction raw materials into a reaction kettle, filling the reaction kettle with protective gas, and sealing; wherein the reaction raw materials comprise an iron source and polytetrafluoroethylene; and (2) carrying out heat treatment on the sealed reaction kettle at the temperature of more than or equal to 400 DEG C to obtain the nano FeF3 / C composite positive electrode material. According to the invention, the property of sublimation of polytetrafluoroethylene at low temperature is utilized, and an iron source and a fluorine source are fully reacted by using a closed reaction kettle; the used polytetrafluoroethylene can provide a fluorine source and can be cracked to obtain the iron trifluoride composite positive electrode material with superfine nano-particles at the same time. The lithium ion battery positive electrode material provided by the invention has the advantages of high reversible specific capacity, excellent rate capability and good cycling stability.

The invention relates to three luorescence complexes formed on the basis of Eu (III) and chlorosulfonation four-tooth Beta-diketone ligands, as well as the application thereof. The three luorescence complexes are formed through Eu3+ and three chlorosulfonation four-tooth Beta-diketone ligands, namely 1, 2-bi (1', 1', 1', 2', 2', 3', 3' -seven fluorine-4', 6- hexanedione-6'-group- para- phenmethyl)-4- chlorine sulfonyl benzene, 1, 2-bi(1', 1', 1', 2', 2'- pentafluoride-3', 5'- pentanedione-5'-group- para- phenmethyl)-4- chlorine sulfonyl benzene and 1, 2-bi(1', 1', 1'- trifluoride-2', 4'- butanedione-4'-group- para- phenmethyl)-4- chlorine sulfonyl benzene. The three chlorosulfonation four-tooth Beta-diketone ligands are that three probes are covalently attached with moleculars such as protein containing amino group, amino acid, peptide, nucleic acid and the like and used as fluorescence labelings for the moleculars, and used for biological determinations such as time-resolved fluoroimmunoassay and the like.