31results about "Boron halogen compounds" patented technology

The present invention provides an oxyhalide, a preparation method therefor, and an all-solid-state lithium battery. The preparation method comprises: (1) grinding a mixture of a lithium source and a boron source, which are weighed in a stoichiometric ratio, tableting the mixture, then putting the tableted mixture into a reaction tube, evacuating the reaction tube to establish a vacuum, sealing the reaction tube, and then performing primary calcination, wherein the primary calcination temperature is 300-450ºC, and the primary calcination time is 4-20 h; and (2) after the primary calcination, cooling to room temperature, taking out the intermediate product from the reaction tube, grinding and tableting the intermediate product, then putting the tableted product into a reaction tube, evacuating the reaction tube to establish a vacuum, sealing the reaction tube, performing secondary calcination, and then cooling to room temperature. The preparation method of the present invention is simple and has high raw material utilization rate and no byproducts, thereby facilitating industrial production. The prepared oxyhalide has relatively high ionic conductivity and stability, and relatively good interface stability with metal lithium. The prepared all-solid-state lithium battery has excellent electrochemical performance.

The invention relates to a preparation method of sodium fluoborate, which comprises the following steps: step a, dissolving sodium fluoride and sodium sulfate solid residues generated in the production process of nuclear grade boron-10 acid in a certain amount of deionized water, and filtering; b, evaporating the filtered solution, crystallizing when the residual volume of the evaporated solution reaches a certain degree, and then filtering again; and step c, dissolving the sodium fluoroborate obtained after filtration in a certain amount of ultrapure water, filtering and drying to obtain the high-purity sodium fluoborate. According to the invention, direct preparation of sodium fluoborate is realized, the step of firstly converting sodium fluoborate into boric acid in the traditional process is omitted, the process steps are optimized, the reaction time is shortened, the reaction flow is reduced, the utilization rate of raw materials is increased, and the reaction economy is improved.

The present invention provides a semiconductor process gas purification system that can repeatedly purify and regenerate semiconductor process gases and purification equipment without cooling them to extremely low temperatures or reducing purification efficiency. [Solution] A process gas purification apparatus comprising a cylindrical container, a heater positioned to cover the outer surface of the container, and a cooling gas pipe passing through the inside of the container, wherein the container is filled with a purifying agent for adsorbing impurity gases contained in the semiconductor process gas to be purified, and a semiconductor process gas inlet and outlet are provided for passing the semiconductor process gas to be purified through and bringing it into contact with the purifying agent, and the cooling gas pipe is covered with the purifying agent inside the container.

The invention provides a method for synchronously removing fluorine and boron in a lithium-containing solution, which comprises the following steps: mixing a lithium-containing leachate of waste battery black powder with a lithium-containing leachate of glass powder to obtain a lithium-containing solution containing fluorine and boron; extracting the lithium-containing solution by adopting an acidified composite extracting agent to obtain an organic phase loaded with fluorine and boron and raffinate; performing post-treatment on the extracting solution to obtain a lithium-containing solution; and washing and reversely extracting the organic phase loaded with fluorine and boron to obtain a solution containing fluorine and boron. According to the method, fluorine in the waste battery black powder lixivium and boron in the glass powder lixivium can be synchronously removed, the lithium loss amount in the impurity removal process is small, the technological process is short, the cost is low, and the obtained lithium-containing solution is high in purity.

The invention discloses a low-cost high-purity potassium fluoborate preparation method based on ammonium fluoride, and belongs to the field of inorganic salt chemical industry, the method comprises the following steps: S1, reacting by-product ammonium fluoride with the purity of more than or equal to 99% with boric acid to synthesize an ammonium fluoborate solution; s2, at 60-80 DEG C, precisely dropwise adding a potassium chloride solution into the ammonium fluoborate solution at a rate of 1-2 mL / (min.L), and carrying out a replacement reaction; s3, performing crystallization and purification by adopting a two-stage gradient cooling program from fast to slow; s4, a low-temperature saturated potassium fluoborate solution and absolute ethyl alcohol are sequentially adopted for targeted washing, and impurities such as chloride ions are effectively removed; and S5, performing vacuum drying to obtain a product. According to the method, the phosphorus fertilizer industrial byproduct ammonium fluoride is originally adopted to replace expensive hydrogen fluoride or fluoboric acid, so that the raw material cost is reduced by 90% or above; meanwhile, impurity inclusion is effectively inhibited, the problem of impurity introduction caused by byproduct raw materials is solved, and the electronic-grade high-purity potassium fluoborate with the main content larger than or equal to 99.95% and the chloride ion smaller than or equal to 10 ppm can be stably prepared.

The present invention relates to a process for preparing hydroboranes by the hydrogenolysis of corresponding (pseudo-)haloboranes, in the presence of a base and optionally a catalyst. The process of the invention contributes to the circularity of the boron element by enabling the recycling of (pseudo-)haloborane compounds, common waste products of boron chemistry, into higher value-added hydroboranes. Figure for the abstract: None

The present disclosure provides a method for producing lithium fluoride, and the like, comprising: a step 1 for preparing an aqueous solution of at least one of lithium chloride and lithium sulfate; a step 2 in which an aqueous solution of at least one of lithium chloride and lithium sulfate is mixed with an aqueous hydrofluoric acid solution; and a step 3 in which a mixed solution of an aqueous solution of at least one of lithium chloride and lithium sulfate and an aqueous solution of hydrofluoric acid is mixed with an alkali, the pH of the liquid obtained in the step 3 being 3-6.

A conjugated acid proton exchange polymer molecule comprising an acidic aromatic unit in a main chain or a side chain wherein the acidic aromatic unit is a conjugated acid of an alkaline aromatic unit; and a non-coordinating counter anion ionically bonded to the acidic aromatic unit.

This invention provides a compound, sodium cesium fluoroborate, and a sodium cesium fluoroborate nonlinear optical crystal, along with their preparation methods and applications. The compound has the chemical formula NaCs7[B3O3F4(OH)]4(H2O)3 and a molecular weight of 1701.16, and is prepared using a room-temperature solution method. The crystal also has the chemical formula NaCs7[B3O3F4(OH)]4(H2O)3 and a molecular weight of 1701.16. This crystal belongs to the monoclinic crystal system and has a space group of [space group missing]. P 21, cell parameters are a =11.5864(15), b =13.463(2), c =12.5958(19), α =90°, β =90°, c =109.697(5)°, unit cell volume is 1849(5) Å 3 The crystal is grown using a room temperature solution method or a hydrothermal method. It has good chemical stability and can be used as a short-wavelength nonlinear optical crystal in all-solid-state lasers.

The invention relates to a preparation method of a high-purity lithium tetrafluoroborate liquid salt, which comprises the following steps of: reacting lithium metaborate serving as a raw material with calcium fluoride and excessive sulfur trioxide gas for 1-5 hours at the temperature of 60-150 DEG C and the high pressure of 0.2-5 MPa, after the reaction is finished, depressurizing to separate out the sulfur trioxide gas for reuse, dissolving a reaction product in a benign organic solvent under the protection of inert gas, filtering out insoluble substances, and performing vacuum drying to obtain the high-purity lithium tetrafluoroborate liquid salt. And performing resin deacidification and membrane filtration on the filtrate to obtain the product. The method is simple in process, mild in condition and high in product yield, the water content of the prepared high-purity lithium tetrafluoroborate liquid salt is lower than 10 ppm, the free acid content (in terms of HF) is lower than 13 ppm, the Cl content is lower than 3 ppm, the SO4 content is lower than 2-5 ppm, and the single content of various metal impurity ions (such as calcium, iron, magnesium, sodium and potassium) is smaller than or equal to 2 ppm.

The present disclosure provides a method of preparing a target compound. The method includes the step of combining (A) an organosilicon component and (B) a catalyst including a boron cluster to give a mixture. The method further includes preparing a reaction mixture including the target compound from the mixture. The organosilicon component (A) includes (A1) a first organosilicon compound having a silicon-bonded C1-C4 alkyl group. When the first organosilicon compound (A1) does not include a silicon-bonded halogen atom, the organosilicon component (A) includes a second organosilicon compound (A2) including at least one silicon-bonded halogen atom. The disclosure further provides a reaction product prepared according to the method.

This invention provides oxyhalides, a method for producing the same, and an all-solid-state lithium battery. The production method includes step 1, in which a mixture of lithium and boron sources weighed in stoichiometric ratios is polished, sheeted, placed in a reaction tube, the reaction tube is vacuumed and sealed, and a first firing is performed at a temperature of 300-450°C for a duration of 4-20 hours; and step 2, after the first firing, the mixture is cooled to room temperature, the intermediate product in the reaction tube is removed, further polished, sheet-pressed, placed in the reaction tube, the reaction tube is vacuumed and sealed, a second firing is performed, and then the mixture is cooled to room temperature. The production method of this invention is simple, has a high utilization rate of raw materials, and does not contain by-products, making it advantageous for industrial production. The oxyhalides produced have high ionic conductivity and stability, and good interfacial stability with metallic lithium. The all-solid-state lithium batteries produced have excellent electrochemical performance.

The present invention relates to metal halide perovskite (CsPbBr3) nano / microcrystals. Specifically, the present invention relates to a method for the synthesis of metal halide perovskite (CsPbBr3) nano / microcrystals. The present invention uses an easy, scalable low temperature growth of metal halide nanoparticles like CsPbBr3. The method uses a clever play on the solubility and ion exchange mechanism to precipitate nano and microcrystals of metal halide perovskites. The synthesis resulted in stable perovskite crystals with high photo- luminescence, ultralow dark current and control over their morphology. The combination of ultralow dark current, high responsivity, exceptional detectivity, and broad-band photon detection capabilities makes these crystals an excellent choice for upcoming sensors and detector technologies.

The invention belongs to the technical field of wet-process phosphoric acid, and particularly relates to a method for breaking a fluorine-aluminum complex and recovering aluminum and magnesium by introducing a boron source. The method comprises the following steps: introducing a boron source into a fluorine-containing aluminum complex solution, and reacting to break the fluorine-containing aluminum complex so as to obtain a reaction solution; wherein the molar ratio of the fluorine element in the fluorine-containing aluminum complex solution to the boron element in the boron source is 12: 1-3: 8; adding ammonium sulfate A into the reaction liquid, and crystallizing to obtain ammonium aluminum sulfate crystals and ammonium aluminum sulfate crystal removal mother liquor; adding ammonium sulfate B into the ammonium aluminum sulfate removal crystallization mother liquor, and crystallizing to obtain ammonium magnesium sulfate crystals and ammonium magnesium sulfate removal crystallization mother liquor; and adding a potassium source into the ammonium magnesium sulfate removal crystallization mother liquor, uniformly mixing, and carrying out precipitation reaction to obtain potassium fluoborate precipitate. According to the method, the problem that a fluorine-aluminum complex hinders recycling of aluminum crystals is solved, recycling of the strip liquor can be achieved, meanwhile, aluminum and magnesium elements are recycled respectively, fluorine elements are recycled, and the purity of recycled aluminum, magnesium and fluorine products is high.

To provide a fluorine-containing compound solid electrolyte having high ion conductivity, a method for producing the same, and a battery.SOLUTION: The general structural formula of the solid electrolyte with relatively high ionic conductivity is (AX) aMBy, wherein A is at least one of Li, Na, K, Ag and Cu; M is at least one of Ti, Sn, Ta, N, Zr, Hf, Ga, Al and Fe, 0.5 <a <4, B is at least one of F and Cl, X is at least one of oxygen-containing anion and fluorine-containing anion, y is 4 or 5, or B is at least one of F, Cl, Br and I, X is BF4, y is 3 or 4 or 5.SELECTED DRAWING: Figure 1

The invention relates to a method for recovering fluorine and potassium in a wet-process phosphoric acid / ammonium phosphate solution system, and belongs to the technical field of wet-process phosphoric acid. The technical problem to be solved by the invention is to provide a new method for recovering fluorine and potassium in a wet-process phosphoric acid / ammonium phosphate solution system. The method comprises the following steps: mixing a phosphoric acid solution with a boron source for reaction to obtain a reaction solution; mixing with a potassium source and carrying out precipitation reaction to obtain turbid liquid; and carrying out solid-liquid separation on the turbid liquid, and drying the solid to obtain potassium fluoborate and liquid which is defluorinated phosphoric acid. According to the method, fluorine in wet-process phosphoric acid is reasonably utilized to prepare potassium fluoborate, and recycling of fluorine and potassium is achieved. A boron source is adopted to break fluorine-aluminum complex bonds in the solution, so that fluorine is convenient to recycle, and meanwhile, release of aluminum ions and subsequent recycling of aluminum resources are also facilitated. The method is simple in reaction, simple and convenient to operate and easy to realize technologized large-scale production.

This invention discloses a method for preparing high-purity potassium fluoroborate using by-product fluorosilicic acid, belonging to the field of fine chemical technology. It aims to solve the problems of incomplete removal of silicon impurities, limited product purity, and high raw material costs and environmental pressures associated with traditional fluorosilicic acid methods for potassium fluoroborate preparation. This invention uses by-product fluorosilicic acid as raw material and achieves green and efficient preparation of high-purity potassium fluoroborate by introducing a multi-stage targeted silicon removal and purification control strategy. The process includes raw material pretreatment and compatibility, primary reaction and initial silicon removal, secondary reaction and deep silicon removal, and tertiary reaction and directional crystallization. This methodological innovation, combined with the discovery of key parameters, enables a product purity of up to 99.7%, with the key impurity silica content below 0.02%, and a product yield as high as 96.2%. This invention not only significantly improves product purity and realizes high-value utilization of by-product resources and reduces production costs, but also has the advantages of being green, environmentally friendly, and highly safe.

The invention relates to the technical field of synthetic lubricating oil, and discloses a method for preparing poly-alpha-olefin from a coal-based alkene mixture and recycling production wastewater. The method comprises the following steps: (1) carrying out polymerization reaction on a coal-based C8-C12 alkene mixture under the catalytic action of boron trifluoride, distilling the obtained reaction product, carrying out alkali washing on the separated heavy component, and carrying out oil-water separation; (2) carrying out hydrofining reaction on an oil phase separated in the oil-water separation process in the step (1) in a hydrogen atmosphere, and then carrying out reduced pressure distillation on a reaction product to obtain poly-alpha-olefin base oil; and (3) carrying out evaporation concentration on the wastewater separated in the oil-water separation process in the step (1), carrying out centrifugal separation on the obtained concentrated solution, adding a sodium tetrafluoroborate seed crystal into the separated solution, crystallizing and drying to obtain a sodium tetrafluoroborate crystal. The technical scheme provided by the invention can realize efficient recovery and utilization of fluorine resources in the production process of poly-alpha olefin.

Aspects of the present disclosure are directed to methods, compositions, and kits for detection and analysis of DNA and RNA modifications, such as DNA and RNA nucleobase methylation. Certain aspects include methods, compositions and kits useful in sequencing of methylated nucleic acids, including methylated nucleic acids from low-input samples such as cell-free DNA and cell-free RNA. Certain aspects include novel N-nitrosation strategies for deamination of DNA and RNA biological macromolecules under mild conditions. In some aspects, provided are compositions, methods, and kits comprising means for cooperative catalysis of a carbonyl organocatalyst with a Lewis acid to facilitate the formation of a C-nitro intermediate from a primary amine, which, upon rearrangement into N-nitrosamine, leads to selective deamination of unsubstituted canonical DNA and RNA bases under mild conditions.

A conjugate acid proton exchange polymer molecule includes an acidic aromatic unit in a main chain or a side chain, wherein the acidic aromatic unit is a conjugate acid of a basic aromatic unit, and a non-coordinating counter anion ionically linked with the acidic aromatic unit.

This invention relates to a compound, potassium fluoroborate, a nonlinear optical crystal of potassium fluoroborate, its preparation method, and its uses. The chemical formula of the compound is K₂B₂OF₆, and its molecular weight is 229.82. It is prepared by a room temperature solution method or a hydrothermal method. The crystal belongs to the hexagonal crystal system, with space group P₆(_)₂m, and cell parameters a=9.1105(13)Å, b=9.1105(13)Å, c=6.9919(17)Å, α=90°, β=90°, γ=120°, Z=3, and V=502.59(16)Å. 3 Potassium fluoroborate nonlinear optical crystals obtained by growing crystals using room-temperature solution methods, hydrothermal methods, or high-temperature melt methods possess advantages such as a wide transmission band, stable physicochemical properties, moderate mechanical hardness, resistance to breakage, and ease of cutting, polishing, and storage. They can be widely used in nonlinear optical devices such as frequency doubling converters and optical parametric oscillators.

The present application relates to the field of comprehensive utilization of wet-process phosphoric acid resources and preparation of new energy materials, and discloses a method for selectively recovering fluorine from wet-process phosphoric acid and preparing lithium difluorophosphate. By adding boric acid to the wet-process phosphoric acid, the fluorine species is converted, and tri-octylamine organic extraction system is used to selectively separate fluorine and phosphorus, and then lithium fluoroborate is prepared by back extraction, and further reacts with anhydrous oxalic acid to generate lithium difluorophosphate, and after recrystallization, battery-grade lithium difluorophosphate with a purity of 99.7% or above is obtained. The method realizes efficient recovery and high-value conversion of by-product fluorine resources in wet-process phosphoric acid, has the advantages of simplified process, high extraction selectivity, high resource utilization rate and significantly improved product added value, and can be used for preparation of lithium ion battery electrolyte.

The invention provides a compound ammonium potassium fluoborate, an ammonium potassium fluoborate nonlinear optical crystal and a preparation method and application thereof. The chemical formula of the compound is Kx (NH4) 2-xB8O12F2 (x is more than 0 and less than 2), the chemical formula of the crystal is Kx (NH4) 2-xB8O12F2, the crystal belongs to an orthorhombic system, the space group is Pna21, and the unit cell parameters are as follows: a = 7.5880 (7) + / -0.02, b = 11.2019 (10) + / -0.02, c = 6.5989 (6) + / -0.02, alpha = beta = gamma = 90 degrees, and Z = 2. The crystal is grown by adopting a vacuum high-temperature solution method, a room-temperature solution method or a hydrothermal method, and the ultraviolet transmission cut-off edge of the crystal is lower than 190 nm. The nonlinear optical effect of the crystal is about 2.8 times that of KH2PO4 (KDP), and the shortest I-type phase matching wavelength is about 165.5 nm. The crystal has the advantages of being simple in preparation method, low in toxicity of used starting raw materials, small in harm to human bodies, not prone to deliquescence, good in thermal stability, easy to apply and the like. The method can be widely applied to nonlinear optical devices such as ultraviolet and deep ultraviolet all-solid-state lasers, optical parametric oscillators and the like.

The invention discloses a synthetic production method of white high-purity anhydrous silver tetrafluoroborate, which comprises the following steps: mixing and reacting mercury-free salt and anhydrous silver tetrafluoroborate in an anhydrous reaction medium to obtain anhydrous silver tetrafluoroborate; the mercury-free salt is at least one of anhydrous silver bis (trifluoromethanesulfonimide), anhydrous silver trifluoroacetate, anhydrous silver trifluoromethanesulfonate and anhydrous silver methanesulfonate; the tetrafluoroboric acid source is selected from at least one of anhydrous tetrafluoroboric acid and anhydrous tetrafluoroborate; the anhydrous reaction medium is at least one of absolute methanol, absolute ethyl alcohol, anhydrous dimethyl sulfoxide, anhydrous N-dimethylformamide, anhydrous dichloromethane, anhydrous tetrahydrofuran, anhydrous ethyl acetate, anhydrous ether, anhydrous petroleum ether, anhydrous isopropanol, anhydrous methyl acetate, anhydrous n-heptane, anhydrous cyclohexane and anhydrous acetone. According to the invention, the raw materials are non-toxic, no water is added or generated in the production process, and the prepared silver tetrafluoroborate is white, high in purity and free of crystal water.

The invention discloses a method for preparing high-purity potassium fluoborate by using byproduct fluosilicic acid, relates to the technical field of fine chemical engineering, and aims to solve the problems that impurity silicon is difficult to thoroughly remove, the product purity is limited, the raw material cost and the environmental protection pressure are high and the like when the potassium fluoborate is prepared by a traditional fluosilicic acid method. According to the method, by-product fluosilicic acid is taken as a raw material, and a multi-stage targeted silicon removal and purification control strategy is introduced, so that green and efficient preparation of high-purity potassium fluoborate is realized. The process comprises the steps of raw material pretreatment and compatibility, first-stage reaction and primary silicon removal, second-stage reaction and deep silicon removal, and third-stage reaction and directional crystallization. The methodology innovation is combined with the discovery of key parameters, so that the product purity can reach 99.7%, the content of key impurity silicon dioxide is lower than 0.02%, and meanwhile, the product yield is as high as 96.2%. According to the method, the product purity is remarkably improved, high-value utilization of byproduct resources is achieved, the production cost is reduced, and the method has the advantages of being environmentally friendly and high in safety.

The present disclosure provides a method of preparing an organosilicon compound. The method includes combining (A) a hydridosilane, (B) an arene compound, and (C) a catalyst including a boron cluster, thereby preparing a reaction mixture including the organosilicon compound. The hydridosilane (A) has the formula HSiQ3, where each Q is an individually selected halogen atom. The organosilicon compound has the formula RSiQ3, where R is an aryl group, and each Q is independently selected and defined above. The present disclosure further provides a reaction product prepared via the method.

The invention relates to the technical field of second-order nonlinear optical materials, in particular to a second-order nonlinear optical material zinc fluoroborate as well as a preparation method and application thereof. The chemical formula of the zinc fluoborate is KZnBO3FH, and the crystallographic characteristics are as follows: the zinc fluoborate belongs to a hexagonal system, the space group is P-6c2, and the crystal unit cell parameters are as follows: alpha is equal to 90 degrees, beta is equal to 90 degrees, and gamma is equal to 120 degrees; z = 2. According to the zinc fluoborate salt, a hydrothermal synthesis process is adopted, boric acid and water are used as solvents, zinc fluoride, potassium carbonate and potassium fluoborate react for 12-48 hours at the temperature of 200-220 DEG C under the condition of a potassium hydroxide strong alkali medium, and finally the potassium zinc fluoborate which has a regular triangular prism shape and is crystallized in a non-centered space group is obtained. The potassium zinc fluoborate shows excellent second-order nonlinear optical characteristics, the powder frequency-doubled effect intensity of the potassium zinc fluoborate can reach 7 times that of a KH2PO4 (KDP) reference material, and meanwhile, the potassium zinc fluoborate has a 379nm short-wave ultraviolet absorption cutoff edge and shows excellent wide-spectrum light transmission performance.

The present application relates to a kind of low-temperature rectification separation methods of high-abundance boron halide-10 in the field of chemical synthesis and separation, comprising: S1, boron halide gas is pumped into dry device and is dry handled;S2, the boron halide gas that is handled by step S1 dry is pumped into rectification pipe body from the bottom of low-temperature rectification tower, rectification tank body is filled with liquid nitrogen, and multiple trays are arranged in rectification tank body, and the filler in the tray is graphene aerogel, and the boron halide pumped from the bottom of rectification tank body rises to the top of tower after sequentially passing through graphene aerogel in each layer of tray from bottom to top;S3, multiple low-temperature rectification towers are sequentially connected to form multistage low-temperature rectification tower, and the abundance of boron halide-10 in the boron halide gas output from the top of last-stage rectification tower is greater than or equal to 99%.The present application solves the technical problems such as corrosion and blockage caused by cracking in the chemical exchange rectification method of boron fluoride-methyl ether complex.

The invention provides a scheelite-like compound antimony fluoroborate, an antimony fluoroborate multifunctional crystal and a preparation method and application of the scheelite-like compound antimony fluoroborate and the antimony fluoroborate multifunctional crystal. The chemical formula of the compound is SbBO2F2, the molecular weight is 202.56, and the compound is prepared through a vacuum tube sealing method or a hydrothermal method; the chemical formula of the crystal is SbBO2F2, the molecular weight is 202.56, the crystal belongs to a monoclinic system, the space group is C2 / c, the cell parameters are as follows: a = 6.3036 (5), b = 12.2182 (10), c = 4.5611 (4), alpha = gamma = 90 degrees, beta = 122.261 (3) degrees, and the unit cell volume is 297.06 (4) 3. The birefringence is 0.22 when the wavelength is 1064 nm, the band gap is relatively large, and the ultraviolet absorption edge is about 215 nm. The crystal is grown by adopting a vacuum tube sealing method or a hydrothermal method, the chemical stability of the crystal is good, and the crystal can be used as a polarization beam splitter prism or an optical element of an infrared-visible light-ultraviolet band and is applied to an all-solid-state laser.