50results 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 provides a compound cesium sodium fluoborate, a cesium sodium fluoborate nonlinear optical crystal and a preparation method and application thereof, the chemical formula of the compound is NaCs7 [B3O3F4 (OH)] 4 (H2O) 3, the molecular weight is 1701.16, and the compound is prepared by a room temperature solution method; the chemical formula of the crystal is NaCs7 [B3O3F4 (OH)] 4 (H2O) 3, the molecular weight is 1701.16, the crystal belongs to a monoclinic system, the space group is P21, the cell parameters are as follows: a is equal to 11.5864 (15), b is equal to 13.463 (2), c is equal to 12.5958 (19), alpha is equal to 90 degrees, beta is equal to 90 degrees, gamma is equal to 109.697 (5) degrees, the unit cell volume is 1849 (5) 3, the crystal is grown by adopting a room temperature solution method or a hydrothermal method, the chemical stability of the crystal is good, and the crystal can be used as a short-wavelength nonlinear optical crystal to be applied to an all-solid-state laser.

The present invention is applicable to the field of gas preparation technology improvement, and provides a preparation method of boron trichloride, including, S1, fully dissolving anhydrous aluminum chloride crystals in the N, N-dimethylformamide solvent in the reactor according to proportion; S2, passing boron trifluoride gas into the mixed solution in the reactor for chemical reaction to generate boron trichloride gas and aluminum fluoride precipitate; S3, collecting and loading the generated boron trichloride gas into a pre-vacuumed collection tank after liquefaction through a condenser. The direct use of chlorine is avoided in the preparation of boron trichloride, the safety factor is improved, it is more in line with environmental protection requirements, the harm to the human body is less, the production temperature is greatly reduced, and it is more energy-saving; the by-product of the output after the reaction is only aluminum fluoride, which reduces the dangerous absorption of by-products, and is safer. After the solution after the reaction removes aluminum fluoride, the N, N-dimethylformamide solvent can be reused, which reduces the cost.

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 utility model relates to the technical field of experimental equipment, in particular to a boron trifluoride gas experimental device which comprises a reaction kettle, a condenser, a first purification tower, a second purification tower, a third purification tower and a gas buffer tank which are sequentially connected through gas pipelines. The reaction kettle is composed of a speed reducer, a stirring paddle, a kettle cover and a kettle body, a cavity is formed in the kettle body, a jacket is arranged outside the cavity, a heat preservation layer is arranged on the outer wall of the jacket, and a gas inlet and outlet is formed in the tail end of a gas pipeline on one side of the top of the gas buffer tank. According to the boron trifluoride gas experimental device, the temperature control in the reaction process is more accurate and stable due to the design of the jacket and the thermal insulation layer of the reaction kettle, so that the reaction efficiency is improved, the reaction speed and efficiency are further improved, impurities and particulate matters in boron trifluoride gas are effectively removed, and the purity of the gas is remarkably improved.

The invention discloses a resource utilization method of potassium fluoride and potassium chloride mixed salt, and belongs to the field of comprehensive utilization of resources. A resource utilization method of potassium fluoride and potassium chloride mixed salt comprises the following steps: S1, taking the mixed salt obtained by fluorination reaction in a certain fine chemical production process, adding water for dissolving, then adding activated carbon, stirring and filtering, then adding an Fe-g-C3N4 / MCM-41 catalyst and hydrogen peroxide, stirring for reaction, then filtering, and collecting filtrate for later use; s2, adding hydrochloric acid and boric acid into the filtrate obtained in the step S1, carrying out a heat preservation reaction, then adjusting the pH value to be neutral, cooling, filtering, and collecting the filtrate and a filter cake; the filter cake is potassium fluoborate; adding calcium chloride into the filtrate, stirring while keeping the temperature, filtering, adjusting the pH value of the filtrate to be neutral, and performing post-treatment to obtain potassium chloride. The method can realize effective utilization of potassium fluoride and potassium chloride mixed salt generated in the production process of the aromatic fluorine-containing fine chemicals, reduces the environmental protection pressure, and realizes resource utilization of wastes and sustainable development of the fluorine chemical industry.

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 invention discloses a method for purifying sodium chloride and sodium fluoborate from synthetic waste liquid of sodium fluoborate, which comprises the following steps: heating and concentrating the synthetic waste liquid of sodium fluoborate to obtain concentrated liquid; cooling, crystallizing and filtering the concentrated solution to obtain filtrate I and filter residue I; leaching the filter residue I to obtain a filter residue II and a filtrate II, and drying the filter residue II to obtain a sodium chloride extract; mixing the filtrate I and the filtrate II, heating, concentrating, crystallizing and filtering to obtain filtrate III and filter residues III; and evaporating, crystallizing and drying the filtrate III to obtain the sodium fluoborate extract. The concentrated solution is cooled, crystallized and filtered to obtain a filtrate I and a filter residue I, sodium fluoride is dissolved in a filtrate II in the presence of a trace amount of sodium fluoborate, sodium chloride mainly remains in the filter residue II, the filtrate I and the filtrate II are combined, evaporated and crystallized, a filtrate III mainly contains sodium fluoborate, and a filter residue III is a mixed salt composed of sodium chloride and sodium fluoborate; and the waste liquid can be mixed with the next batch of waste liquid, so that sodium chloride and sodium fluoride in the waste liquid are recovered.

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.

The present invention relates to a method for producing an oxide-based solid electrolyte powder. A method for producing an oxide-based solid electrolyte powder, according to one embodiment of the present invention, comprises the steps of: vibrating an aqueous precursor solution containing Li2CO3, H3BO3, Al2O3, and LiCl to generate fine droplets; a step of spraying fine liquid droplets; a step for generating a powder by heating the sprayed fine droplets; and a step for collecting the generated powder.

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 invention belongs to the technical field of fine chemical engineering, and relates to a microwave method-based high-abundance boron isotope separation method, which comprises the following steps of: by taking a boron trifluoride ether compound as a boron isotope exchange working system, enabling the boron trifluoride ether compound to be subjected to boron isotope rapid exchange through a two-stage exchange rectifying tower and an auxiliary stepped microwave heating device; the device has the advantages that the structure is compact, the operation is simple, the continuous automation is easy, the reaction time can be shortened by microwave heating, byproducts are reduced, the reaction yield is improved, the energy consumption is reduced by about 60%, the production cost is greatly reduced, and the concentration of the obtained boron-10 and boron-11 is greater than or equal to 99%.

A method for fabricating an ionic liquid electrolyte such as a spiro-based ionic liquid electrolyte, the method has the steps of: synthesizing an intermediate spiro-based product, and applying an ionic exchange process to the intermediate spiro-based product to obtain the ionic liquid electrolyte. The obtained an ionic liquid electrolyte comprising an ionic liquid salt with a cation of: (I) The ionic liquid electrolyte may be used in an electrochemical energy-storage apparatus such as a supercapacitor.

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

A compound has the formula Li4−xB7−yMyO12−zClw, wherein Li, O, and Cl vacancies are allowed and M is either a one-way, two-way or three-way combination of the following species: Al3+, Fe3+, B3+, La3+, Y3+, Mo3+, Be2+, Si4+, Cr4+, As3+, Mn2+, V2+, Co2+, Ge2+, Fe2+, Mo4+, Mo6+, As3−, Ti2+, P5+, As0+, and wherein 0≤x<2, 0<y<6, 0≤z<1, and 0<w<2 either satisfy a charge balance mechanism with their respective defect site B3+, Li+, O2−, or Cl−, or satisfy any combination that maintains charge neutrality of the compound, and wherein when M comprises Al3+, M is a two-way or three-way combination. A glass ceramic composition includes the compound. A lithium ion battery includes a solid state ionic conductor, wherein the solid state ionic conductor includes the compound.

To provide a liquid dispersion of fluoride particles, which has a low viscosity and excellent dispersibility and is suitable for the production of an optical film such as an antireflective film; a method for producing the liquid dispersion; and an optical film using the liquid dispersion.SOLUTION: A liquid dispersion of fluoride, which is characterized in that particles of a fluoride represented by chemical formula: AxCFy (wherein A represents sodium or potassium; C represents silicon or boron; x represents 1 or 2; and y represents 4 or 6) are dispersed in an aprotic organic solvent having a relative dielectric constant of 5 to 40. And an optical film produced using the liquid dispersion of fluoride particles.SELECTED DRAWING: None

The invention relates to a sulfuric acid decomposition production process of bastnaesite. The sulfuric acid decomposition production process comprises the following steps: S1, raw material pretreatment; s2, slurrying reaction: after the raw materials are pretreated, slowly adding concentrated sulfuric acid into the obtained solution, and stirring to carry out slurrying reaction; s3, clear water is added into the pulpified slurry container, the slurry rare earth sulfate obtained in the step S2 is stirred and dissolved, and a mixed solution of the rare earth sulfate is obtained; wherein in the step S3, the ratio of the slurry sulfuric acid rare earth to the clear water is 1: (1-5); the stirring time is 5-60 minutes, and the dissolving temperature is 50-95 DEG C; the method has the beneficial effects that the influence of fluorine in bastnaesite on rare earth is well removed, and fluorine is recycled in tail gas; the rare earth extraction rate is high, the waste residue amount is small, the technological process is short, the production cost is low, the rare earth productivity is greatly improved, the waste water amount and the waste water treatment cost are reduced, the content of sulfur in tail gas is very low, and the tail gas treatment cost is low.

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.

To provide a lithium ion conductor having high ionic conductivity in a high temperature range (80°C or higher).SOLUTION: A lithium ion conductor containing Li-B-I causes a phase transition at 60-80°C, showing high ionic conductivity. It also shows higher ionic conductivity than those of iodide- or bromide-based one of the same group, as well as iodinated sulfide-based one.SELECTED DRAWING: None