65 results about "Phosphorus sulfide" patented technology

The invention provides a lithium sulfur battery electrolyte for improving safety and stability. The electrolyte is prepared from lithium salt, solvents and additives, The lithium salt is a mixture oflithium bis-trifluoromethanesulfonimide (LiTFSI), lithium bis-oxalate borate (LiBOB) and lithium difluorooxalate borate (LiODFB), the solvent is a mixture of dioxolane (DOL) and tetraethanol dimethylether (TEGDEM), and the additive is lithium nitrate and phosphorus pentasulfide. The phosphorus sulfide additive in the battery prepared by the electrolyte reacts with the negative electrode lithium metal to form a passivation layer, At that same time, the decomposition of lithium bis (trifluoromethanesulfonimide) on the negative electrode side can be inhibit by the action of lithium bis (oxalate)and lithium difluorooxalate, so that the stability and cycle performance of the battery can be improved. The lithium bis (trifluoromethanesulfonimide) can protect the negative electrode, effectivelyreduce the generation of lithium dendrite and improve the safety of the battery.

A method for producing an ionic conductive substance, including a step of contacting raw materials in a solvent, wherein the raw materials include: one or more compounds selected from phosphorus sulfide, germanium sulfide, silicon sulfide and boron sulfide; a sulfide of a metal element belonging to group I or group II of the periodic table; and a halogen compound represented by MwXx wherein M is Li, B, Na, K, Rb, Cs, Ca, Mg, Sr, Ba, Al, Si, P, S, Ge, As, Se, Sn, Sb, Te, Pb or Bi, w is 1 or 2, X is F, Cl, Br or I, and x is an arbitrary integer selected from 1 to 10.

The invention discloses a preparation method of a nitrogen-phosphorus double-doped hollow carbon nanotube. The method comprises the following steps: soaking a nickel-based material in hydrogen peroxide in mass concentration of 15-30%, carrying out heating treatment for 2-10 hours at the temperature of 40-80 DEG C, and oxidizing the surface of the nickel-based material to generate nickel hydroxide. The method is capable of thermally decomposing the compound containing nitrogen and phosphorus; compared with the conventional nanotube containing nitrogen and carbon, the nitrogen-phosphorus double-doped hollow carbon nanotube prepared by the method has obvious structure advantages; the method is simple in reaction equipment, easily achievable and controllable in reaction conditions and low in cost; the prepared nitrogen-phosphorus double-doped hollow carbon nanotube has the structure advantage, shows high electrocatalytic activity extremely close to the commercial platinum carbon and more remarkable stability in oxygen reduction reaction of negative electrodes of fuel cells, and has great economic value and social value.

The invention provides a novel preparation method for ternary alloy type CdSeS quantum dots, which includes the following steps: mixing long-chain fatty acid cadmium with long-chain trialkylamine to obtain a precursor solution A; mixing trialkyl phosphine selenium, trialkyl phosphorus sulfide and trialkyl phosphine oxide to obtain a solution B, injecting the solution B in the precursor solution A for reaction, so as to obtain a CdSeS quantum dot solution C, removing non-reacted reactants, impurities and the long-chain trialkylamine as a solvent, and obtaining CdSeS quantum dot powder. The novel preparation method has the benefits that the preparation technology is simple, good safety, stability and repeatability are realized, the cost is low, high-quality quantum dots can be prepared in a large-scale manner; the optical property of the prepared quantum dots is stable, the spectroscopic property is excellent, the photoluminescence spectra are continuous and adjustable; the chemical reaction of the preparation method is limited in one container, the operation is simple, precise control of the reaction conditions is easier, and proprieties of products in batch production are more stable.

A method for producing sulfide glass wherein phosphorus sulfide satisfying the following formula (1) is used as a raw material:100×A / B≧37   (1)wherein in the formula, A is peak areas of peaks that appear at peak positions in a range of 57.2 ppm or more and 58.3 ppm or less, and 63.0 ppm or more and 64.5 ppm or less in 31PNMR spectroscopy, and B is the total of peak areas of all peaks measured in 31PNMR spectroscopy.

The invention is suitable for the technical field of electro-catalysis, and provides a transition metal phosphorus sulfide and a preparation method and application thereof. The preparation method of the transition metal phosphorus sulfide comprises the following steps of mixing nickel nitrate, cobalt nitrate, urea and ammonium fluoride and preparing a solution to obtain a precursor solution; adding foamed nickel into the precursor solution for hydrothermal reaction to obtain a precursor; and under a protective atmosphere, placing the precursor in an environment containing sodium hydrosulfide and sodium hypophosphite, and carrying out calcination treatment to obtain the transition metal phosphorus sulfide. According to the preparation method, a nickel-cobalt hydroxide precursor is generated through a hydrothermal method, then a phosphorus source and a sulfur source are doped at the same time in a protective gas heating mode, and S and P can be induced to generate a heterostructure. Due to the synergistic effect of different elements, the structure accelerates electron transmission, so that the conductivity of the transition metal phosphorus sulfide can be improved, and the advantages show high catalytic activity and long-acting stability in an electro-catalysis test.

The invention discloses a lithium sulfide solid electrolyte material of silver-containing halogen compound composite powder and a preparation method thereof. The preparation method comprises the steps of 1) weighing 35-50% lithium sulfide and the balance of phosphorus sulfide according to weight percentage under the condition of atmosphere protection, and mixing the lithium sulfide and the phosphorus sulfide uniformly to obtain a lithium-sulfur-phosphorus ternary mixture; 2) taking the lithium-sulfur-phosphorus ternary mixture, silver iodide which accounts for 2-6% by weight of the lithium-sulfur-phosphorus ternary mixture, silver bromide which accounts for 1-3% by weight of the lithium-sulfur-phosphorus ternary mixture and silver chloride which accounts for 1-3% by weight of the lithium-sulfur-phosphorus ternary mixture, putting the taken materials in a ball milling pot to obtain an amorphous lithium-sulfur-phosphorus mixture containing silver iodide, silver bromide and silver chloride; and 3) sealing the amorphous lithium-sulfur-phosphorus mixture containing silver iodide, silver bromide and silver chloride under the condition of atmosphere protection and red light, and then heating the mixture to 60-180 DEG C under a vacuum or atmosphere protection condition for heat treatment so as to obtain the lithium sulfide solid electrolyte material of the silver-containing halogen compound composite powder.

A method for preparing a solid electrolyte for an all-solid state battery, may include obtaining a slurry by dispersing a first raw material comprising lithium sulfide; and a second raw material selected from the group consisting of silicon sulfide, phosphorus sulfide, germanium sulfide, boron sulfide, and a combination thereof in a solvent; and drying the slurry.

The invention relates to a transition metal phosphorus sulfide active phase preparation method, which comprises: treating a VI group and VIII group covalent transition metal phosphide catalyst by using an organic sulfur-containing compound containing alkyl or cycloalkyl C-S bond as a vulcanizing agent in an inert atmosphere to prepare the phosphorus sulfide active phase, wherein the transition metal phosphide is prepared by using a transition metal phosphate as a precursor through temperature-programmed reduction in a hydrogen atmosphere. Compared with the existing transition metal phosphorussulfide preparation method, the preparation method of the present invention does not require expensive and dangerous hydrogen, does not require or generate highly toxic H2S gas, and further has advantages of safety, low cost and good application prospect in industry.

The invention discloses a synthesis method of an alkali metal salt containing sulfonyl chloride or phosphorus imide: the alkali metal salt is prepared by subjecting compound (V-2) and sulfuryl chloride or phosphorus oxychloride to nucleophilic substitution under the presentation of acid binding agents; the invention further discloses a synthesis method of an alkali metal salt containing fluorine sulfonyl or phosphorus imide, the alkali metal salt is prepared by reacting (sulfonyl chloride) (perfluorinated alkyl) imide salt (V-1) or (dichloro phosphoryl) (perfluorinated alkyl sulfonyl) imide salt (V-2) with fluorinated reagents. The synthesis methods have the advantages that the experiment condition is mild, and the used materials are convenient to store and prepare; the preparation rate is high, the purification is simple, the preparation cost is low, and the methods are suitable for mass industrial preparation. The preparation rate and the purity of the resultants are high, and the resultants can be used as lithium salt electrolyte materials for lithium batteries, or for preparing catalytic agents, and for synthesizing high-performance ionic liquids.

The invention discloses a polymer containing membrane for hydrometallurgy separation of precious metals, base metals and rare elements, and belongs to the technical field of metallurgy. The polymer containing membrane is prepared from the raw materials of PVC, an extracting agent and NPOE, and the extracting agent is tris(2-methylpropyl)phosphorus sulfide and tris(2-ethylhexyl)amine at the mass ratio of (1.36-1.56): 1. A preparation method comprises the steps of dissolving the PVC, the NPOE and the extracting agent in a volatile polar solvent, stirring for reaction to obtain a solution, pouring the solution into a container after the reaction is completed, and standing at 24-26 DEG C until the volatile polar solvent is completely volatilized so as to obtain the polymer containing membrane. The polymer containing membrane is capable of efficiently and selectively separating the precious metals and rare metals contained in base metal ore deposits, excellent in mechanical property and recycling performance and flexible in separation method, and has important popularization value in the field of hydrometallurgy.

The present invention provides a method of preparing a phosphonium salt of the formula [R1R2R3P—CR4R5R6]X, comprising ball-milling a phosphine of the formula R1R2R3P with a compound of the formula XCR4R5R6; a method of preparing a phosphorus ylide of the formula R1R2R3P═CR4R5, comprising ball-milling a phosphonium salt of the formula [R1R2R3P—HCR4R5]X in the presence of a base; and a method of preparing an olefin of the formula R4R5C═CR7H or R4R5C═CR7R8, comprising ball-milling a phosphorus ylide of the formula R1R2R3P═CR4R5 with a compound of the formula R7C(O)H or R7C(O)R8. The inventive method produces phosphonium salts and phosphorus ylides by mechanical processing solid reagents under solvent-free conditions. The advantages of the present invention over conventional solution methods, include: (1) extremely high selectivity; (2) high yields; (3) low processing temperatures; (4) simple and scalable reactions using commercially available equipment; and (5) the complete elimination of solvents from the reaction.

A method of synthesis of lithium titanium thiophosphate LiTi2(PS4)3 including the steps of: (a) providing a mixture of lithium sulfide Li2S, phosphorus sulfide P2S5 and titanium sulfide TiS2; (b) subjecting the mixture prepared in step (a) to a preliminary reaction step through mechanical milling or melt-quenching to produce an intermediate amorphous sulfide mixture; (c) subjecting the mixture prepared in step (b) to a heat treatment step at a maximum plateau temperature of at least 350° C. and less than 500° C.

The invention discloses a lithium sulfide series solid electrolyte material added with lithium silicon alloy and silver iodide and a preparation method thereof. The preparation method comprises the following steps that (1) under the atmosphere protection condition, lithium sulfide, phosphorus sulfide, lithium silicon alloy powder and sulfur are weighed according to a mole ratio of (2.5 to 3.5) to (0.5 to 1.0) to (0.05 to 0.20) to (0.01 to 0.1); the materials are uniformly mixed to obtain a lithium sulfur phosphorus and silicon mixture; (2) under the conditions of atmosphere protection and safe red light, the lithium sulfur phosphorus and silicon mixture and the silver iodide accounting for 1 to 5 percent of the mass of the lithium sulfur phosphorus and silicon mixture are taken to be put into a ball milling tank and are subjected to ball milling to obtain an amorphous state lithium sulfur phosphorus and silicon mixture containing the silver iodide; (3) the obtained amorphous state lithium sulfur phosphorus and silicon mixture containing the silver iodide is sealed under the atmosphere protection condition; then, the temperature is raised to 120 to 200 DEG C under the vacuum condition; heat treatment is performed; the lithium sulfide series solid electrolyte material is obtained. The lithium ion conductivity of the obtained solid electrolyte material can be improved through simultaneously adding the lithium silicon alloy and the silver iodide.

The invention belongs to the technical field of sodium-ion batteries, and particularly discloses a three-dimensional composite negative electrode material of a sodium-ion battery as well as a preparation method and application of the three-dimensional composite negative electrode material. The three-dimensional composite negative electrode material FePS3 / rGO of the sodium ion battery has a lamellar structure, and tiny FePS3 nanosheets are uniformly attached to the surface of a rGO lamellar layer. FePS3 is a ternary transition metal phosphorus sulfide and has a special two-dimensional layered structure, the layers are combined by Van der Waals force, and the structure is beneficial to the rapid movement and storage of sodium ions between the layers. According to the present invention, FePS3 and rGO are compounded, so that volume expansion of the FePS3 material in a reaction process is effectively buffered, the rapid transfer of electrons / ions is promoted, and a longer cycle life can be realized on the premise of keeping higher specific capacity. Meanwhile, the improvement of the stability of a material system also greatly enhances the rate capability of the material, and the sodium ion battery prepared from the material has high discharge capacity and excellent rate capability.

The invention discloses a preparation method and application of a phosphorus cobalt nickel sulfide heterostructure nanosheet, and relates to a preparation method of phosphorus cobalt nickel sulfide. The invention aims to solve the problems that phosphorus and sulfur elements in a phosphorus and sulfur-containing material synthesized by the existing method are relatively low, the synergistic effect between phosphorus and sulfur substances is reduced, and the capacitive performance is low when the material is used as an electrode material. The method comprises the following steps: 1, preparing reaction liquid I; 2, preparing a reaction liquid II; 3, preparing a reaction solution III; 4, carrying out hydrothermal reaction; 5, centrifuging and cleaning; and 6, phosphating treatment. The phosphorus sulfide cobalt nickel heterostructure nanosheet is used as an electrode material. The phosphorus sulfide cobalt nickel heterostructure nanosheet prepared by the invention is a potential candidate of a supercapacitor positive electrode material, and has a wide application prospect. According to the preparation method, the nickel cobalt phosphorus sulfide heterostructure nanosheet can be obtained.

The invention provides a preparation method of a palladium catalyst, the catalyst and application. The catalyst is prepared by directly using aromatic compounds containing phosphorus and sulfur substituents, such as triphenylphosphine sulfur, diphenyl phosphorus hydrosulfide and the like, as modifiers to modify Pd or Pd / X with a carrier. The amount of modifiers for preparing the catalyst is low and the preparation method is simple and convenient; the prepared catalyst has efficient and stable catalytic activity and can be used for alkyne semi-hydrogenation reaction, wherein high selectivity isachieved on terminal alkyne compound semi-hydrogenation, and industrial application is facilitated.

The invention relates to the technical field of catalysts. The invention discloses a sulfur defect-rich sulfurized ferrophosphorus nanosheet as well as a preparation method and application thereof. The preparation method includes following steps: stripping the blocky phosphorus sulfide into phosphorus sulfide nanosheets by adopting an electrochemical stripping method; respectively carrying out low-speed centrifugal separation and high-speed centrifugal separation; washing and drying the product, and calcining the product to obtain a phosphorus sulfide nanosheet rich in sulfur defects. According to the invention, the nanosheet has good electrochemical performance and stability, when the nanosheet is applied to electrochemical nitrogen fixation ammonia synthesis, the maximum ammonia synthesis rate can reach 6.27 [mu]g*h<-1>mg<-1>cat; the preparation method has the advantages of being simple, efficient, low in cost, high in controllability, good in reproducibility and suitable for industrial production.

The invention discloses a sulfur-phosphorus co-doped in-situ growth graphene coated nickel-cobalt-iron hydrogen evolution catalyst, which is composed of Ni, Co, Fe, S and P in the form of phosphorus sulfide, is loaded on carbon paper, and has the general formula of (NixCoyFez) SvPu@CP, in the formula, x / y is more than or equal to 0 and less than or equal to 10, x / z is more than or equal to 0 and less than or equal to 10, v is more than or equal to 0 and less than or equal to 10, and u is more than or equal to 0 and less than or equal to 10. In addition, the invention further discloses a preparation method of the sulfur-phosphorus co-doped in-situ growth graphene coated nickel-cobalt-iron hydrogen evolution catalyst. The integrated (NixCoyFez) SvPu@CP catalyst electrode shows very prominent HER activity, has higher catalytic activity, higher hydrogen yield and more stable performance, can be widely applied to various hydrogen evolution electrolysis water catalysis, and has the advantages of energy conservation, environmental protection and low cost.

The invention discloses a lithium sulfide series solid electrolyte material added with lithium tin alloy and a preparation method thereof. The preparation method comprises the following steps that (1) under the atmosphere protection condition, lithium sulfide, phosphorus sulfide, lithium tin alloy powder and sulfur are weighed according to a mol ratio of (2.5 to 4.0):(0.5 to 1.0):(0.02 to 0.1):(0.01 to 0.05); the materials are uniformly mixed to obtain an amorphous lithium sulfur phosphorus and tin mixture; (2) the amorphous lithium sulfur phosphorus and tin mixture is sealed under the atmosphere protection condition; then, the temperature is raised to 120 to 260 DEG C under the vacuum or atmosphere protection condition; heat treatment is performed; the lithium sulfide series solid electrolyte material is obtained. The concentration of migratable lithium irons in the lithium sulfide series solid electrolyte is improved through adding the high-lithium-content lithium tin alloy capable of easily forming the amorphous state, so that the lithium ion conductivity is improved.

The invention relates to an inorganic compound as well as a preparation method and application thereof. The chemical formula of the inorganic compound is AgGa2PS6 and belongs to a monoclinic crystal system; the inorganic compound has a space group Cc, and a single cell parameter shown in the description, wherein alpha is equal to gamma and is 90 degrees, beta is 106.5 to 108.5 degrees and Z is 4.The inorganic compound is prepared by adopting a vacuum high temperature solid phase method; a power frequency multiplication (SHG) coefficient of the inorganic compound is one time that of AgGa2S2(AGS).

The invention discloses a lithium sulfide solid electrolyte material with lithium tin alloy and silver chloride and preparation method therefor. The preparation method comprises the following steps of: 1) under the condition of atmosphere protection, weighing and taking the lithium sulfide, phosphorus sulfide, lithium tin alloy powder and sulphur with a mole ratio of 2.5-4.0:0.5-1.0:0.02-0.1:0.01-0.05, and mixing evenly so as to obtain a lithium-sulfur-phosphorus-tin mixture; 2) under the conditions of atmosphere protection and safe red light, taking the lithium-sulfur-phosphorus-tin mixture and the silver chloride of which the quality is equivalent to 1-5% of the quality of the mixture, and putting into a ball mill tank for ball milling so as to obtain an amorphous lithium-sulfur-phosphorus-tin mixture containing the silver chloride; and 3) carrying out sealing on the amorphous lithium-sulfur-phosphorus-tin mixture containing the silver chloride obtained under the condition of atmosphere protection; and carrying out heat treatment under the condition of vacuum by heating up to 80-150 DEG C, thus obtaining the lithium sulfide solid electrolyte material with lithium tin alloy and silver chloride. According to the lithium sulfide solid electrolyte material with lithium tin alloy and silver chloride and preparation method therefor, the lithium tin alloy and the silver chloride are added simultaneously, so that lithium ion conductivity of the solid electrolyte material obtained can be improved.

The invention discloses a lithium sulfide solid electrolyte material with the addition of lithium-tin alloy and silver bromide and a preparation method thereof. The preparation method comprises the following steps: (1) weighing lithium sulfide, phosphorus sulfide, lithium-tin alloy powder and sulfur according to a molar ratio of (2.5 to 4.0) to (0.5 to 1.0) to (0.02 to 0. 1) to (0.01 to 0.05) under an atmosphere protection condition, and uniformly mixing, thus obtaining a lithium-sulfur-phosphorus-tin mixture; (2) taking and putting the lithium-sulfur-phosphorus-tin mixture and the silver bromide which accounts for 1 to 5 percent of the lithium-sulfur-phosphorus-tin mixture in mass percentage in a ball-milling tank under atmosphere protection and safe red light conditions, and carrying out ball milling, thus obtaining an amorphous lithium-sulfur-phosphorus-tin mixture containing the silver bromide; (3) sealing the amorphous lithium-sulfur-phosphorus-tin mixture containing the silver bromide under the atmosphere protection condition, and heating to 60 to 150 DEG C under a vacuum condition for carrying out thermal treatment, thus obtaining the lithium sulfide solid electrolyte material. According to the preparation method disclosed by the invention, the lithium ionic conductivity of the obtained lithium sulfide solid electrolyte material is increased by simultaneously adding the lithium-tin alloy and the silver bromide.

The present invention relates to a new and simple purification process of phosphorus decasulfide (P4S10), also called phosphorus pentasulfide (P2S5), which is used as thionating agent for the syntheses of various organic compounds, particularly the organic compounds having sulfur heteroatom(s).