25 results about "Phosphorus pentasulfide" patented technology

The invention provides a sulfide electrolyte material and a preparation method and application thereof, and the preparation method comprises the following steps: mixing lithium sulfide, phosphorus pentasulfide, rare earth sulfide and a solvent, and reacting to obtain a sulfide electrolyte precursor; and carrying out pressing treatment on the sulfide electrolyte precursor, and carrying out low-temperature sintering on the material obtained by pressing at 250-500 DEG C to obtain the sulfide electrolyte material. According to the method disclosed by the invention, the synthesis of the rare earth element doped sulfide precursor is realized by adopting a pure liquid phase method, particles are dispersed in a liquid phase solvent, and the particle uniformity and dispersity of the obtained finished product are obviously superior to those of a solid phase method. After the precursor obtained by the liquid phase method is pressed and sintered at low temperature, the crystal boundary between crystals of the electrolyte material is relatively small, the energy barrier of ion transmission is remarkably enhanced, the conductivity of the electrolyte is optimized, and the long-cycle stability of the all-solid-state battery is improved.

The invention discloses a synthesis method of lithium phosphorus sulfur chloride, and relates to the technical field of preparation of sulfide solid electrolyte for all-solid-state lithium ion batteries, and the scheme is as follows: the synthesis method of lithium phosphorus sulfur chloride comprises the following steps: pretreatment of raw materials: mixing lithium carbonate (Li2CO3), phosphorus pentasulfide (P2S5), lithium chloride (LiCl) and elemental sulfur (S) according to a preset ratio, and then adding a catalyst, grinding and dispersing for a preset time to obtain uniformly dispersed mixed powder; reduction reaction: fully mixing the mixed powder with a reducing agent, heating to a first preset temperature condition, and carrying out reduction reaction to obtain a reduction product; sintering and purifying: heating the reduction product to a second preset temperature, and sintering to form a lithium phosphorus sulfur chloride (Li6PS5Cl) crystal phase to obtain a lithium phosphorus sulfur chloride (Li6PS5Cl) product; the raw material cost can be remarkably reduced, the process safety and economy are optimized, and large-scale industrial preparation of lithium phosphorus sulfur chlorine is realized.

This invention relates to a method for preparing high-purity phosphorus pentasulfide using a low-temperature liquid phase and its application, belonging to the technical field of key materials for lithium-sulfur batteries and solid-state batteries. It solves the technical problems of high reaction temperature and high energy consumption in existing phosphorus pentasulfide preparation processes. The method includes the following steps: Step 1: Select phosphorus pentachloride, dry it, and place the treated phosphorus pentachloride in an organic solvent to form a suspension or slurry system; Step 2: Place the suspension or slurry system in a closed reactor; Step 3: Introduce a sulfur source into the reactor to allow phosphorus pentachloride to undergo a sulfidation reaction with the sulfur source; Step 4: Raise the temperature to a set point and maintain a deep sulfidation reaction to generate phosphorus pentasulfide; Step 5: After the reaction, cool, separate the solid and liquid phases, and dry to obtain the solid product of phosphorus pentasulfide. This invention features mild reaction conditions, a simplified process flow, high safety, and recyclable solvents, making it suitable for continuous and large-scale production.

A method of making a solid-state electrode sheet is provided. The method includes mixing precursors capable of chemically reacting to form a target solid-state electrolyte (SSE) together with one or more of a binder, an electrode active material, and a conductive carbon in a solvent to form a coating slurry. The precursors a undergoes a chemical reaction in the solvent to form the target SSE. The coating slurry is applied onto a current collector. The solvent is evaporated from the coating slurry on the current collector, thereby producing a solid-state electrode sheet having a target SSE. The precursors may be lithium sulfide (Li2S) and phosphorus pentasulfide (P2S5) reacting in a tetrahydrofuran (THF) solvent to produce a sulfide-base SSE such as Li3PS4.

The invention belongs to the technical field of wet-process phosphoric acid purification, and provides a method for efficiently removing arsenic from wet-process phosphoric acid. According to the method, wet-process phosphoric acid is mixed with an arsenic removal agent A and an arsenic removal agent B for reaction, and efficient arsenic removal of wet-process phosphoric acid is completed; the arsenic removal agent A comprises one or more of phosphorus pentasulfide, hydrogen sulfide and sodium sulfide; and the arsenic removal agent B comprises one or more of a sulfate salt anionic surfactant, a sulfonate anionic surfactant and a carboxylate anionic surfactant. The method is simple, environment-friendly and low in production and operation cost, the sulfide and the anionic surfactant are used as the composite arsenic removal agent, the arsenic removal efficiency is improved, the use amount of the arsenic removal agent is greatly reduced, the advantage of arsenic removal of the sulfide is reserved, the defect of rapid decomposition of the sulfide is overcome, escape of H2S is reduced, and the method is suitable for industrial production. The safety is higher, and the application prospect is very wide.

The invention belongs to the technical field of solid electrolyte, and provides a method for regenerating sulfide solid electrolyte, which is characterized by comprising the following steps: (S1) mixing Li2S (lithium sulfide), P2S5 (phosphorus pentasulfide) and sulfide solid electrolyte waste powder to obtain regenerated powder; (S2) carrying out heat treatment on the regenerated powder to obtain a sintered body; and (S3) molding the sintered body to obtain the regenerated sulfide solid electrolyte, because the regenerated sulfide solid electrolyte does not contain LiCl, it can be ensured that the regenerated sulfide solid electrolyte has high ionic conductivity, and the prepared battery has excellent electrochemical performance.

The invention provides a preparation method of an LMPSC sulfide solid electrolyte, which comprises the following steps: adding an additive into a main raw material, calcining and doping metal elements to obtain the LMPSC sulfide solid electrolyte, wherein the main raw materials comprise phosphorus pentasulfide, lithium sulfide and lithium chloride; the additive is metal chloride. The invention further provides the obtained LMPSC sulfide solid electrolyte and application of the LMPSC sulfide solid electrolyte in a power automobile. According to the preparation method, by introducing metal elements, the LMPSC sulfide solid electrolyte capable of providing capacity and transmitting Li < + > can be obtained.

This invention discloses a dithiophosphoryl-substituted azine compound and its synthetic method, belonging to the field of organic synthesis technology. The synthetic method uses azine compounds, phosphorus pentasulfide, and alcohols as substrates. In a membrane-free electrolytic cell, using tetrabutylammonium bisulfate as the electrolyte and acetonitrile as the solvent, a three-component dehydrogenation coupling reaction is achieved by constant current electrolysis at room temperature. No metal catalyst or external chemical oxidant is required. Inexpensive phosphorus pentasulfide serves as both the sulfur and phosphorus source. By controlling the electrolysis time, mono- or bis-dithiophosphoryl-substituted azine compounds can be selectively prepared with moderate to excellent product yields. Mechanistic studies show that the reaction proceeds via a free radical-mediated pathway. This method is mild, simple to operate, and has a wide range of applicable substrates, meeting the requirements of green chemistry and providing a new route for the efficient synthesis of functionalized phenoxazine derivatives.

The invention provides a preparation method of an LPSC sulfide solid electrolyte, which comprises the following steps: (1) adding an additive into a main raw material, and calcining for Si doping to obtain a first sintered material; wherein the main raw material is a first raw material and comprises phosphorus pentasulfide, lithium sulfide and lithium chloride; the additive is a first additive and is a Si-containing compound; (2) repeating the step (1) by taking a second raw material as a main raw material and taking a second additive as an additive to perform CaF2 coating to obtain a secondary sintered material, namely an LPSC sulfide solid electrolyte; wherein the second raw material is a sintered material; and the second additive is CaF2. The invention further provides the obtained LPSC sulfide solid electrolyte and application of the LPSC sulfide solid electrolyte in a power automobile. According to the preparation method, the high-chlorine LPSC sulfide solid electrolyte is subjected to secondary sintering and CaF2 coating treatment, and the prepared LPSC sulfide solid electrolyte has the dual effects of high magnification and low side reaction.

This invention relates to the field of solid-state lithium battery technology, and in particular to a method for preparing a sulfide solid electrolyte. The method includes the following steps: under an inert atmosphere, lithium sulfide, sulfur, red phosphorus, and lithium chloride are mixed; the mixed raw materials are ball-milled to obtain a precursor; and the precursor is then sintered, cooled, and ground to obtain the sulfide solid electrolyte. The sulfide solid electrolyte preparation method provided by this invention allows the in-situ generated P2S5 to bind more tightly with surrounding substances during the formation of lithium phosphorus, sulfur, and chloride, thus improving product purity. Using sulfur and red phosphorus instead of phosphorus pentasulfide provides readily available and cost-effective raw materials, avoids the toxicity of phosphorus pentasulfide, and further avoids the risk of severe exothermic reactions caused by localized overheating when directly using P2S5.

The utility model provides a cyclone dust removal device suitable for phosphorus pentasulfide feeding, which comprises a cyclone dust removal device body, and a main pipeline is arranged at the end part of an exhaust pipe of the cyclone dust removal device body and is used for guiding clean airflow to be discharged to form negative pressure in the cyclone dust removal device body. Inert gas is introduced into the cyclone dust collector body through the main pipeline when materials are discharged, a three-way reversing valve is arranged at one end of the main pipeline, a breather pipe is connected to one connector of the three-way reversing valve and used for introducing the inert gas into the main pipeline, one end of the breather pipe is connected with a gas outlet of an inert gas storage tank, and the other end of the breather pipe is connected with a gas outlet of the inert gas storage tank. According to the utility model, the main pipeline is matched with the adjustment of the electric three-way ball valve, so that positive pressure is formed in the cyclone dust collector body, phosphorus pentasulfide dust can be conveniently discharged and recycled, reentrainment of dust is inhibited, phosphorus pentasulfide is prevented from being hydrolyzed with moisture in the air, the safe operation of equipment is guaranteed, and the risk of environmental pollution is reduced.

The application relates to a method for preparing high-purity phosphorus pentasulfide in a low-temperature liquid phase and application thereof, and belongs to the technical field of key materials for lithium-sulfur batteries and solid-state batteries. The method solves the technical problems of high reaction temperature and large energy consumption in the existing preparation process of phosphorus pentasulfide. The method comprises the following steps: step 1, selecting phosphorus pentachloride, drying the phosphorus pentachloride, and placing the treated phosphorus pentachloride in an organic solvent to form a suspension phase or a slurry system; step 2, placing the suspension phase or the slurry system in a closed reactor; step 3, introducing a sulfur source into the reactor to make the phosphorus pentachloride and the sulfur source undergo a sulfuration reaction; step 4, keeping the deep sulfuration reaction after being heated to a set temperature to generate phosphorus pentasulfide; and step 5, cooling, solid-liquid separation and drying after the reaction to obtain a phosphorus pentasulfide solid product. The application has the advantages of mild reaction conditions, simplified process flow, high safety, recyclable solvent and suitability for continuous and large-scale production.

This invention proposes a fully sulfurized DOPO flame retardant, its preparation method, and its application. The preparation method of the fully sulfurized DOPO flame retardant includes the following steps: reacting 2-mercapto[1,1'-biphenyl], trifluoromethanesulfonic acid, and phosphorus trichloride to introduce a cyclic Cl-P-S bond, then reacting with water to replace Cl with O, yielding a semi-sulfurized DOPO flame retardant; reacting the semi-sulfurized DOPO flame retardant, anhydrous toluene, and phosphorus pentasulfide to replace O with S, yielding a fully sulfurized DOPO flame retardant. This invention replaces the oxygen element that supports combustion in DOPO with sulfur, which has flame-retardant properties, thus synthesizing a fully sulfurized DOPO flame retardant with better flame-retardant effects.

The invention relates to the technical field of all-solid-state lithium battery materials, and discloses a manufacturing method and application of a high-performance sulfide solid electrolyte which comprises the following components in parts by mole: 2.50-2.90 parts of lithium sulfide, 0.10-0.40 part of phosphorus pentasulfide, 0.20-0.80 part of germanium disulfide and 0.80-1.20 parts of lithium chloride. The manufacturing method comprises the following steps: carrying out ball milling on raw materials in an inert atmosphere to obtain amorphous precursor powder; sealing the amorphous precursor powder in a carbon coating quartz tube for vacuum constant-temperature heat treatment; and controlling the heating device to slowly reduce the temperature to below 200 DEG C after the heat treatment is finished. According to the invention, a lithium ion transmission channel is expanded through multi-element co-doping, and the crystallinity is improved and the grain boundary impedance is reduced in cooperation with a controlled slow cooling process. The obtained high-performance sulfide solid electrolyte has high ionic conductivity and excellent electrochemical stability, and is suitable for preparing an all-solid-state battery with a wide voltage window.

The invention provides a solid sulfide electrolyte and a preparation method thereof. The preparation method of the solid sulfide electrolyte comprises the following steps: S1, mixing phosphorus pentasulfide, lithium sulfide, lithium chloride and a first solvent, and carrying out ball milling to obtain a precursor; s2, performing heat treatment on the precursor to obtain precursor powder; s3, performing tabletting treatment on the precursor powder to obtain a flaky precursor; s4, sintering the flaky precursor in an inert protective atmosphere to obtain a sintered product; s5, mixing the sintered product with a second solvent, and performing graded liquid-phase grinding to obtain a graded grinding final product; and step S6, carrying out heat treatment on the graded grinding final product to obtain the solid sulfide electrolyte. According to the preparation method of the solid-state sulfide electrolyte, the particle consistency of the solid-state sulfide electrolyte product can be improved through the synergistic effect of tabletting treatment and graded liquid-phase grinding.

The safe and environment-friendly storage and transportation device comprises a storage box, the upper portion of the storage box is provided with an air inlet and a feeding port, the bottom of the storage box is provided with a discharging port, the air inlet is provided with a quick connector, and one end of the quick connector is connected with a breather pipe. The nitrogen inlet is arranged in the storage box and used for introducing inert gas into the storage box to form inert gas protection in the storage box, a rotary valve is arranged at the feed port, a connecting pipe is arranged at the feed end of the rotary valve, a sealing cover is arranged at the upper end of the connecting pipe, and an exhaust valve is arranged at the upper part of the storage box. A dynamic inert gas protection layer is formed to isolate outside moisture and oxygen, the hydrolysis reaction of phosphorus pentasulfide is remarkably inhibited, corrosive phosphoric acid and highly toxic hydrogen sulfide gas are prevented from being generated, the caused explosion risk is avoided, and transportation safety and stable chemical properties of materials are guaranteed.

This invention provides a flotation collector for high-sulfur complex lead-zinc polymetallic ores, its preparation method, and its application. The collector is N,N'-dibromophenyl dithioaminophosphate, prepared by reacting o-bromoaniline with phosphorus pentasulfide in toluene. This collector exhibits strong collecting ability, good selectivity, non-sticky flotation froth, low middlings recycling volume, and strong adaptability for lead sulfide minerals. It is convenient to use, requires a small dosage, and simplifies the flotation process, reducing flotation costs and environmental impact, thus achieving better flotation separation of high-sulfur lead-zinc ores. Furthermore, this collector can also recover various associated gold and silver minerals in high-sulfur complex lead-zinc polymetallic ores, demonstrating broad applicability and strong adaptability, especially for fine-grained associated gold and silver minerals with a particle size less than 37 μm, exhibiting strong collecting ability and good selectivity.

This invention belongs to the technical field of solid electrolytes and discloses a method for preparing a liquid-phase doped silver-germanium sulfide solid electrolyte with high ionic conductivity. The method includes: 1) dispersing lithium sulfide and phosphorus pentasulfide in an organic solvent, heating and stirring to obtain a precursor solution containing Li3PS4; 2) mixing lithium iodide, sulfur powder, and additives with the precursor solution, heating and stirring to remove the organic solvent, and obtaining a powder; 3) sintering the powder under a protective atmosphere to obtain a silver-germanium sulfide solid electrolyte; the additives are one or more of SiS2, GeS2, SnS2, As2S3, and Sb2S3. This invention is simple, and the prepared silver-germanium sulfide electrolyte undergoes elemental doping during thermal crystallization, improving the electrolyte's ionic conductivity and air stability. This method is suitable for industrial production.

The invention relates to a preparation method of a lithium-containing sulfide, lithium thiophosphate and a sulfide solid electrolyte. The preparation method comprises the following steps: providing a first raw material containing liquid phosphorus pentasulfide and / or liquid sulfur and a second raw material containing a lithium element; wherein the second raw material containing the lithium element comprises lithium sulfide powder or liquid lithium; in an inert gas atmosphere, the first raw material and the second raw material are contacted and react in a reactor; the reaction temperature ranges from 280 DEG C to 500 DEG C. According to the method, the liquid phosphorus pentasulfide and the second raw material containing the lithium element are contacted and react at a relatively low temperature, so that the problem of low purity possibly caused by a grinding process is avoided, the lithium-containing sulfide with high purity and controllable particle size can be obtained through rapid, continuous and large-scale production, and the production cost is reduced.

The application discloses a preparation method of a 2'-iodo[1,1'-biaryl]-2-dithiophosphate compound, wherein phosphorus pentasulfide, alcohol, dianyl trifluoromethanesulfonic acid periodate, an organic ligand, a base, a catalyst and an organic solvent are mixed in a reaction container under an air atmosphere, and the mixture is reacted under stirring at 25-100 DEG C for 6-12 hours to obtain the corresponding 2'-iodo[1,1'-biaryl]-2-dithiophosphate compound. The application provides a method for efficiently and selectively synthesizing 2'-iodo[1,1'-biaryl]-2-dithiophosphate compounds by copper catalysis of phosphorus pentasulfide, alcohol and dianyl trifluoromethanesulfonic acid periodate. The reaction process is mild and easy to control. The method is simple and easy to implement, the catalyst is cheap and easy to obtain, the preparation is simple, and the method has a good industrial application prospect.

The present invention provides a sulfide electrolyte and a preparation method and application thereof, and relates to the technical field of all-solid-state batteries, and the preparation method comprises the following steps: a phosphorus source, a sulfur source, a halogen source and a first additive are mixed to obtain a first mixture, the first additive comprises a phosphorus-sulfur compound, and the phosphorus-sulfur compound is less than the phosphorus source as a raw material, and is less than the phosphorus source as a raw material. The polymer has an irregular molecular structure; carrying out primary calcination on the first mixture to obtain a first calcined material; the first sintered material is mixed with a second additive to obtain a second mixture, and the second additive comprises a metal oxide; and carrying out secondary calcination on the second mixture to obtain the sulfide electrolyte. The method comprises the following steps: modifying LPSC particles by using a first additive (preferably phosphorus pentasulfide) to regulate and control electron cloud distribution in unit cells for the first time, modifying again by using a multi-metal element high-entropy process to regulate and control electron cloud distribution, and effectively improving the steady state of LPSC through two times of modification.

The utility model provides an intensified refined phosphoric acid arsenic removal device which comprises a hydrolysis tank and a multi-stage intensified refining tower which are connected in sequence, a plurality of intensified units are vertically arranged in the multi-stage intensified refining tower, a gas outlet is formed in the top of the multi-stage intensified refining tower, and a gas outlet is formed in the bottom of the multi-stage intensified refining tower. A liquid phase feeding hole and a gas inlet are formed in the bottom of the multi-stage enhanced refining tower, a circulating feeding hole is also formed in the middle section of the multi-stage enhanced refining tower, and a discharging hole is formed in the bottom of the multi-stage enhanced refining tower; a phosphorus pentasulfide feeding hole and a water inlet are formed in the bottom of the hydrolysis tank, a strengthening unit is arranged at the bottom in the hydrolysis tank, and a hydrogen sulfide outlet is formed in the top of the hydrolysis tank. According to the utility model, the contact area between raw materials is strengthened by using the multi-stage strengthening refining tower, the mass transfer efficiency and the reaction efficiency are improved, the raw materials are converted into microbubbles through the strengthening unit while the hydrolysis of the raw materials is accelerated, so that the retention time between the raw materials is greatly prolonged, and the arsenic removal reaction is fully carried out.

This invention relates to a method for deep removal of heavy metals in a wet-process phosphoric acid process, comprising the following steps: (1) using a straight-chain or branched alcohol as a raw material, reacting it with phosphorus pentasulfide to obtain dialkyl dithiophosphate, and then reacting it with metal oxides, hydroxides or salts to synthesize dialkyl dithiophosphate (DDP); (2) reacting the DDP with one or more of the following: phosphoric acid slurry containing heavy metals, dilute phosphoric acid, concentrated phosphoric acid, and residual acid from phosphoric acid purification, to generate a heavy metal complex precipitate. After the reaction is complete, the purified phosphoric acid is separated to achieve the removal of heavy metals. This method has low raw material costs, and the cadmium content after heavy metal removal of phosphoric acid is ≤2ppm with a removal rate ≥96%; the copper content is ≤0.5ppm with a removal rate ≥99.5%; the arsenic content is ≤5ppm with a removal rate ≥70%; phosphorus loss is ≤0.5%; no reducing agent is required, thus avoiding hydrogen generation; it has little impact on the decrease in phosphoric acid concentration; and no H2S is generated. It is suitable for the removal of heavy metals from wet-process phosphoric acid slurry, dilute phosphoric acid, concentrated phosphoric acid, and other systems, and can be directly integrated into existing production lines.

This invention discloses an arsenic removal process for producing 105% polyphosphoric acid using the thermal method, belonging to the field of phosphoric acid production technology. The invention includes the following steps: (1) Preparation of the arsenic removal agent solution: Polyvinylpyrrolidone, water, and phosphorus pentasulfide are mixed to obtain an arsenic removal agent solution; (2) Primary arsenic removal: The arsenic removal agent solution is added to 107% polyphosphoric acid for arsenic removal reaction; (3) Preparation of arsenic removal agent microspheres: Sodium hydroxide, water, metakaolin, and rice bran are mixed to obtain a suspension, which is then dripped into white oil, filtered, washed, dried, calcined, and sieved to obtain arsenic removal agent microspheres; (4) Secondary arsenic removal using the arsenic removal agent microspheres; (5) Filtration. The arsenic removal process of this invention can reduce the arsenic content in 105% polyphosphoric acid produced by the thermal method to below 0.5 PPM, meeting the needs of special industries such as lithium hexafluorophosphate electrolyte, pharmaceutical synthesis, electronics, and food in domestic and international markets.

The invention provides a preparation method of an LPSC sulfide solid electrolyte, which comprises the following steps: (1) adding an additive into a main raw material, calcining and doping selenium to obtain a first sintered material; the main raw materials comprise phosphorus pentasulfide, lithium sulfide and lithium chloride; the additive is selenium dioxide; (2) taking the primary sintered material as a main raw material, taking a metal oxide as an additive, repeating the step (1), and carrying out metal element coating, so as to obtain a secondary sintered material; and (3) repeating the step (1) by taking the secondary sintered material as a main raw material and taking a Si-containing compound as an additive to coat the Si element to obtain a tertiary sintered material, namely the LPSC sulfide solid electrolyte. The invention further provides the obtained LPSC sulfide solid electrolyte and application of the LPSC sulfide solid electrolyte in a power automobile. According to the preparation method, through a doping introduction process, the LPSC sulfide solid electrolyte with high air stability and small H2S release amount can be obtained on the basis of ensuring the ionic conductivity.