112results about "Phosphorus preparation" patented technology

The invention provides a superfine nano phosphorus-carbon negative electrode material prepared based on in-situ high-temperature phase change in a confinement microcavity and a preparation method of the superfine nano phosphorus-carbon negative electrode material. The method aims to solve the problems of large volume expansion, poor conductivity, poor cycling stability and the like when phosphorus is used as a negative electrode material of an alkali metal ion battery. By constructing a confinement microcavity on the surface of a porous conductive material and combining a transient high-temperature phase change technology, phosphorus can be uniformly distributed and nanocrystallized. The method comprises the following steps: mixing phosphorus and a conductive porous material in a solvent, sanding, forming solid particles through reforming granulation, and constructing the confinement microcavity through coating treatment. Transient heating is carried out in a high-temperature device, so that the phosphorus source is quickly sublimated and uniformly distributed, finally, heat-preservation conversion is carried out in a sealed container, and the stability of the material is improved. The method not only improves the utilization efficiency of phosphorus and the conductivity of the material, but also enhances the cycle life and energy density of the battery, and has the advantages of simplifying the process flow and reducing the production cost.

The invention belongs to the technical field of electrocatalysis, and particularly relates to a preparation method of a nickel-iron-based transition metal boride / black phosphorus composite oxygen evolution reaction electrocatalyst. The invention provides a preparation method of a ferronickel-based transition metal boride / black phosphorus composite oxygen evolution reaction electrocatalyst, which is characterized by comprising the following steps: synthesizing a quasi-two-dimensional ethylenediamine modified black phosphorus nanosheet (eda-BP) by a hydrothermal method, and carrying out ultrasonic treatment on the surface of the obtained eda-BP to obtain the ferronickel-based transition metal boride / black phosphorus composite oxygen evolution reaction electrocatalyst. The nickel-iron-based transition metal boride / black phosphorus composite oxygen evolution reaction (OER) electrocatalyst (Ni < x > FeyB / eda-BP) is prepared by loading nickel-iron-based transition metal boride (Ni < x > FeyB) through an in-situ chemical reduction method, so that modification of a two-dimensional black phosphorus electrocatalyst is realized; the problems of instability of a quasi-two-dimensional black phosphorus catalyst, serious Fe loss of a nickel-iron-based catalyst, poor reaction kinetics and the like are solved to a great extent, and under the synergistic effect of the two parts, the electro-catalytic oxygen evolution reaction activity and the electro-catalytic stability of the composite catalyst are remarkably improved. The preparation method of the nickel-iron-based transition metal boride / black phosphorus composite oxygen evolution reaction electrocatalyst provides a new thought and a new way for designing and developing a novel efficient and stable oxygen evolution reaction electrocatalyst.

The utility model relates to the technical field of high-purity phosphorus product preparation and collection, and discloses a product collection device for preparing high-purity phosphorus through bromine reduction, which comprises a fixing plate, a fixing frame fixedly mounted at the top of the fixing plate, a reaction barrel arranged inside the fixing frame, a feeding pipe and a gas outlet pipe arranged outside the reaction barrel, a mounting top frame is fixedly mounted at the top of the reaction barrel, reaction mixing mechanisms are arranged at the top of the mounting top frame and inside the reaction barrel, auxiliary collecting mechanisms are arranged inside the fixing frame and outside the reaction barrel, and a waste gas treatment tower is arranged on the side, away from the reaction barrel, of the gas outlet pipe. The reaction mixing mechanism is arranged, corresponding gears in a selectable gear set are meshed with first gears, the mixture attached to the inner wall of the reaction barrel can be scraped while the mixture is stirred, and the auxiliary collecting mechanism is arranged, so that in the using process, a material partition plate can be dynamically opened, and products are better discharged and collected.

The present invention provides a method for preparing high-stability two-dimensional black phosphorus. First, a phosphorus source and an iodine source are introduced into a reaction system for preliminary preheating and activation. After being fully activated in the raw material area of ​​the reaction system, they are slowly transferred to the crystal growth area of ​​the reaction system. The phosphorus source and the transport agent flow through the liquid to the catalyst and are fully converted in the intermediate formation area. The converted intermediate slowly moves to the crystal nucleation growth area to begin crystal nucleation and growth. After further sufficient reaction, the crystal nucleation growth point continues to extend and grow, and finally the black phosphorus crystal slowly nucleates and grows in blocks. After the crystal growth is completely cooled to room temperature, the unconverted raw materials are reused until they are finally converted into black phosphorus crystals and tail gas. The tail gas is absorbed and converted into other by-products. The use of high-temperature and high-pressure resistant pipelines can achieve efficient transportation of gaseous phosphorus, thereby extending the growth time of black phosphorus crystals and improving the growth efficiency of black phosphorus crystals.

The invention discloses a regeneration and activation method of an inactivated black phosphorus catalyst, and belongs to the technical field of phosphorus chemical new materials. The method comprises the following steps: placing an inactivated black phosphorus catalyst in a high-temperature area of a separator, separating an inert substance on the surface of the inactivated catalyst from the catalyst by controlling a separation temperature gradient in the separator under a vacuum or inert atmosphere sealing condition, then taking out the catalyst, and mixing the catalyst with iodine or an iodine compound, under the sealing condition of vacuum or inert atmosphere, reacting at 400-550 DEG C for 20-120 minutes, and cooling to 200-350 DEG C within 60-120 minutes, so as to realize the activation of the deactivated catalyst; and the activated catalyst has good reaction activity and very high cycle stability.

The invention belongs to the technical field of battery negative electrode materials, and particularly relates to a black phosphorus carbon negative electrode, a synthesis method and synthesis equipment thereof and a battery comprising the black phosphorus carbon negative electrode. The black phosphorus carbon negative electrode comprises porous carbon, black phosphorus loaded in the porous carbon and coating carbon for coating the porous carbon, the black phosphorus is deposited into the porous carbon after gas-phase phosphorus except the black phosphorus is subjected to catalytic conversion, and the mass ratio of the black phosphorus is 10%-80%. Cheap phosphorus materials such as red phosphorus are used as raw materials, gas-phase black phosphorus is formed through gasification and catalysis and is deposited into porous carbon under the action of temperature difference, then the outermost layer is coated with a layer of coating carbon to obtain the black phosphorus carbon negative electrode, the performance of the negative electrode material is improved, and the cost advantage is obvious.

The invention discloses a phosphorus-carbon composite negative electrode material as well as a preparation method and application thereof, and belongs to the technical field of sodium-ion battery negative electrode materials. Aluminum powder, melamine, conductive carbon black and P2O5 which are cheap and easy to obtain are used as raw materials, the phosphorus-carbon composite negative electrode material composed of phosphorus nanoparticles and a nanometer wrinkled carbon layer wrapping the phosphorus nanoparticles is prepared through in-situ reaction ball milling and acid pickling processes, and the phosphorus-carbon composite negative electrode material has excellent rate capability, high specific discharge capacity, first-week coulombic efficiency and cycling stability and can be applied to the field of lithium ion batteries. The preparation method is simple, efficient, low in cost and easy to realize industrial production.

The invention provides a preparation method of a Cu-Bp / escherichia coli (Cu-BP / E. coli) semi-artificial photosynthetic system for efficient biological hydrogen production. The preparation method comprises the following steps: designing black phosphorus nanosheets doped with copper quantum dots, testing the catalytic performance of Cu-Bp, and testing the hydrogen production performance of the Cu-BP / E. coli semi-artificial photosynthetic system. The system combines Escherichia coli capable of effectively catalyzing hydrogen generation and excellent light absorption performance of inorganic materials, and energy in sunlight is converted into chemical energy. Under the irradiation of visible light with the wavelength range of 420-780 nm and the light intensity of 2000 Wm, the system shows excellent hydrogen production performance, the hydrogen production amount within 5 hours reaches up to 2.12 mmol, and the hydrogen production amount is 2.07 times that of a BP / E. coli system and 2.32 times that of pure escherichia coli. A new path is opened up for the development of the field of biological hydrogen production.

A phosphorus-carbon composite material includes: phosphorus atoms; and carbon atoms, in which a content ratio of the phosphorus atoms in the phosphorus-carbon composite material is 10 mass % or more and 95 mass % or less, a content ratio of the carbon atoms in the phosphorus-carbon composite material is 5 mass % or more and 90 mass % or less, and a ratio WL620 / WL780 of a weight loss ratio WL620 at a measurement temperature of 620° C. and a weight loss ratio WL780 at a measurement temperature of 780° C., which are obtained by thermogravimetric measurement under the following conditions, is 0.1 or more and 0.9 or less. (Thermogravimetric measurement) 10 mg of the phosphorus-carbon composite material is accurately weighed to prepare a sample, and using a thermogravimetric measuring device, a weight change when the sample is heated from 50° C. to 780° C. at a temperature rising rate of 10° C. / min in N2 is measured. (Weight loss ratio) A ratio of a weight of the sample at the measurement temperature to a weight of the accurately weighed sample is defined as a weight loss ratio (weight %) at the measurement temperature.

The invention relates to the technical field of phosphorus chemical new materials, in particular to a preparation method for synthesizing a supported Sn24P19.3I8 catalyst in one step. According to the method, the phosphorus source, the tin powder, the iodine and the carbon additive are used as raw materials, and the supported Sn24P19.3I8 catalyst is prepared through one-step solvothermal reaction, so that the preparation process of the catalyst is simplified, the preparation efficiency and scale of the supported Sn24P19.3I8 catalyst are remarkably improved, meanwhile, the energy consumption in the production process is reduced, the catalytic activity and stability of the catalyst are improved, and the method is suitable for industrial production. The method has important significance for promoting large-scale efficient preparation of black phosphorus, lays a catalyst foundation for developing more novel elemental phosphorus, and promotes market promotion and industrial development of phosphorus chemical new materials.

The utility model discloses a device for efficiently preparing black phosphorus, which belongs to the technical field of phosphorus chemical new materials and comprises a reactor, a reaction area is arranged in the reactor, a charging mechanism is arranged in the reaction area and comprises an outer lining reaction kettle arranged in the reaction area, a first sealing mechanism is arranged on the top surface of the outer lining reaction kettle, and a lining is arranged in the outer lining reaction kettle. A plurality of flat bottom pipes are arranged in the lining at equal intervals, supporting nets are arranged in the flat bottom pipes, a heating resistance wire is arranged in the reaction area, and a second sealing mechanism is arranged outside the reaction area. The supporting net is placed in the flat-bottom pipe, the catalyst is filled in the flat-bottom pipe under the inert atmosphere condition, then the flat-bottom pipe is placed in the lining, and the phosphorus source is evenly distributed at the bottom of the lining. After the filling is completed, putting the whole lining into an outer lining reaction kettle, sealing the outer lining reaction kettle, and carrying out high-temperature heat treatment in a reaction system through accurately controlled temperature; after the reaction is finished, black phosphorus is deposited and grows in an internal flat-bottom tube, and high-quality black phosphorus crystals are obtained.

The invention discloses a low-cost and green phosphorus coal composite negative electrode material and a preparation method thereof. The preparation method specifically comprises the following steps: pretreating phosphate ore and raw coal; mixing the phosphate ore powder with the raw coal powder to obtain a phosphorus-coal mixed precursor; feeding the phosphorus-coal mixed precursor into a fluidized bed reactor for reaction to generate mixed gas; introducing the mixed gas into a cyclone separator, and separating solid particle impurities; the phosphorus steam is converted into liquid phosphorus, residual phosphorus steam and other impurities are adsorbed, and primary separation of the phosphorus steam from CO and H2 is achieved; and mixing phosphorus steam and H2, introducing the mixture into a CVD reactor, adding the high-specific-surface coal matrix, carrying out a reaction, and carrying out washing and drying. According to the phosphorus-carbon composite material disclosed by the invention, phosphorus steam is uniformly deposited on the surface and pores of a high-specific-surface coal matrix; the porous structure of the high-specific-surface coal matrix provides an expansion buffer space for phosphorus, and meanwhile, part of phosphorus and oxygen-containing functional groups on the carbon surface form chemical bonds, so that the interface bonding strength is enhanced.

The present invention belongs to the technical field of phosphorus chemical industry, and relates to an efficient preparation method of a purple phosphorus-based material. The present invention uses a phosphorus source as a reactant, an ammonium salt as a catalyst, mixes the phosphorus source and the ammonium salt under low oxygen conditions, heats the reaction, and obtains the purple phosphorus-based material after cooling. By using the ammonium salt as a catalyst, the conversion of the phosphorus source to the purple phosphorus-based material is promoted under oxygen-free and high temperature conditions, and the generation of harmful byproducts is reduced. At the same time, the ammonium salt is used as a catalyst, which is easily decomposed into gas in the reaction, and will not be sintered and deactivated at high temperature, thereby reducing production costs, improving resource utilization efficiency, and being easy to separate from the product, improving the quality of the product, realizing efficient and low-cost industrial production of purple phosphorus-based materials, and then promoting the wide application of purple phosphorus-based materials in multiple fields such as energy storage, electronic devices, and catalytic reactions.

The present invention provides a solid electrolyte material that can suppress a decrease in filling efficiency. [Solution] A solid electrolyte material comprising a sulfide solid electrolyte containing lithium, sulfur, and phosphorus, and an organic compound, wherein the organic compound has two or more benzene rings, and the melting point of the organic compound is 82°C or lower.

The invention relates to a method for recovering silicon in the form of silicon tetrachloride, in which biochar having a silicon content of at least 1% by weight, expressed as% by weight of elemental silicon, is reacted with elemental chlorine at a temperature of 350 to 900 DEG C and the formed silicon tetrachloride is separated from the exhaust gas stream, preferably by condensation.

The invention relates to a process for recovering phosphorus in the form of its chlorides, in which sewage sludge ash with a phosphorus content, expressed in wt.% of elemental phosphorus in the ash, of at least 2 wt.% is reacted with elemental chlorine in the presence of a carbon source at a temperature of 350 to 900°C and the phosphorus chlorides formed are separated from the exhaust gas stream.

A method for producing phosphorus in which a reaction for forming gaseous phosphorus (g) by bringing phosphorus oxide generated by heating a liquid phosphoric acid compound into contact with a carbon material to reduce the phosphorus oxide and for condensing the gaseous phosphorus (g) to obtain liquid phosphorus (L) is conducted by a flow reaction with a nonoxidizing gas flow, wherein the reduction reaction of the phosphorus oxide is conducted in a carbon material-packed bed, and the condensation of the formed gaseous phosphorus (g) is substantially conducted in a condensation accelerator-packed bed which is disposed downstream of the carbon material-packed bed in contact with the carbon material-packed bed.

The invention relates to a process for recovering silicon in the form of tetrachloride, in which biochar with a silicon content, expressed in wt.% of elemental silicon, of at least 1 wt.% is reacted with elemental chlorine at a temperature of 350 to 900°C and the silicon tetrachloride formed is separated from the exhaust gas stream, preferably by condensation.

The invention relates to a method for synthesizing black phosphorus - polyglycerol (BP-PG) nanoparticles comprising the step of adding (100) black phosphorus (BP) nanoparticles, glycidol and a plurality of beads (10) to a chamber (21) of a milling device (20) and the step of rotating (200) the chamber (21) over a defined period of time. The invention also relates to a method for recovering a precious metal from a precious metal containing matrix comprising the step of providing (300) the precious metal containing matrix in the form of a solution containing dissolved precious metal ions and the step of adding (400) black phosphorus - polyglycerol (BP-PG) nanoparticles to the solution, wherein the black phosphorus - polyglycerol (BP-PG) nanoparticles are synthesized using the method for synthesizing black phosphorus - polyglycerol (BP-PG) nanoparticles.

This invention relates to the field of oil additives for power generation, specifically a method for in-situ preparation of black phosphorus nanoparticles (BPNPs) using PVA / PAAM interpenetrating network hydrogel as a microreactor and its application as a wear-resistant additive in lubricating oils. The confinement effect of the interpenetrating network hydrogel results in uniform BPNP size and high crystallinity, thus endowing BPNPs with excellent air / water / oil stability, with an oxidation rate of <5% within 7 days. Swelling allows RP / KI to permeate uniformly and be physically embedded in the network. Subsequently, under a nitrogen protective atmosphere, photolysis of iodine ions generates solvated electrons (e). ‑ (aq) restores RP to P ‑ P ‑ The BP crystal nucleus is formed by recombination, and the IPN three-dimensional nanochannels (pore size 30~120nm) confine and inhibit excessive growth of the crystal nucleus. At the same time, the PVA hydroxyl groups and PAAm amide groups passivate the BP surface in situ through hydrogen bonding / coordination, preventing oxidation.

This invention relates to a non-metallic porous carbon anode material, its preparation method, and its application. The preparation method includes: activating a carbon-containing raw material in a hydrogen-containing mixed gas to obtain porous carbon and a benzene-rich hydrocarbon gas; depositing the non-metallic source gas and the porous carbon in a primary deposition; and then depositing the non-metallic source gas and the benzene-rich hydrocarbon gas in a secondary deposition to obtain the non-metallic porous carbon anode material. The carbon-containing raw material is further de-ashed before use, or the porous carbon is de-ashed and then mixed. This invention achieves continuous preparation of porous carbon and non-metallic porous carbon anode materials by activating the carbon-containing raw material with hydrogen. The excess hydrogen generated in this process can be recycled to the hydrogen activation step for reuse. Hydrogen activation enables efficient deoxygenation of the carbon-containing material, avoiding the generation of other oxide impurities during the deposition of non-metals, effectively ensuring the safety of the deposition process. The benzene-rich hydrocarbon byproduct generated during the preparation of porous carbon can further carbonize the material, achieving efficient utilization of carbon resources.

This method for recovering phosphorus includes adding a reducing agent containing at least one of metallic silicon and metallic aluminum and an alkali metal compound to steelmaking slag containing a phosphorus oxide to reduce the phosphorus oxide with the reducing agent in a state including the liquid phase.

To efficiently produce phosphorus from a phosphoric acid solution.SOLUTION: A reducing agent and a phosphoric acid solution containing phosphoric acid are charged into a container, and the container is heated while controlling the internal pressure of the container, resulting in the reduction of the phosphoric acid. Preferably, the internal pressure of the container is controlled to a range of 0.12 MPa or less. Preferably, the internal pressure of the container is controlled to a range of 0.03 MPa or more. Preferably, the reducing agent and the phosphoric acid solution are charged into the container such that the mass ratio of the reducing agent to phosphoric acid (reducing agent / phosphoric acid) is 1 / 2-1 / 10.SELECTED DRAWING: None

A method for preparing a metal-free few-layer phosphorous nanomaterial. The method comprises an ice-assisted exfoliation process (or solvent ice-assisted exfoliation process). The method allows for the preparation of a few-layer phosphorous nanomaterial with improved yield and reduced duration and exfoliation power. The few-layer phosphorous nanomaterial is used in the preparation of a photocatalyst. The photocatalyst exhibits a long-term stability, high photocatalytic H2 evolution efficiency from water, and good stability under visible light irradiation.

The present invention discloses a nitrogen-doped black phosphorus nanosheet / graphene composite material, its preparation method, and application. First, amorphous red phosphorus, a nitrogen-containing compound, and graphene oxide are added to a solvent, followed by a solvothermal reaction at 150-200°C. After the reaction, a product is obtained, which is filtered, washed, and dried to prepare the nitrogen-doped black phosphorus nanosheet / graphene composite material. The prepared nitrogen-doped black phosphorus nanosheet / graphene composite material is modified on a carbon ethylenediamine (CGE) and used for the detection of trace amounts of hydroquinone in the environment, demonstrating excellent sensitivity and promising application prospects.

Provided are a black phosphorus-two dimensional material complex and a method of manufacturing the black phosphorus-two dimensional material complex. The black phosphorus-two dimensional material complex includes: first and second two-dimensional material layers, which each have a two-dimensional crystal structure and are coupled to each other by van der Waals force; and a black phosphorus sheet which between the first and second two-dimensional material layers and having a two-dimensional crystal structure in which a plurality of phosphorus atoms are covalently bonded.

The invention discloses a purple phosphorus micron tube array and a preparation method thereof. The purple phosphorus micro-tube array has unique structural characteristics, the diameter of a micro-tube is 1-10 [mu] m, the aperture is 0.3-1.7 [mu] m, and the tube length is 10-500 [mu] m. The preparation method comprises the following steps: mixing amorphous red phosphorus (the purity is 99.99%-99.9999%) and iodine elementary substance (the purity is 99.8%-99.99%) according to the mass ratio of 15: 1-25: 1, sealing the mixture in a quartz tube under the vacuum condition of 10 <-4 >-10 <-5 > Pa, and carrying out gradient temperature control through a horizontal double-temperature-zone tubular furnace: heating a medicine zone to 470-520 DEG C at a speed of 2-5 DEG C / min and carrying out heat preservation for 20-25 hours, and synchronously heating a non-medicine zone to 450-460 DEG C; the inclined angle design of 5-60 degrees of the quartz tube is combined with the synergistic effect of double temperature zones, and directional growth of Hittorf purple phosphorus microcrystals is realized through an iodine steam transport mechanism. The method is simplified in process and low in cost, the high-purity purple phosphorus micron tube array is obtained, the band gap is about 1.90 eV, the method can be used for field effect transistors, photoelectric detectors, photo-thermal conversion, photocatalysis and electro-catalysis, and a novel structure semiconductor material is provided for the field of photoelectric devices.

The present invention discloses a method for exfoliating two-dimensional materials based on the synergistic effect of resonance crushing and crystal growth, comprising: crushing a bulk material and uniformly dispersing it in a solvent to form a dispersion; freezing the dispersion to form a solid material; placing the solid material in a low-temperature environment where the temperature is lower than or equal to the freezing point of the solvent, and subjecting the solid material to ultrasonic treatment to resonate the solvent crystallized between layers, so that at least part of the crystallized solvent is crushed, and at the same time enabling the liquid solvent in the surrounding environment to enter the broken gaps and continue to solidify and crystallize in this low-temperature environment. With the continuous crushing and growth of the crystals between the material layers, two-dimensional materials are finally exfoliated from the bulk material; the surface tension of the solvent matches the surface energy of the two-dimensional material. The method for exfoliating two-dimensional materials of the present invention is convenient to operate, has a small solvent usage amount, high exfoliation efficiency, good quality of the exfoliated two-dimensional materials, is suitable for large-scale production, and has potential industrialization value.

The invention relates to the technical field of target material preparation, and provides a phosphorus-doped silicon target material, a preparation method thereof and a photovoltaic cell, and the preparation method comprises the following steps: carrying out smelting treatment on a silicon dioxide block and a phosphorus-containing compound, and then cooling and crushing to obtain silicon phosphorus oxide powder; the silicon-phosphorus oxide powder is subjected to reduction treatment, and silicon-phosphorus alloy powder is obtained; carrying out coating treatment on the silicon-phosphorus alloy powder by utilizing silicon powder to obtain composite powder; and thermally spraying the composite powder onto a back tube, and then machining to obtain the phosphorus-doped silicon target material. According to the preparation method, the silicon dioxide and the phosphorus-containing compound are smelted, so that the silicon dioxide and the phosphorus-containing compound fully react, uniform silicon-phosphorus oxide powder with stable chemical properties is formed after cooling and curing, and more uniform and stable silicon-phosphorus alloy powder is formed after the silicon-phosphorus oxide powder is reduced, so that the prepared silicon target material is better in structure uniformity; and the phosphorus content of the silicon target material is favorably controlled. And the silicon powder is used for coating the silicon-phosphorus alloy powder, so that the volatilization of phosphorus in the spraying process is reduced, and the phosphorus content of the silicon target material can be better controlled.

The invention relates to a process for the recovery of silicon in the form of silicon tetrachloride, in which biochar having a silicon content, expressed in % by weight of elemental silicon, of at least 1% by weight is reacted with elemental chlorine at a temperature of 350 to 900°C and the silicon tetrachloride formed is separated from the exhaust gas stream, preferably by condensation.