266results about "Phosphorus preparation" patented technology

The invention discloses a black phosphorus preparation method with a high conversion rate. The preparation method comprises the following steps: mixing red phosphorus, tin and tin tetraiodide in a mass ratio of (1-6):(40-50):(1-2), filling the mixture into a quartz tube, vacuumizing until the pressure in the quartz tube is smaller than 0.05 Pa, sealing the tube, heating to ensure that the raw material end temperature in the quartz tube is 100-400 DEG C, heating to 400-700 DEG C in 1-2 hours, keeping the temperature for 5-10 hours, then cooling to 200-500 DEG C in 6-8 hours, keeping the temperature for 1-3 days, and finally cooling to the room temperature in 10-15 hours to obtain black phosphorus. The preparation method disclosed by the invention is simple in step and strong in operability; on the one hand, a nontoxic raw material is adopted to achieve effects of cleanliness and environmental friendliness, and on the other hand, only a mild reaction condition is needed, so that the energy consumption and cost are reduced, and the prepared black phosphorus has good crystallinity and a high conversion rate. The preparation method disclosed by the invention has strong repeatability and is favorable for industrial popularization and application.

Disclosed is black phosphorus or black phosphorus-carbon composite, which is very suitable for an anode material of lithium rechargeable battery. The black phosphorus or black phosphorus-carbon composite is prepared by using high energy ball-milling, which is easy and efficient way in transforming amorphous red phosphorus into orthorhombic black phosphorus at ambient temperature and pressure.

The invention provides black phosphorus nanosheet and a preparation method and application thereof. The method comprises the following steps: placing black phosphorus powder into anaerobic water to form a dispersion of black phosphorus powder, and selectively controlling pH of the dispersion to alkaline level; carrying out ultrasonic treatment on the dispersion of black phosphorus powder in an inert environment; and after the ultrasonic treatment, centrifuging and collecting a supernatant so as to obtain the black phosphorus nanosheet. The invention also provides the black phosphorus nanosheet prepared by the method and application of the black phosphorus nanosheet. As no organic solvent is used by the method, the prepared black phosphorus nanosheet has no organic solvent residue, will not pollute the environment and can be applied in the field of biomedicine.

The invention belongs to the technical field of chemical material synthesis and electrochemistry and particularly relates to a method for preparing composite materials and black phosphorus of negative electrode materials of a high-capacity lithium-ion battery. According to the method, the black phosphorus of negative electrode materials of the high-capacity lithium-ion battery is synthesized by a high-pressure synthesis method. On one hand, a high-pressure synthesis device is adopted, white phosphorus and red phosphorus are respectively used as raw materials, and pure-phase black phosphorus is synthesized at different pressures and temperatures; on the other hand, the white phosphorus and the red phosphorus are used as raw materials, modified materials are doped, modified black phosphorus is synthesized, the raw materials account for 10 to 90 percent, and the modified materials account for 5 to 50 percent. The black phosphorus prepared by the method is used as the negative electrode materials of the lithium-ion battery, the specific capacity is 3 to 7 times of that of the industrialized graphite negative electrode, the tap density of the black phosphorus negative electrode materials reaches 1.7 to 2.4g/cm<3> and is 2 to 3 times of that of the graphite negative electrode, and the black phosphorus negative electrode has good compatibility with the existing electrolyte and is hopeful to become a new generation of negative electrode materials of the high-capacity lithium-ion battery.

The invention relates to a method for preparing few-layer black scales by ultrasonically stripping a black scale. The method comprises the steps of uniformly mixing black scale powder and an intercalator in an organic solvent according to a given ratio to obtain a mixture, insulating the air, ultrasonically treating the mixture in water bath, and carrying out vacuum suction filtration and vacuum drying to obtain a few-layer black scale material. A series of compounds such as cetyl trimethyl ammonium bromide, phenanthrene and naphthalene are used as the intercalator to prepare the few-layer black scale. Compared with the prior art, the prepared few-layer black scale has advantages of few defects, few impurities, high quality and the like. Meanwhile, the process is simple to operate and low in cost, and the prepared few-layer black scale is expected to substitute the graphene material to be applied to the field of a photoelectric material.

The invention discloses a preparation method and application of black phosphorus quantum dots with high yield. The preparation method comprises the following steps: firstly performing ultrasonic treatment on a massive black phosphorus crystal for 1-3 hours by adopting a liquid phase stripping method; after the completion of ultrasonic treatment, standing for 1-2 hours and then taking upper liquid for centrifugal separation, wherein the rotating speed is 1500-2000 rpm, and the time is 20-40 minutes; dispersing in a N-methyl pyrrolidone solvent, then standing, performing centrifugal separation, taking liquid supernatant and pouring into a teflon-lined high-pressure reactor for solvothermal reaction; after the end of reaction, obtaining black phosphorus quantum dot dispersion liquid with uniform size. A material prepared by the preparation method disclosed by the invention has potential application to the fields of optoelectronics, electronic sensors, semiconductors and the like.

A method of producing biodiesel through the trans-esterification of a triglyceride, comprising mixing a triglyceride, an alcohol, and a catalyst to form a mixture, where said catalyst is non-metal quaternary ammonium hydroxide or non-metal quaternary phosphonium hydroxide, removing volatile components from said mixture, and allowing the remaining mixture to separate into a biodiesel-rich layer and a glycerol-rich layer.

The invention discloses a preparation method of black a phosphene nano sheet. The black phosphene nano sheet is prepared by stripping black phosphorus crystals through liquid phase shear force generated by a high-speed rotation cutter head, wherein the whole preparation process is carried out in an argon environment. The preparation method particularly includes the following steps: placing the black phosphorus crystals and an organic solvent in a stirring barrel; setting the rotation speed of the high-speed rotation cutter head; connecting a power supply to drive the high-speed rotation cutter head to rotate in the stirring barrel; setting stripping time to prepare a dispersion liquid of the black phosphene nano sheet; and finally performing centrifugation, filtration and cleaning to obtain clean black phosphene nano sheets. The preparation method is low in cost and has potential of large-scale production.

The invention discloses a constant-temperature large-scale preparing method of belt-shaped black phosphorus to prepare the black phosphorus in a constant-temperature manner. Cheap red phosphorus, tin and iodine are adopted as raw materials and subjected to a solid-phase reaction at a constant temperature under a low pressure to prepare the pure-phase belt-shaped black phosphorus. The method is simple in steps and high in operability. The method is advantageous in that 1) the adopted raw materials are nontoxic so that the method is clean and environmental friendly, 2) tin tetraiodide is replaced by the iodine, thus greatly reducing a cost, 3) the conversion ratio of the black phosphorus is high, and 4) black phosphorus growth is performed with a muffle furnace in place of a tube furnace, so that the yield of the black phosphorus is greatly increased, a single-pass black phosphorus yield only depends on the volume of the muffle furnace, and the single-pass yield is increased by at least 10 times or above than a single-pass yield when black phosphorus growth is performed in a tube furnace. The prepared belt-shaped black phosphorus is characterized in that crystallinity is good, and thin-layer black phosphorus with a large area can be stripped mechanically more easily. The method provides great convenience for subsequent preparation and applications of photoelectric devices based on the black phosphorus.

The invention provides nanoscale black phosphorus as well as a preparation method and application thereof. The preparation method comprises the following steps that in protective gas, adding bulk red phosphorus of which the dimension is greater than 0.1cm and stainless steel balls of which the diameters are 6mm-12mm to a high energy ball milling pot in the mass ratio of the bulk red phosphorus to the stainless steel balls being 1 to (20-60), performing sealing, and then performing a ball milling reaction, so as to prepare the nanoscale black phosphorus. The temperature of the ball milling reaction is from room temperature to 60 DEG C, the ball milling rotational speed is 1100r/min-1500r/min, and the ball milling time is 2h-8h. The invention further provides the nanoscale black phosphorus prepared by the preparation method, the particle diameters of the nanoscale black phosphorus are 1nm-5nm. The invention further provides an application of the nanoscale black phosphorus in photoelectric devices, solar batteries, lithium batteries and biomedical science.

The invention relates to an ore extraction technology, in particular to a method for leaching low-grade phosphorite with mixed bacillus, wherein the mixed bacillus consists of a thiobacillus thioxidans At.t which is separated from soil sample of the Hubei tongshankou copper mine and a thiobacillus ferrooxidans At.f which is separated from acid water hole of the Hubei tonglushan copper mine. The method comprises the following steps of: 1) sampling from the soil sample of the Hubei tongshankou copper mine and the acid water hole of the Hubei tonglushan copper mine; 2) separating the thiobacillus thioxidans and the thiobacillus ferrooxidans in an enrichment way and domesticating; and 3) leading the phosphorus. The method has the beneficial effects of: 1. being high in the activity of mixed bacillus: the phosphorus leading rate is high up to 88.75%; 2. being low in cost: the cost of the 10% inoculum size is far lower than that of the 20%-30% inoculum size of the thiobacillus thiooxidans in the prior art, so that the cost for preparing culture solution with plenty of expensive medicaments is reduced; 3. being short in period and high in efficiency; and 4. being environment-friendly: the usage amount of the acid bacillus is small, thereby being good for reducing environment pollution.

The invention relates to a liquid-phase stripping preparation method of single-layer or few-layer phosphaalkene. The preparation method comprises the following steps: mixing flaky black phosphorus and an organic solvent, sequentially carrying out ultrasonic cracking treatment and centrifugation, dropwisely adding the supernate of the product onto a substrate, and carrying out spin coating or drying to obtain the single-layer or few-layer phosphaalkene. The method can implement mass production on phosphaalkene with the minimum single layer, has the advantages of low cost and high yield, and is beneficial to further scientific research and popularization and application of phosphaalkene.

The invention provides a preparation method of a large-size black phosphorus slice. The method comprises the steps of soaking a black phosphorus block body into an organic solvent, and stirring, wherein the rotating speed of stirring is 1000-3000r/min, and the stirring time is 20-30 hours; centrifuging the stirred solution at low speed, collecting supernatant, centrifuging the supernatant at high speed, removing the supernatant, and collecting the solid precipitate, wherein the solid precipitate is the large-size black phosphorus slice. The method is simple in operation, mild in conditions, low in price, good in reproducibility and high in yield; oscillation and ultrasound are not needed in the preparation process, so that low-cost industrial production is easily realized. The large-size black phosphorus slice has the lateral dimension of 5-25 micrometers, thus being able to be applied to the fields such as preparation of a photoelectric device or a sensor, and the like.

The invention provides a method for large-scale preparation of black phosphorus with a bilayer structure. The method is characterized by comprising steps as follows: 1), white phosphorus or red phosphorus reacts for at least one min at the temperature of 600 DEG C-800 DEG C under the pressure of 6-8 Kbar; 2), a product obtained from the step 1) is placed in an ethanol water solution to be soaked for 4-6 hours; 3), the product is processed for at least 10 min by ultrasonic waves, and the ultrasonic power is 70-80 W. The preparation process is simple, the black phosphorus with the bilayer structure and a higher generation rate can be obtained, and the generation rate can be up to 91.0%. The preparation process is low in cost and facilitates large-scale application.

The invention relates to the field of a nanometer material and preparation thereof, and discloses a two-dimensional material nanometer roll as well as a preparation method and application thereof, wherein the two-dimensional material nanometer roll is obtained by soaking and/or dripping and coating a solution onto the surface of a two-dimensional material thin film and thus automatically curling the two-dimensional material thin film, wherein the two-dimensional material nanometer roll is in a hollow rod shape; the length is 50nm to 1cm; the outer diameter is 5 to 500nm; the inner hollow layerdiameter is 2 to 100 nm; the layer space is 0.3 to 10 nm. The migration rate of a prepared field effect transistor based on the two-dimensional material nanometer roll is 8 to 4000 cm/(V.sec). By using the method, the two-dimensional material nanometer roll with high quality can be prepared at high yield. In addition, the operation of the method is simple and flexible; the synthesis cost is low;the reaction time is short.

The invention discloses a black phosphorus crystal with a high photoelectric response rate as well as a preparation method and application thereof. The black phosphorus crystal with the high photoelectric response rate is a monocrystal, with a space point group Cmca (no.64); lattice parameters are as follows: a=3.2 to 3.4 angstroms, b=10.4 to 10.6 angstroms, c=4.3 to 4.5 angstroms, and interlamellar spacing=4 to 6 angstroms. The preparation method comprises the following steps: placing a growth precursor containing red phosphorus, a mineralizer and a doping element into a sealed reaction container, of which an inner cavity is in a vacuum environment, and performing heating, heat preservation and cooling on the reaction container in sequence, thus growing and forming the black phosphorus crystal. A carrier type and a carrier concentration of the black phosphorus crystal provided by the invention can be adjusted; the black phosphorus crystal can show an extremely high photoelectric response rate without subsequent modification; moreover, the preparation method is simple, low in cost, low in pollution, high in yield, high in product crystallinity and uniform in doping; and the black phosphorus crystal has a wide application prospect in the field of photoelectronic devices.

The invention discloses a method for preparing a two-dimensional nanomaterial film on the basis of a liquid phase method. According to the method, an organic solution is prepared from two-dimensional nanomaterials and placed on the surface or inside an aqueous or saline solution, the two-dimensional nanomaterials are quickly assembled on the surface of the aqueous or saline solution to from a large-area film, the film is formed by stacking two-dimensional nanomaterial laminates, the film thickness is only 2-10 nm, and the film can be transferred onto any substrate. The method has the advantages that the cost is low, the energy consumption is low, the preparation cycle is short, the repeatability is high, the operation process is safe and simple, the preparation process is environment-friendly, and the method can be applied to large-scale industrial production; the film has high light transmission, the resistance of the film is very sensitive to deformation responses, and the film can be used as a high-sensitivity flexible strain sensor.

The invention discloses a preparation method of nano black phosphorus, and belongs to the field of novel materials. A novel technology for synthesizing the nano black phosphorus by a mechanical and physical method is adopted, and the technology is an ultrahigh-energy ball milling method comprising optimization of a ball-hammer type instantaneous high-frequency impact pressure and parameters, atmosphere control, and addition of a modified material, wherein red phosphorus is used as a raw material, a milling tank is vacuumized and filled with argon before ball milling, ball milling is performed for 8-10 hours at an impact frequency of 800-1600 times per minute to obtain crystal black phosphorus with an average size of 100-300 nanometers, and tank unloading, material taking and packaging needs to be completed in a vacuum glove box. According to a demand of oxidation resistance and high conductivity, during preparation of modified nano black phosphorus, a metal or metal alloy or metal oxide or nonmetal material is needed, and a high polymer material is used as a modifying material for grinding after being added with an added amount accounting for 0.1-10%.

The invention belongs to the field of material chemistry, and in particular relates to a method for preparing yttria-stabilized zirconia powder. The method particularly adopts an ultrasonic-microwave synthesis method, carries out precursor preparation under an ultrasonic condition so as to ensure that a system can be better dispersed and doped, and adopts a microwave heating mode to dry the precursor so as to avoid agglomeration of the precursor. After the precursor is calcined at high temperature, the yttria-stabilized zirconia powder can be obtained. The powder has good dispersity, and has grain diameter reaching nanometer grade, uniform sizes and uniform distributions. The method has the advantages of simple process, low cost and the like.

The invention discloses a preparation method of organic metal framework-coated two-dimensional black phosphorus nanosheets, and relates to black phosphorus nanosheets. The preparation method comprisesthe following steps: preparing two-dimensional black phosphorus nanosheets; preparing metal ion-modified black phosphorus nanosheets; mixing and dispersing the metal ion-modified black phosphorus nanosheets and an organic ligand in N,N-dimethylformamide DMF, and then transferring a mixed solution to a reaction kettle for constant-temperature crystallization; cooling the reaction kettle to room temperature, centrifuging, and washing to obtain the organic metal framework-coated two-dimensional black phosphorus nanosheets. By a method for forming a metal organic framework on the surface of blackphosphorus, fixation of the metal ions to the surface of the black phosphorus is achieved, the metal ions reduce the electron cloud density on the surface of the black phosphorus, and coating of theMOF (metal organic framework) reduces contact with water and oxygen and improves the stability of the black phosphorus itself. Due to high porosity of the organic metal framework, the prepared organicmetal framework-coated black phosphorus can be applied to gas detection or gas storage.

The invention relates to a preparation method of a black phosphorus nano lamina for photocatalytic degradation of dye wastewater. The method specifically comprises the following steps: (1) preparing multilayer black phosphorus, namely grinding red phosphorus without a surface oxidation layer in a mortar, and then performing mechanical ball milling to obtain the multilayer black phosphorus; and (2) preparing the black phosphorus nano lamina, namely adding the multilayer black phosphorus and a surfactant into water together, performing primary ultrasonic treatment and primary centrifugation, then collecting supernatant, adding the supernatant into water, stirring the materials uniformly, then performing secondary ultrasonic treatment, performing secondary centrifugation to obtain a solid deposit, and drying the solid deposit to obtain the black phosphorus nano lamina. Compared with the prior art, the preparation method provided by the invention is simple in preparation process, high in preparation efficiency, and suitable for large-scale production, and the prepared black phosphorus nano lamina has a higher specific surface area and band gap and photocatalytic activity, and can be used for performing photocatalytic efficient degradation on coloring agents including methylene blue in the dye wastewater.

The invention relates to a liquid phase stripping preparation method for a phosphaalkene nanoribbon or phosphorus nanoribbon. The method consists of: mixing ribbon or flake black phosphorus with an organic solvent, conducting ultrasonic transverse tearing treatment and centrifugal treatment, then adding a supernatant rich in phosphaalkene nanoribbon in the product on a substrate, and then performing spin coating or drying. The phosphaalkene nanoribbon prepared by the method provided by the invention has better quality. The method is low in cost and has high yield, thus being beneficial to further scientific research and popularization and application of phosphaalkene nanoribbons.