40 results about "Phospholenes" patented technology

Disclosed are a macrocyclic carbodiimide (MC-CDI) and a process for synthesizing the same through condensation of a molecule with multiple-isocyanate terminal functional groups under high dilution in the presence of a phospholene catalyst such as phospholene or arsenic catalyst. Also disclosed are MC-CDI derivatives, such as MC-urea (MC-U), MC-acylurea (MC-ACU), acid functionalized MC-ACU, and anhydride functionalized MC-ACU, processes for synthesizing the same, and the applications of such derivatives as hydrolysis stabilizers in organic polymeric materials, such as polyurethane (PU) and polyesters, as well as the applications in the syntheses of the amide- and imide-modified polyurethane by ring-opening reaction of the MC-ACU.

A flexible polyurethane foam article exhibiting flame resistance comprises the reaction product of an isocyanate and an isocyanate-reactive component comprising a polyol reactive with the isocyanate. The isocyanate and the isocyanate-reactive component are reacted in the presence of a blowing agent and a phospholene oxide. A method of producing the flexible polyurethane foam article includes the step of reacting the isocyanate and the isocyanate-reactive component in the presence of the blowing agent and an effective amount of the phospholene oxide to form the flexible polyurethane foam article which is flame resistant.

A proppant comprises a particle and a polycarbodiimide coating disposed on the particle. The polycarbodiimide coating comprises the reaction product of an isocyanate reacted in the presence of a phospholene oxide catalyst. A method of forming the proppant comprises the steps of providing the particle, providing the isocyanate, providing the phospholene oxide catalyst, reacting the isocyanate in the presence of the phospholene oxide catalyst to form the polycarbodiimide coating, and coating the particle with the polycarbodiimide coating.

The invention relates to a preparation method of two-dimensional crystal black phosphorene. A preparation method of two-dimensional crystal black phosphorene, which is characterized in that it comprises the following preparation steps: taking red phosphorus, silver zinc oxide and tin tetraiodide for subsequent use; taking red phosphorus, silver zinc oxide and tin tetraiodide and fully mixing them, Sealed together in a quartz tube with an inner diameter of 10mm, placed in a single-temperature zone furnace to raise the temperature to 400-800°C and keep the temperature constant for 15-40h; the preparation method of the two-dimensional crystal black phosphorene of the present invention has simple preparation process, mild conditions, High Yield.

A rigid foam having increased flame retardance comprises the reaction product of an isocyanate component and an isocyanate-reactive component. The isocyanate component and an isocyanate-reactive component are reacted in the presence of an isocyanurate catalyst component and a carbodiimide catalyst component. The isocyanurate catalyst component comprises 1,3,5-tris(3-(dimethylamino)propyl)-hexahydro-s-triazine and the carbodiimide catalyst component comprises 3-methyl-1-phenyl-2-phospholene-1-oxide. A method of forming the rigid foam on a surface comprises the steps of providing the isocyanate component, providing the isocyanate-reactive component, providing the isocyanurate catalyst component, providing the carbodiimide catalyst component, and spraying the isocyanate component, isocyanate-reactive component, isocyanurate catalyst component, and carbodiimide catalyst component onto the surface to form the rigid foam on the surface.

Disclosed are a macrocyclic carbodiimide (MC-CDI) and a process for synthesizing the same through condensation of a molecule with multiple-isocyanate terminal functional groups under high dilution in the presence of a phospholene catalyst such as phospholene or arsenic catalyst. Also disclosed are MC-CDI derivatives, such as MC-urea (MC-U), MC-acylurea (MC-ACU), acid functionalized MC-ACU, and anhydride functionalized MC-ACU, processes for synthesizing the same, and the applications of such derivatives as hydrolysis stabilizers in organic polymeric materials, such as polyurethane (PU) and polyesters, as well as the applications in the syntheses of the amide- and imide-modified polyurethane by ring-opening reaction of the MC-ACU.

Provided is a method for producing an alkenyl phosphorus compound which can produce an alkenyl phosphorus compound efficiently even with a smaller amount of a catalyst used than that used conventionally, and further which can maintain catalytic activity to produce an alkenyl phosphorus compound in high yield even at a larger reaction scale, and which can also be applied to quantity synthesis at an industrial scale using a conventional batch reactor or continuous reactor.A method for producing an alkenyl phosphorus compound, comprising:a step of reacting a compound represented by the following formula (1):[In formula (1), R1 represents OR3 or R3, R2 represents OR4 or R4, and R3 and R4 represent, for example, each independently a substituted or unsubstituted alkyl group.]with a compound represented by the following formula (2):R5—C≡CH  (2)[In formula (2), R5 represents, for example, a hydrogen atom, or a substituted or unsubstituted alkyl group.]to produce the phosphorus alkenyl compound presented by at least any of the following formulas (3a) or (3b):[In formulas (3a) and (3b), R1 and R2 have the same meaning as defined in formula (1), and R5 has the same meaning as defined in formula (2).],In which the compound represented by formula (1) is reacted with the compound represented by formula (2) using a transition metal catalyst, and a phosphorus oxo acid compound having an intramolecular P—H bond.

The invention discloses a preparation method of a phosphorene-functional-modified 3D-print polylactic acid bionic nanofiber support and aims to provide a multifunctional support material for repairing bone defects and a preparation method thereof. The preparation method is characterized by comprising the following steps: loading an anti-inflammatory drug ibuprofen onto nano flaky phosphorene prepared by a liquid-phase stripping method, and coating the surface of the phosphorene with a polydopamine coating, so as to realize intelligent controlled release of the drug; and uniformly doping the obtained drug-loaded phosphorene into an amination-modified polylactic acid matrix to obtain a size mixture, constructing a personalized support by adopting a low-temperature 3D printing technology, and enabling the support to be subjected to phase separation under a low-temperature printing condition so as to form a reticular nanofiber structure of a bionic extracellular matrix. The preparation method has the characteristics that the prepared support can be subjected to personalized designing according to characteristics of a bone defect part of a patient, and the prepared support has good actions of cellular affinity, photothermal conversion performance, bone growth promotion, intelligent drug release and long-acting inflammation resisting and has potential application prospects in the field of bone tissue engineering.

A method of producing a phospholene oxide is disclosed. A dihalohydrocarbylphosphine, 2-methyl-1,3-butadiene, and a halogenated hydrocarbon solvent are combined to form an adduct via an addition reaction in a homogenous system wherein the ratio of the 2-methyl-1,3-butadiene to the dihalohydrocarbylphosphine is from 1.0 to 2.0 and wherein the solvent is present in an amount of greater than 200 mL per mole of dihalohydrocarbylphosphine. The adduct is combined with alcohol and a carbonate or with a solution of metal hydroxide and water to form the phospholene oxide.

The invention discloses an MXene black phosphorene composite sponge and a preparation method thereof. The MXene black phosphorene composite sponge has a three-dimensional macrostructure, has a continuous three-dimensional porous structure inside, contains micropores, mesopores and macropores, and has a specific surface area of 3-500 m<2> / g and conductivity of 0.01-1000 S / cm. The preparation methodcomprises the following steps: adding black phosphorene into an MXene dispersion under the protection of inert gas, uniformly dispersing, adding a cross-linking agent, standing, molding, carrying outsolution replacement, and carrying out circulating freeze-drying treatment to obtain the MXene black phosphorene composite sponge material. The MXene black phosphorene composite sponge provided by the invention has the advantages of high conductivity, high strength, high specific surface area and excellent photoelectric properties, and has wide application prospects in the fields of electronic information, energy environments and the like.

The invention belongs to the field of heat-conducting materials, and discloses a preparation method and application of a green nanocellulose high-heat-conductivity composite film. The green nanocellulose high-thermal-conductivity composite film is prepared by the following steps: firstly, preparing aminated phosphorene by a ball milling method, then carrying out covalent reaction on the aminated phosphorene and carboxymethyl chitosan, and finally adding the aminated phosphorene and carboxymethyl chitosan into a nanocellulose solution, wherein the mass ratio of the aminated phosphorene to the carboxymethyl chitosan is (1:1)-(1:10), and the mass ratio of the aminated phosphorene / carboxymethyl chitosan to the nanocellulose is (1:1)-(1:10). The heat conductivity coefficient of the green nanocellulose high-heat-conductivity composite film in the plane direction is larger than 5 W / m.k.

The invention relates to a preparation method of phospholene oxide, substituted phospholene oxide and a preparation method of the substituted phospholene oxide and belongs to the technical field of organic synthesis. The preparation method of the phospholene oxide comprises the following steps: 1) enabling phosphorus trihalide and chloroethanol to react at -10 to 40 DEG C for 0.5 to 3h so as to obtain a compound shown as a formula I; 2) enabling the compound shown as the formula I, a catalyst, a polymerization inhibitor and 1,3-butadiene to react at room temperature for 4 to 10h; then raisingthe temperature to 40 to 80 DEG C and reacting for 12 to 24h; then raising the temperature to 80 to 100 DEG C and reacting for 8 to 14h to obtain the phospholene oxide. The e preparation method of thephospholene oxide, provided by the invention, takes the phosphorus halide and the chloroethanol as raw materials, and the raw materials are easy to obtain and the price is low; reaction conditions are moderate and the method is simple and feasible and is low-cost.

The invention discloses a preparation method of a nucleophilic phosphorene compound, and belongs to the field of chemical medicine preparation. Phosphorene (RP) is a monovalent phosphorus compound with a six-electron structure. As a phosphorus analogue of carbene, phosphorene is always an important organophosphorus reagent. Due to the instability of free phosphorene, chemists synthesize Lewis acidand Lewis alkali complexes of phosphorene by utilizing the dual characteristics of phosphorene molecules. The two types of complexed phosphorene are higher in stability and easier to regulate and control in reactivity, especially nucleophilic phosphorene coordinated by Lewis alkali. According to the invention, the nucleophilic phosphorene compound can be obtained with high yield by using the hydride of precursor phosphorus to react with alkali at low temperature in the presence of crown ether / cryptand. The obtained target product can be used as a catalyst for various catalytic reactions.

The present invention provides novel cyclic phosphorus-containing compounds, namely hydroxyl-functional phospholene-1-oxides, serving as highly efficient reactive flame retardants in urethane systems, particularly in flexible polyurethane foams, semi-rigid and rigid polyurethane and polyisocyanurate foams. The invention further provides fire-retarded polyurethane compositions comprising said hydroxyl-functional phospholene-1-oxides.

The invention discloses a method for preparing phosphaalkene by utilizing electrochemistry. The method comprises the following steps: firstly, assembling an electrolytic cell by using an inert electrode as a positive electrode and phosphorus as a negative electrode, wherein in the electrolytic cell, the electrolyte solution is one or several of an aqueous electrolyte solution, an organic electrolyte solution and an ionic liquid electrolyte solution containing the electrolyte; applying direct current or alternating current voltage between the two electrodes of the electrolytic cell and stripping the phosphorus into phosphaalkene under a function of a direct current electric field or an alternating current electric field; and performing filtration treatment to obtain a stripped product, washing the stripped product for a plurality of times by using an organic solvent, centrifugally separating and drying to obtain the required phosphaalkene. According to the method, a phosphaalkene material with good quality, high yield and low cost can be conveniently, quickly and securely produced in an environment-friendly form, and can be applied to multiple fields of secondary ion batteries, supercapacitors, solar batteries, fuel batteries, electro-catalysis, electronic elements, bioanalysis, biological sensors and the like.

The present invention relates to a kind of preparation method of flame retardant methylphenylmethoxy (phosphacyclomethoxy) silane compound, the structure of the compound is shown in the following formula: the preparation method is: under the protection of nitrogen, add an organic solvent, Then add 1-oxygen-1-methyl-4-ethyl-4-hydroxymethyl-2, 6-dioxa-1-phosphorinane and methylphenyldimethoxysilane to control its The molar ratio is 1:1-1:1.4, the temperature is raised to 100-140°C, the temperature at the top of the fractionation column is controlled not to be higher than 65°C, and the generated methanol is fractionated, and the fractionation reaction is 6-10h until the fractionated methanol reaches the theoretical amount. The reaction is stopped, and after purification treatment, methylphenylmethoxyl (phosphacyclomethoxyl) silane is obtained; the product of the present invention has high flame retardancy, good compatibility with macromolecules, and is suitable for use as polyvinyl chloride, polyurethane, Flame retardant for polyester, unsaturated resin, epoxy resin, furan resin, polyvinyl alcohol and other materials. The preparation process is simple, the equipment investment is small, the large-scale production is easy, and the application and development prospects are very good.

The invention discloses a nitrogen-doped phosphorene quantum dot and a preparation method thereof. The preparation method comprises the steps that red phosphorus, a cyanamide compound and a catalyst are mixed and heated, and a nitrogen-doped black phosphorus material is generated through a reaction; the nitrogen-doped black phosphorus material is ground into powder, a dispersion medium and sulfonate containing trivalent rare earth elements are added, and ultrasonic treatment is carried out to obtain an ultrasonic dispersion liquid; the ultrasonic dispersion liquid is centrifuged, and the nitrogen-doped phosphorene quantum dots are prepared. According to the nitrogen-doped phosphorene quantum dot, the nitride with the layered structure is doped in the black phosphorus material, so that the prepared nitrogen-doped phosphorene quantum dot has relatively high polarity, nitrogen atoms in the nitrogen-doped phosphorene quantum dot can generate hydrogen bond interaction with hydrogen atoms in water, and the nitrogen-doped quantum dot has relatively high water solubility compared with the phosphorene quantum dot; therefore, agglomeration of the nitrogen-doped phosphorene quantum dots in a water solvent can be effectively avoided, and the nitrogen-doped phosphorene quantum dots are easy to disperse after being dried.

The invention discloses a porous three-dimensional phosphorene and its preparation method and application. The porous three-dimensional phosphorene has a stable three-dimensional structure formed by the self-crosslinking assembly of black phosphorene, the porosity is 50% to 98%, and the specific surface area is 200~2000m 2 / g. In the present invention, a strong electric field is applied in a two-electrode or multi-electrode system through an electrochemical method, and the intercalation agent and the auxiliary intercalation agent move directionally to the black phosphorus crystal and enter the interlayer, destroying the interlayer force of the black phosphorus crystal, and making the black phosphorus crystal The phosphorus layers maintain cross-linking but the interlayer distance increases, so that the black phosphorus crystals expand and the pores become larger, and the expanded black phosphorus is treated by freeze-drying to obtain porous three-dimensional black phosphorene. The porous three-dimensional black phosphorene has excellent physical and chemical properties, which can not only increase the wettability of the electrolyte to the electrode material, but also facilitate the adsorption and diffusion of reactants and metabolites during the reaction process, which can be applied to electrochemical catalytic hydrogen production field.

The invention relates to a method for preparing black phosphorus and phosphorene. The method for preparing black phosphorus includes reacting tin tetraiodide, tin and red phosphorus as raw materials to prepare black phosphorus. The involved preparation method of phosphorene includes treating the black phosphorus prepared in the present invention in N-methylpyrrolidone, absolute ethanol or N-cycloethylpyrrolidone for a reasonable period of time under the conditions of stirring, ultrasonic and 20-50°C. . The preparation method of the present invention adopts reasonable preparation raw materials and reaction conditions, and the synthesis time only requires 21-32 hours. Few-layer black phosphorus was successfully prepared using liquid phase exfoliation method. The preparation method has simple process, cheap raw materials and good repeatability.

The invention relates to the technical field of flame retardants, in particular to a preparation method of a novel phosphorus-nitrogen flame retardant, which comprises the following steps: step 1, mixing and ball-milling black phosphorus crystals and amine substances in an inert atmosphere; 2, transferring a ball-milled product obtained in the step 1 into a centrifugal tube by using a polar solvent, carrying out centrifugal treatment, then collecting an upper-layer suspension, continuously centrifuging, collecting a lower-layer precipitate, and drying, so as to obtain an amino-grafted phosphorene nanosheet; 3, melamine is dissolved in deionized water, a formaldehyde solution is slowly added under the heating condition, the pH is adjusted to be alkaline, a reaction is conducted, and a melamine-formaldehyde prepolymer is obtained; and 4, adding the amino-grafted phosphorene nanosheet prepared in the step 2 into the melamine-formaldehyde prepolymer prepared in the step 3, mixing, dispersing, filtering, and drying in vacuum to obtain the novel phosphorus-nitrogen flame retardant.

A flexible polyurethane foam article exhibiting flame resistance comprises the reaction product of an isocyanate and an isocyanate-reactive component comprising a polyol reactive with the isocyanate. The isocyanate and the isocyanate-reactive component are reacted in the presence of a blowing agent and a phospholene oxide. A method of producing the flexible polyurethane foam article includes the step of reacting the isocyanate and the isocyanate-reactive component in the presence of the blowing agent and an effective amount of the phospholene oxide to form the flexible polyurethane foam article which is flame resistant.

The invention relates to a rhodium / phosphorene supported catalyst and its preparation method and application. The rhodium / phosphorene supported catalyst consists of sheet-layer phosphorene and RhCl 3 Made, the preparation method comprises: black phosphorus is assisted by liquid-phase ultrasonic exfoliation to obtain graphene-like sheet structure; RhCl 3 Dissolved in deionized water, stirred evenly, added to the sheet-layer phosphorene according to the proportion, reacted at 30-150°C for 60-600min, and then centrifuged and dried to obtain the product. The preparation method of the rhodium / phosphorene supported catalyst is simple, convenient and environmentally friendly; the prepared supported catalyst has high activity and good performance. The prepared supported catalyst is used for hydrogenation catalysis of rubber to achieve a higher degree of hydrogenation.

The invention belongs to the field of heat-conducting materials, and discloses a preparation method and application of a green nano-cellulose high heat-conductivity composite film. The green nanocellulose high thermal conductivity composite film is prepared by firstly preparing the amidated phosphorene by ball milling, then covalently reacting with carboxymethyl chitosan, and finally adding it to the nanocellulose solution; the The mass ratio of the aminated phosphorene to the carboxymethyl chitosan is 1:1 to 1:10; the mass ratio of the aminoated phosphorene / carboxymethyl chitosan to the nanocellulose is 1:1 to 1: 10. The green nanocellulose high thermal conductivity composite film of the present invention has a thermal conductivity greater than 5 W / m·k in the plane direction.

The invention provides a coating preparation method of a nano composite material membrane. The method comprises the following steps: adding two kinds of nano powder of graphene and phosphorene into a solvent, or adding nano carbon powder, nano gold powder and nano silver powder into the solvent, and fusing to prepare conductive paste; and uniformly coating a flexible membranewith the conductive paste to form the flexible nano composite material membrane. According to the prepared nano composite material membrane, the flexible membrane is taken as the substrate, so that the flexibility and the strength of the nano composite material membrane can be ensured, and the prepared nano composite material membrane is not easy to damage so as to meet the requirements of preparing health care or physiotherapy products; and by adopting a conductive paste coating mode, the conductive performance of the product can be guaranteed, the two can be firmly combined and are not easy to fall off, and the service life of the product is guaranteed.

The present invention provides novel cyclic phosphorus-containing compounds, namely hydroxyl-functional phospholene-1-oxides, serving as highly efficient reactive flame retardants in urethane systems, particularly in flexible polyurethane foams, rigid polyurethane foams and rigid polyisocyanurate foams. The invention further provides fire-retarded polyurethane compositions comprising said hydroxyl-functional phospholene-1-oxides.

The invention relates to the technical field of hard alloys, in particular to a high-hardness and high-toughness hard alloy and a preparation method thereof. The high-hardness and high-toughness hard alloy is prepared from 60-95 wt% of WC powder, 5-10 wt% of Co powder, 2-5 wt% of Ni powder and 0.1-1 wt% of phosphorene. The preparation method comprises the steps that WC powder, Co powder, Ni powder and phosphorene are mixed and added into absolute ethyl alcohol, dried mixed powder is obtained through ultrasonic treatment, vacuum drying and stoving, then the mixed powder is placed in spark plasma sintering equipment to be sintered, and the corresponding high-hardness and high-toughness hard alloy is obtained. The hard alloy with high hardness and high toughness is obtained by modifying the hard alloy, and the hard alloy has excellent application prospects.

The invention relates to a preparing method for a phosphorus-silicon synergistic flame retardant phenyl dimethoxy (phosphor heterocycle methoxyl) silicane compound. The structure of the compound is as shown in the description. The preparing method comprises the steps that under protection of nitrogen, the mole ratio of 1-oxo-1-methyl-4-ethyl-4-hydroxymethyl-2,6-dioxa-1-phosphorinane to phenyl trimethoxy silane is controlled to be 1:1-1:1.4, organic solvent is added, temperature is raised to 100 DEG C-140 DEG C, the temperature of a fractional distillation column top is controlled to be not higher than 65 DEG C, generated methyl alcohol is distilled, the fractional distillation reaction is carried out for 5-9 h, the reaction is not stopped until the quantity of methyl alcohol distilled reaches the theory amount, and purification is carried out to obtain phenyl dimethoxy (phosphor heterocycle methoxyl) silicane. The compound is suitable for serving as flame retardant of materials such as polyvinyl chloride, polyurethane, unsaturated polyester resin, epoxy resin, furan resin and polyvinyl alcohol, the production technology is simple, equipment investment is small, industrialized production is achieved easily, and the compound has good application and development prospects.

The invention relates to a preparation method of a flame retardant dodecyl dimethoxy (phosphacyclomethoxy) silane compound. The structure of the compound is shown in the following formula: the preparation method is: under the protection of nitrogen, the In a reactor with a high-efficiency fractionation device, control 1-oxygen-1-methyl-4-ethyl-4-hydroxymethyl-2, 6-dioxa-1-phosphorinyl and dodecyl The molar ratio of trimethoxysilane is 1:1-1:1.4, adding an organic solvent, raising the temperature to 90-140°C, and fractionally distilling off the generated methanol. The fractional distillation reaction lasts for 6-11 hours until no methanol is produced, and is purified to obtain dodecane Dimethoxy (phosphacyclomethoxy) silane; the product of the present invention is suitable for flame retardants of materials such as polyvinyl chloride, polyurethane, unsaturated resin, epoxy resin, furan resin, polyvinyl alcohol, and production The process is simple, the equipment investment is small, the industrialized production is easy to realize, and the method has good application and development prospects.

The invention discloses a nitrogen-doped phosphorene quantum dot and a preparation method thereof, wherein the preparation method comprises the steps of: mixing and heating red phosphorus, a cyanamide compound and a catalyst, and reacting to form a nitrogen-doped black phosphorus material; After grinding the nitrogen-doped black phosphorus material into powder, adding a dispersion medium and a sulfonate containing trivalent rare earth elements for ultrasonic treatment to obtain an ultrasonic dispersion; centrifuging the ultrasonic dispersion to obtain the Nitrogen-doped phosphorene quantum dots. The present invention makes the nitrogen-doped phosphorene quantum dots have higher polarity by doping layered nitrides in the black phosphorus material, and the nitrogen atoms in the nitrogen-doped phosphorene quantum dots can be combined with The hydrogen atoms in the water produce hydrogen bond interactions, making the nitrogen-doped quantum dots have higher water solubility than the phosphorene quantum dots, thereby effectively avoiding the agglomeration of the nitrogen-doped phosphorene quantum dots in the water solvent, This makes nitrogen-doped phosphorene quantum dots easy to disperse after drying.