17 results about "Phosphorous chloride" patented technology

The invention relates to a preparation process of high-purity lithium hexafluorophosphate, which comprises the following specific steps: S1, quantitatively adding anhydrous hydrogen fluoride into a corresponding reaction kettle body, and controlling the environment temperature in the reaction kettle body at-50 DEG C to-20 DEG C through a temperature control device; s2, maintaining the pressure in the reaction kettle body at 0.1-0.5 MPa, dispersing and adding solid phosphorus pentachloride into the reaction kettle body through a corresponding feeding device, and enabling the solid phosphorus pentachloride to react with the anhydrous hydrogen fluoride in the step S1 at the temperature of-50 DEG C to-20 DEG C to obtain phosphorus pentafluoride and gaseous hydrogen chloride, the gaseous hydrogen chloride escapes from the reaction liquid and then is discharged for recovery or absorption treatment; and S3, dispersing and adding lithium fluoride into the reaction kettle body through the feeding device, and carrying out complexing reaction on the lithium fluoride and phosphorus pentafluoride in the anhydrous hydrogen fluoride to obtain lithium hexafluorophosphate. The reaction process is high in controllability, so that the high-purity lithium hexafluorophosphate product can be stably prepared.

This invention belongs to the field of oxyacid synthesis technology of phosphorus, specifically relating to a method for producing phosphorous acid. The production method includes: (1) adding a metal precursor, organic ligand, reaction promoter, structure directing agent and swelling resistant agent to a pore-forming agent and heating to react, to obtain a mixture; then mixing the mixture with a polymer monomer, crosslinking agent and initiator to obtain an oil phase for later use; mixing a dispersant with water and removing oxygen to obtain an aqueous phase for later use; (2) mixing the oil phase and the aqueous phase to carry out a crosslinking reaction to obtain a crude product; (3) washing, acidifying and vacuum drying the crude product to obtain a porous polymer carrier; (4) after the porous polymer carrier swells in water, adding phosphorus trichloride to it, carrying out a heat preservation reaction, and post-treatment to obtain phosphorous acid. This invention improves the production efficiency of phosphorous acid while ensuring a high yield of phosphorous acid by preparing a porous polymer carrier and using it as a medium for the hydrolysis of phosphorus trichloride to prepare phosphorous acid.

A method for synthesizing an antioxidant 168 by using a microchannel continuous flow process belongs to the technical field of chemical synthesis, adopts a microchannel esterification-microchannel ester exchange two-stage continuous process, and realizes the reaction of phosphorus trichloride and low-carbon chain alcohol to generate phosphorous acid dialkyl ester through the efficient mass transfer characteristic of a microchannel reactor in the esterification stage; hydrogen chloride generated by the reaction is immediately and directionally led out and recycled as industrial hydrochloric acid, a neutralizer does not need to be added, a microchannel reactor with an inner wall immobilized catalyst or a high-temperature and high-pressure strengthening process is adopted in the ester exchange stage, the reaction without catalyst residue or participation of the dialkyl phosphite and the 2, 4-di-tert-butylphenol is realized, no salt impurities are generated in the whole process, and the production cost is reduced. The method solves the problems of quality, cost, safety and the like caused by the use of a neutralizer, complex desalination, catalyst residue, salt-containing wastewater, remarkable amplification effect and the like in the traditional process, and has the industrial advantages of continuity, cleanness and high purity.

The invention relates to the technical field of chemical intermediates, and relates to C07F, in particular to a preparation method for co-production of acetyl chloride and phosphorous acid as well as a product and application thereof. The preparation method at least comprises the following steps: S1, stirring and cooling acetic acid and a catalyst, dropwise adding phosphorus trichloride, heating to 20-45 DEG C, and reacting for 0.5-6 hours; s2, after the reaction is finished, carrying out negative pressure desolvation to obtain a crude product acetyl chloride, and continuously heating to remove excessive phosphorus trichloride, so as to obtain a crude product phosphorous acid; s3, rectifying the crude product acetyl chloride to obtain an acetyl chloride product; recrystallizing the crude phosphorous acid to obtain a phosphorous acid product; the catalyst comprises at least one of aluminum trichloride, ferric trichloride, titanium tetrachloride, ytterbium trifluoromethanesulfonate and iodine; the mass ratio of the acetic acid to the catalyst is 1: (0-0.003). The method provided by the invention has the characteristics of high conversion rate, high yield, high content, small amount of three wastes, no solvent pollution, simple process, easy industrial preparation of acetyl chloride and the like.

The invention provides low-ring reactive silicone oil and a preparation method and application thereof.The preparation method includes the steps that low-ring-terminated vinyl silicone oil, a platinum-containing catalyst and inorganic filler are mixed according to a certain proportion to obtain a component A, low-ring-side-chain hydrogen-containing silicone oil, an inhibitor and inorganic filler are mixed according to a certain proportion to obtain a component B, and the mass ratio of the component A to the component B is 1: (0.5-2). Wherein the low-ring-body vinyl-terminated silicone oil and the low-ring-body side-chain hydrogen-containing silicone oil are obtained by respectively carrying out polycondensation on hydroxyl-terminated silicone oil and a vinyl-terminated silicone oil end-capping agent and a side-chain hydrogen-containing silicone oil end-capping agent under the catalysis of phosphonitrile chloride, then neutralizing by using a crown ether neutralizer and carrying out heating and low-temperature removal, and the low-ring-body vinyl-terminated silicone oil and the low-ring-body side-chain hydrogen-containing silicone oil are low in ring content; when the silicon rubber is further applied to double-component addition type silicon rubber for electronic packaging, poor contact of contacts after long-term service of electric appliance components can be avoided; meanwhile, an organic amine neutralizer is not used, so that the adverse effect on a hydrosilylation platinum catalyst is avoided, the hydrosilylation rate is high, and the curing time is short.

The invention discloses a fluororubber composition. The invention discloses a preparation method of the fluororubber composition, which comprises the following steps: mixing and stirring hollow activated graphene, vinyl-terminated polydimethylsiloxane, alpha, omega-dihydroxy polydimethylsiloxane, an addition reaction catalyst and a plasticizer, and then adding fluororubber for plastication to obtain the fluororubber compound; the preparation method comprises the following steps: fully stirring vinyl-terminated polydimethylsiloxane, expanded graphite particles, alumina powder, a cross-linking agent and an addition reaction inhibitor to obtain an expanded graphite-alumina compound; mixing the fluororubber compound, the expanded graphite-aluminum oxide compound, calcium hydroxide, active magnesium oxide, palm wax, hexafluorobisphenol A and benzyltriphenyl phosphorus chloride, carrying out thin-passing blanking, carrying out compression molding, standing, vulcanizing at 150-170 DEG C for 5-12 minutes, and cooling to room temperature to obtain the fluororubber composition.

The invention discloses a nanosheet composite material as well as a preparation method and application thereof, and belongs to the technical field of photocatalysis. The preparation method of the nanosheet composite material comprises the following steps: forming a deep eutectic solvent DESs under a heating condition of a bismuth source, tetrabutyl phosphorus chloride and polyhydric alcohol; placing the deep eutectic solvent DESs in a microwave reactor for reaction, cooling to room temperature along with a furnace after the reaction, cleaning with a cleaning agent, and drying to obtain the nanosheet composite material. The preparation method disclosed by the invention is simple to operate, low in preparation cost, short in reaction time and easy for industrial production, and the obtained Bi-BiOCl material is regular in morphology and has better crystal form and photocatalytic activity.

The invention relates to a preparation method of low-ring high-viscosity methyl silicone oil, which comprises the following steps: (S1) carrying out condensation polymerization on 100 parts by mass of hydroxyl-terminated polydimethylsiloxane and 1-20 parts by mass of dimethyl silicone oil under the action of 0.001-0.005 part by mass of phosphonitrile chloride catalyst; (S2) adding 0.004-0.015 part of a neutralizing agent, and carrying out a neutralization reaction; the neutralizer is prepared from 10 to 70 weight percent of crown ether substances and the balance of non-polar solvent; and (S3) raising the temperature to remove the low-viscosity methyl silicone oil to obtain the low-ring-body high-viscosity methyl silicone oil. By adopting the neutralizer including crown ether, the defects of unstable viscosity and high ring content caused by the conventional neutralizer are avoided, the low-ring high-viscosity methyl silicone oil with stable viscosity is obtained, and the low-ring high-viscosity methyl silicone oil is suitable for being prepared into shampoo products.

The application relates to a preparation method of a multi-element doped carbon-coated ternary positive electrode material, and the preparation method is as follows: ternary precursors are placed into a solution, trimeric phosphonitrilic chloride and 4,4'-sulfonyl diphenol are added and stirred, trithylamine is added after stirring for a certain time, continuous stirring is carried out, and after washing, drying is carried out to obtain a PZS (polytrimeric phosphonitrilic chloride-co-4,4'-sulfonyl diphenol) coated ternary positive electrode material; the ternary positive electrode material after coating is mixed with a lithium source in a high-speed mixer, the mixed sample is placed in a tube furnace for sintering, and the sample after sintering is the multi-element doped carbon-coated ternary positive electrode material NCM@C. The multi-element doped carbon layer coating can improve the better conductivity and the stronger hardness, and therefore, the lithium nickel mixed arrangement, soluble lithium, the first discharge specific capacity, the first coulomb efficiency, the capacity retention rate and other parameters are better.

The application relates to the technical field of coatings, and discloses a preparation method of impact-resistant high-strength polyurethane coating and application of the impact-resistant high-strength polyurethane coating in stone materials. The preparation method comprises the following steps: taking tri(2-hydroxyethyl) isocyanurate, 2,2-dimethylol propionic acid, epichlorohydrin and N-benzyl ethanolamine as raw materials, and performing esterification reaction, substitution reaction and ring-opening reaction to obtain a triazine-based hyperbranched polyol. Taking phenyl dichlorophosphine and ethylene glycol as raw materials, substitution reaction is performed to obtain phenyl dihydroxy phosphine oxide. Taking polyethylene glycol as a soft segment, isophorone diisocyanate as a hard segment, phenyl dihydroxy phosphine oxide as a chain extender and the triazine-based hyperbranched polyol with a hydroxyl group as a terminal, a polyurethane emulsion is prepared, and further, the impact-resistant high-strength polyurethane coating is obtained. The polyurethane coating prepared by the application has good impact resistance, flame resistance and strength.

The invention discloses a cross-linked polymer flame retardant containing nitrogen and phosphorus elements. The molecular structure of the cross-linked polymer flame retardant comprises the following raw materials: cyanuric acid, phosphorus trichloride, a bifunctional compound of which the end group contains binary hydroxyl, trialkyl phosphite and the like. A macromolecular structure unit containing a cyanuric acid phosphate cross-linked structure is obtained through two steps of mixing reaction and transesterification isomerization ring-opening polymerization reaction; the molecular weight of the cross-linked polymer flame retardant is 10000 to 100000. The cross-linked polymer flame retardant disclosed by the invention not only has high melting point, moisture absorption resistance and excellent flame retardant property, but also has good compatibility with a high polymer material matrix, low chloride ion residue and low preparation cost. The invention also discloses a preparation method of the cross-linked polymer flame retardant containing nitrogen and phosphorus elements. The method is simple and easy to control, high in yield and easy for industrial production.

The invention belongs to the technical field of oxygen-containing acid synthesis of phosphorus, and particularly relates to a phosphorous acid production method. The production method comprises the following steps: (1) adding a metal precursor, an organic ligand, a reaction promoter, a structure-directing agent and a swelling-resistant agent into a pore-foaming agent, and carrying out a heating reaction to prepare a mixture; then blending the mixture with a polymer monomer, a cross-linking agent and an initiator to obtain an oil phase for later use; blending the dispersing agent with water, and deoxidizing to obtain a water phase for later use; (2) blending the oil phase and the water phase for cross-linking reaction to obtain a crude product; (3) carrying out washing, acidification and vacuum drying on the crude product to obtain a porous polymer carrier; and (4) after the porous polymer carrier swells in water, adding phosphorus trichloride into the porous polymer carrier, and carrying out heat preservation reaction and post-treatment to obtain the phosphorous acid. According to the method, the porous polymer carrier is prepared and used as a medium for preparing the phosphorous acid by hydrolyzing phosphorus trichloride, so that the production efficiency of the phosphorous acid is further improved while the high yield of the phosphorous acid is ensured.

The invention discloses a preparation method of a chlorine-free and fluorine-free combined vulcanizing agent, which comprises the following steps: a) adding benzyl triphenyl phosphorus chloride and an organic solvent into a reaction kettle, and heating and refluxing to completely dissolve the benzyl triphenyl phosphorus chloride; b) slowly adding strong base and an organic solvent into the solution in the step a), and reacting for 2-3 hours; c) adding organic acid into the mixed solution in the step b to neutralize the pH value to 7.5-9; d) adding a bisphenol vulcanizing agent into the reaction system in the step c, and heating and refluxing to obtain a co-melt of benzyltriphenylphosphine hydroxide and the bisphenol vulcanizing agent; e) heating the reactant obtained in the step d to remove the solvent, and repeatedly washing until the detected chloride ion content in the water layer at the upper part is lower than 5ppm; and f) after moisture removal, granulating to obtain the uniform semitransparent granular chlorine-free fluorine combined vulcanizing agent. The fluorine combined vulcanizing agent with the chlorine ion content of less than 5 ppm and stable high-temperature performance is provided, and fluororubber produced and prepared by adopting the fluorine combined vulcanizing agent is very friendly to electronic products.

The present invention relates to the field of photodynamic technology, and in particular to a fully organic nano photosensitizer with high singlet oxygen production activity, and its preparation method and application. 3-amino-1,2,4-triazole is mixed with tripolyphosphazene chloride, followed by thermal polymerization and copolymerization heat treatment to obtain P-C3N5; P-C3N5 is ultrasonically mixed with a 3,4,9,10-perylenetetracarboxylic acid diimide solution and water, and filtered after standing. The filter residue is washed and dried to obtain P-C3N5 / PDI; P-C3N5 / PDI is mixed with a nitric acid solution and heat-treated, and the obtained heat-treated product is washed and dried to obtain a dried product; the dried product is mixed with sodium hydroxide and water and then heat-treated to obtain a heat-treated product; the heat-treated product is centrifuged, and the obtained clear liquid is dialyzed to neutrality to obtain a fully organic nano photosensitizer. The fully organic nano photosensitizer material has good water dispersibility and can efficiently produce singlet oxygen under near-infrared light.

This utility model discloses a phosphorus trichloride tail gas buffer treatment device, belonging to the field of tail gas treatment technology. Key technical features include a spray purification chamber with a connecting pipe on its left side. A buffer tank is fixedly connected to the left side of the connecting pipe, and an air inlet pipe is fixedly connected to the bottom left side of the buffer tank. A pretreatment mechanism is fixedly connected to the left side of the air inlet pipe, and a refrigeration mechanism is installed at the front of the pretreatment mechanism. The pretreatment mechanism, through a limiting baffle and an electromagnetic one-way valve, separates and collects crystalline particles such as phosphorous acid and ferric phosphate in the tail gas into a collection box at the bottom, reducing the probability of them entering subsequent pipelines and causing blockages. The flared design of the exhaust hopper expands the diffusion area of ​​the cold air, further improving particle settling efficiency. The temperature sensor and PLC controller of the refrigeration mechanism monitor the temperature inside the buffer tank in real time, and the tail gas is cooled below the melting point of the crystals through a semiconductor cooling plate, promoting the early precipitation of crystals.

The application discloses a preparation method of methylene phosphorus dichloride, which comprises the following steps: in the presence of an organic solvent, taking compound 1 as a substrate, and under the action of trimethyl halosilane, the compound 1 is subjected to a cleavage reaction to generate an intermediate product, and the intermediate product is subjected to a chlorination reaction with a chlorinating agent to finally generate a product methylene phosphorus dichloride. Compared with the prior art, the method has the advantages of easy raw material acquisition, low cost, high yield, mild reaction condition, low danger coefficient and facilitation of large-scale industrial production.

The invention relates to the technical field of catalyst preparation and fine chemical separation, in particular to a preparation method, a product and application of a Ru-coated HENC catalyst. The preparation method comprises the following steps: adding 4, 4-sulfonyl diphenol and tripolyphosphazene chloride into an organic solvent 1 to obtain a solution D; adding a ZIF-8 solution into the solution D, uniformly mixing, and then adding triethylamine for reaction to obtain ZIF-8 (at) PZS; the ZIF-8 (at) PZS is calcined for the first time, and PSN / C is obtained; mixing the PSN / C with boric acid and polytetrafluoroethylene, and calcining 2 to obtain HENC; and dissolving the HENC and ruthenium salt in an organic solvent 2, adjusting the pH value of the reaction system to 7-8, and adding excessive reducing agent to react until no bubble is released, thereby obtaining the Ru-coated HENC catalyst. The Ru-coated HENC catalyst has a good removal effect on the valeraldehyde in the 1, 2-pentanediol.