10 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 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 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.

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 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.