46 results about "Phosphorous chloride" patented technology

The invention relates to a continuous synthesis technique of hydroxyethylidenediphosphonic acid, which comprises the following steps: 1. mixing raw materials: mixing phosphorus trichloride and acetic acid in a mol ratio of 1:(2.8-3.0) in a mixing kettle; 2. sending the mixture into a tubular reactor: pumping the mixture into the tubular reactor through a diaphragm pump; 3. carrying out esterification reaction while controlling the temperature of the tubular reactor at 70-130 DEG C; 4. separating the reaction mixture in a gas-liquid separator for recycling; 5. carrying out hydrolysis reaction to obtain the hydroxyethylidenediphosphonic acid; and 6. distilling out acetic acid under negative pressure to separate the acetic acid from the product, wherein the acetic acid enters an acetic acid storage tank as a raw material. In the invention, the hydroxyethylidenediphosphonic acid is continuously produced in a semi-closed system, thereby changing the existing intermittent production mode and enhancing the production efficiency; and the invention overcomes the defects of low product yield, too many side reactions and high contents of phosphorous acid and phosphoric acid in other preparation techniques, and implements complete cyclic utilization of acetic acids with different concentrations.

The invention discloses an ultra-long-life pure organic phosphorescent material with afterglow luminescence performance and its preparation method and application. The pure organic phosphorescent material is composed of phenylphosphorus and carbazole structure, which is DNCzPS or DNCzPSe. The carbazole React with phenylphosphorous dichloride at low temperature to obtain the intermediate dicarbazolylphenylphosphorus; then the intermediate can be subjected to sulfidation or selenization reaction to obtain the corresponding products DNCzPS and DNCzPSe. This type of pure organic phosphorescent material has obvious afterglow luminescence properties, which greatly prolongs the luminescence lifetime of organic materials. The prepared RMB anti-counterfeiting and multi-level two-dimensional code anti-prototype device has the characteristics of high resolution and multi-level anti-counterfeiting.

The invention discloses a synthetic method of photoinitiator dual (2, 4, 6-trimethylbenzene formyl group) phenyl phosphine oxide. The synthetic method comprises processes of using dichlorophenylphosphine and 2, 4, 6-trimethylbenzene acyl chloride to serve as raw materials, conducting a classification reaction under protection of nitrogen to generate dual(2, 4, 6-trimethylbenzene formyl group) phenyl phosphine, oxidizing hydrogen peroxide to obtain a target object-dual (2, 4, 6-trimethylbenzene formyl group) phenyl phosphine oxide. Compared with the existing industrial production, the process has the advantages of being safe in operation process, free of needs of dangerous metallic sodium or potassium, free of needs of using inflammable midbody phenyl phosphine, simple in reaction process, safe, easy to control, high in obtained product yield, good in quality and prone to achieve mass production and the like.

A method for synthesizing hydroxyl ethylidenediphosphonic acid belongs to synthesis of organo-phosphonic acid and is used in water stabilization. The phsophorus trichloride and acetic acid react at a temperature between 80 DEG C and 150 DEG C with an absolute pressure less than 760 millimeters mercury column, and the byproducts of hydrochloride and a few acetyl chlorides free of condensation are respectively retrieved and reused by combined recovery system of acetic acid and hydrochloric acid. The product of this method is obtained by hydrolyzing the acetylated hydroxyl ethylidenediphosphonic acid at a temperature between 80 DEG C and 150 DEG C with an absolute pressure no more than 760 millimeters mercury column; the collected hydrolysate of acetic acid after the distillation and the condensation is selected as raw material together with the acetic acid solution from the reclamation tower of acetic acid. The autoclave of 1000 litres daily produces products of 2500 kilograms with 60 % of solid content and less than 0.15 % of phosphorous acid; the yield rate of the products is more than 98 % calculated by phsophorus trichloride and is more than 96 % calculated by acetic acid.

The invention discloses a synthesis method of bis (2, 4-dibutylbenzene) pentaerythritol diphosphite, which comprises 1, synthesizing dichloropentaerythritol diphosphite: using xylene as solvent, adding pentaerythritol and catalyst, feeding nitrogen gas, adding phosphorous trichloride and absorbing generated hydrogen chloride gas via sodium hydroxide solution, and purifying reaction product to obtain the dichloropentaerythritol diphosphite, 2, synthesizing bis (2, 4-dibutylbenzene) pentaerythritol diphosphite: adding 2, 4-bis-tert-butylphenol into the reaction product of step 1, feeding nitrogen gas and mixing, absorbing generated hydrogen chloride gas via sodium hydroxide solution, and purifying the reaction product to obtain final product. The invention uses 2, 4-bis-tert-butylphenol, pentaerythritol and phosphorous trichloride as main materials, with low cost, easily processed reaction and high reaction yield.

The invention provides a chirality phosphine nitrogen compound containing N-aryl as well as a synthetic method and application thereof. The phosphine nitrogen compound is based on axial chirality or comprises a helical chirality skeleton, and is synthetized by taking optically pure axial chirality or helical chirality glycols compound, phosphorus trichloride and aromatic secondary amine as raw material for reaction. The raw material used in the method is easy to obtain, the reaction condition is mild, and the products are easy to separate and purify. The N-aryl phosphine nitrogen compound base on the axial chirality or the helical chirality skeleton synthetized by the method can be effectively applied in substitution reaction of allyl catalyzed by metal iridium, so that the product can be obtained with high enantioselectivity and regioselectivity, and the substrate scope of the product is greatly widened.

The invention discloses a high-performance natural rubber/styrene-butadiene rubber composite material. The raw materials include: natural rubber, styrene-butadiene rubber, rare-earth isoprene rubber, zinc oxide, stearic acid, sulfur, benzoyl peroxide, and an accelerator CZ, accelerator DM, accelerator NOBS, antioxidant, light calcium carbonate, magnesium oxide, calcium hydroxide, graphene oxide, bamboo charcoal powder, aluminum silicate, diatomaceous earth, sodium montmorillonite, benzyl triphenyl Phosphorous chloride, polyethylene glycol. The high-performance natural rubber/styrene-butadiene rubber composite material proposed by the invention has high strength, good heat resistance and wear resistance, can meet the use requirements of various fields, and has a long service life.

The invention discloses a continuous flow preparation method of diethyl methyl phosphite, which comprises the following steps: continuously adding ethanol and methyl phosphorus dichloride into a feedport of a continuous flow reactor, and continuously obtaining diethyl methyl phosphite at a discharge port of the continuous flow reactor. The method has the advantages of small liquid holdup, safe and efficient production process, solving of the problems of long reaction time and low efficiency in kettle type reaction, high product yield and purity, and simple and efficient process operation.

The invention discloses a continuous flow preparation method of diethyl methyl phosphite, which comprises the following steps: continuously adding ethanol and methyl phosphorus dichloride solution into a feed port of a continuous flow reactor, and continuously obtaining diethyl methyl phosphite at a discharge port of the continuous flow reactor. The method has the advantages of small liquid holdup, safe and efficient production process, solving of the problems of long reaction time and low efficiency in a kettle type reaction, high product yield and purity, and simple and efficient process operation.

The invention provides a method for preparing phosphorous acid and hydrogen chloride in an inner circulation tower by using phosphorus trichloride. The method comprises the following steps of: intermittently or continuously adding the phosphorus trichloride to the inner circulation tower, and then making the phosphorus trichloride react with a water solution in the tower to prepare a phosphorous acid water solution and a hydrogen chloride gas with large scale and high efficiency and yield and smoothly export the hydrogen chloride gas and heat. The method has the advantages of high reaction conversion rate and yield, steady reaction, high safety and the like and can be used for continuous production.

The application discloses a water-treated potassium ferrate sterilizing agent and a preparation method thereof. The water-treated potassium ferrate sterilizing agent is prepared by weighing and uniformly mixing potassium permanganate, concentrated hydrochloric acid, potassium hydroxide, iron nitrate nonahydrate, manganese dioxide, potassium chlorate, a polymerization inhibitor, triethylene tetramine, formaldehyde, phosphorus trichloride, a dispersing agent, sodium hydroxide, phosphorous acid, glycine and polyaspartic acid according to parts by weight. The melting point of the product is 205 DEG C; the scale inhibition rate is 96.9-98.9%; the sterilizing rate to escherichia coli, staphylococcus aureus, candida albicans, neisseria gonorrhoeae, penicillium, aspergillus, saprophytic bacteria and salmonella is 99-100%; when the water-treated potassium ferrate sterilizing agent is placed at 50-60 DEG C for a month, the sterilizing rate is 97.5-99.5%; when the water-treated potassium ferrate sterilizing agent is placed at 40-50 DEG C for half a year, the sterilizing rate is 96-99%; when the water-treated potassium ferrate sterilizing agent is placed at the room temperature for 1-2 years, the sterilizing rate is 95-97%.

The invention provides a bio-based macromolecular flame retardant as well as a preparation method and application thereof. The preparation method comprises the following steps of (1) preparing tanninphosphonitrile chloride ester by a grafting method: adding 10-30g of tannin and 5-20mL of triethylamine into 50-200ml of acetonitrile to obtain a mixture, heating the mixture to 30-45 DEG C, dropwiseadding 10-40ml of phosphonitrilic chloride trimer into the mixture, and then heating the mixture at 50 DEG C for 1-3h to obtain a mixed solution containing tannin phosphonitrile chloride ester; and (2) enabling the tannin phosphonitrile chloride to react with metaphenylenediamine: adding 10-30g of the metaphenylenediamine into the mixed solution obtained in the step (1), performing heating to 60-80 DEG C, performing reacting for 2-4 hours, performing filtering, performing cleaning with the acetonitrile, and performing drying to obtain the bio-based macromolecular flame retardant. The flame retardant provided by the invention has good thermal stability and flame retardance, and solves the problem of poor thermal stability of the tannin, and besides, as a flame retardant curing agent, the reticular macromolecular structure has less influence on the mechanical properties of epoxy resins.

The invention provides a graphene based anti-bacterial and wear-resistant double-component coating. According to the specific scheme, the coating contains a component A and a component B, wherein thecomponent A is prepared through steps as follows: an acrylic polymer aqueous dispersion is taken as a substrate, and graphene supported titanium dioxide serving as an anti-bacterial agent, 2-acryloyloxyethyl tributylphosphonium chloride-trimethoxy vinyl silicon oligomer containing fluoroalkyl as well as other auxiliaries are added; the component B is ketimine; graphene supported titanium dioxide is prepared from 1-10 mu m graphene oxide, 10-15 nm titanium dioxide particles and a silane coupling agent through uniform dispersion in water, reduction and drying. Acrylic polymers are subjected to monomer selection, glass beads are introduced, so that wear resistance is improved, a final product has excellent anti-bacterial performance, wear resistance, stain resistance and adhesive force, and the coating with the excellent anti-bacterial performance and wear resistance is suitable for being used in hospitals and schools with large volume of people.

The invention discloses a preparation method of a binder, namely, metharcylic acid, 2-isocyanatoethyl ester. The preparation method comprises the following steps of: (1) adding ethanol amine and an organic solvent into a reactor with a stirrer, a thermometer and a condensing tube, slowly dropping methylclhlorofonmate at 50-60 DEG C, and after dropping, continuously reacting for 2-4 hours; (2) adding a catalyst into the reactor, slowly dropping methylacryloyl at 80-100 DEG C, and after dropping, continuously reacting for 3-8 hours; (3) adding phosphorus pentachloride into the reactor to react at 50-100 DEG C and reacting for 48-72 hours; and (4) carrying out solid-liquid separation on the reactant obtained in step (3), depressurizing and distilling the filtrate, and collecting the fraction so as to obtain the metharcylic acid, 2-isocyanatoethyl ester. By utilizing the method, the generation of toxic phosgene in the production process is greatly reduced, so that potential safety hazard is reduced; the total yield is over 85%; and the whole process is generally free of environmental pollution.

The invention discloses a synthetic method of citicoline sodium. The synthetic method comprises the following steps: adding 5'-cytidylic acid, calcium phosphorylcholine chloride, ATP, an aqueous magnesium chloride solution and a Tris-HCl buffer solution into a reaction vessel, and carrying out uniform mixing; then, adjusting a pH value to 6.0-8.0, adding CMP phosphokinase, nucleoside diphosphate kinase and choline phosphate-cytidyltransferase, and carrying out a stirring reaction for 4-10 hours at a temperature of 25-50 DEG C; and conducting high-speed centrifugation, and taking a supernatantto obtain citicoline sodium. Compared with the traditional citicoline sodium synthesis process, the synthetic method provided by the invention is environment-friendly in a synthesis route, stable in yield and is beneficial for reducing energy consumption and protecting the environment, so the synthetic method is suitable for large-scale industrial production.

The invention relates to a method for synthesizing tri(3,5,6-trichloropyridinyl)phosphite, which comprises the following steps of: synthesizing 2-hydroxy-3,5,6-trichloropyridine under an acidic condition by using sodium 3,5,6-trichloropyridin-2-olate as a raw material, conducting drying and dehydrating, and controlling the reaction temperature of the product, a catalyst and phosphorus trichlorideto be 70-93 DEG C on the premise of micro-negative pressure to obtain the tri(3,5,6-trichloropyridinyl)phosphite. The specific synthetic route is shown in the specification. Micro negative pressure and the catalyst are introduced in the reaction process, so that the generation of diester and other side reactions is reduced, the reaction speed is increased, the reaction time is shortened, the purity and yield of a target product are improved, meanwhile, an organic alkali or organic ammonia acid-binding agent is not used, the production cost is reduced, and three wastes are reduced.

The invention relates to a self-loading diphosphine-palladium catalyst and a preparation method and application thereof. According to the preparation method, diphenyl phosphorous chloride is used as a raw material, and after the chloride is replaced by a Grignard reagent, the raw material is coordinated with palladium bichloride to form the catalyst. The catalyst has the advantages that (1), the catalyst has higher thermal stability; (2), the catalyst can be used for catalyzing a Suzuki-Miyaura coupling reaction under a mild condition and acquires an excellent catalyzing effect; (3), after a catalyzing reaction is completed, the catalyst can be reused through simple centrifugal filtration, and the difficult problem of recycling and reutilization of a homogeneous catalyst is solved. The preparation method is simple and feasible in reaction routes, and the catalyst can be used as an efficient catalyst to be applied to the synthesis of medicines, spices, pesticides and functional materials.

The invention discloses a synthetic method of a surfactant. The synthetic method comprises the following steps: (1) adding fatty alcohol, a catalyst and amino acid ester into a reactor; (2) closing the reactor, and slowly heating to 200-300 DEG C; (3) carrying out a heat preservation reaction for 2-10 hours; (4) degassing; and (5) treating to obtain a finished product. According to the invention,fatty alcohol is directly selected as an acylation reagent to perform a reaction, so that the step of fatty acid acylation is omitted, the selection of dangerous substance acylation reagents such as phosgene, thionyl chloride, trichloromethyl chloroformate, phosphorus trichloride, phosphorus pentachloride and phosphorus oxychloride is reduced, the emission of byproducts such as phosphorous acid and the like is reduced, and the method is feasible from the aspect of reaction mechanism; and fatty alcohol and amino acid ester are selected to be subjected to a direct reaction, so that impurities such as chlorine ions and the like are not introduced in the process, and the target product is obtained through the direct reaction so as to eliminate the steps of acidification, salification or waterwashing desalination and reduce the use and discharge of salt-containing wastewater or an organic solvent.

The invention relates to a method for determination of the content of main components of a phosphorus trichloride hydrolysis solution. The method is carried out according to the following steps: 1) accurately weighing a phosphorus trichloride hydrolysis solution sample, adding water, in the condition of stirring, titrating the solution to the pH of 4.5 with a sodium hydroxide standard titration solution, and recording consumption volume V1 of the sodium hydroxide standard titration solution; 2) continuing to titrate the solution to the pH of 9.5 with the sodium hydroxide standard titration solution, and recording consumption volume V2 of the sodium hydroxide standard titration solution; 3) further adding an excess neutral calcium chloride solution, titrating the solution to the pH of 7.53 with the sodium hydroxide standard titration solution, and recording consumption volume V3 of the sodium hydroxide standard titration solution; and 4) calculating results. Through use of the method, fast and real-time detection of the content of hydrochloric acid, phosphorous acid and phosphoric acid in the phosphorus trichloride hydrolysis solution can be realized, and the method has the advantages of simple operation, high accuracy, good precision, good reproducibility and the like. But if a conventional acid-base indicator method is adopted, the phosphorus trichloride hydrolysis solution sample cannot be accurately determined because of low phosphoric acid content in the phosphorus trichloride hydrolysis solution sample.

The invention provides disinfection powder of landscape fish pond water, and relates to the technical field of aquaculture. The disinfection powder is prepared from the following raw materials: 30 to 40 parts of a chlorine dioxide solution, 15 to 25 parts of a hydrogen peroxide solution, 10 to 20 parts of dodecyl dimethyl benzyl ammonium chloride, 8 to 10 parts of polyhydroxypropyl polyethylene-polyamine, 2 to 4 parts of dodecyl triphenyl phosphorous chloride, 3 to 5 parts of salviae miltiorrhizae radix et rhizoma, 2 to 4 parts of radix angelicae pubescentis, 3 to 5 parts of herba junci setchuensis, 2 to 4 parts of fructus gleditsiae, 3 to 5 parts of folium artemisiae argyi, 2 to 4 parts of radix angelicae dahurioae, 2 to 4 parts of herba pogostemonis, 1 to 3 parts of rhizoma kaempferiae, 1 to 3 parts of Chinese angelica, 2 to 4 parts of fortune loosestrife herb, 1 to 3 parts of shrubalthea bark, 1 to 3 parts of cuckoo-bud and 2 to 4 parts of carpesium herb. The disinfection powder of the landscape fish pond water has the beneficial effects that the prepared disinfection powder has a reasonable formula and a simple preparation process, has a very great sterilization effect on fish culture water; the content of toxic substances in a water body is small; normal survive of landscape fishes is guaranteed; the fish water does not need to be frequently replaced, and the disinfection powder is convenient and simple to use.

A process for preparing Alunphosphonic acid includes such steps as reflux reaction between gamma-aminobutanoic acid, PCl3, and phosphorous acid in the inertial solvent whose boiling point is 50-90 deg.C, and post-treating. Its reaction temp can be controlled well.

The invention discloses a benzyltriphenylphosphine tetranuclear manganese (II) complex, and the molecular formula of the complex is as follows: metal chloride, benzyltriphenylphosphonium chloride andpotassium thiocyanate are used as raw materials to synthesize a hybrid material at room temperature. The material has excellent fluorescence property and important value in the aspects of nonlinear optical property and information storage.

The invention provides a synthesizing method of 3, 3-dimethyl butyraldehyde, relates to an organic synthesis intermediate, particularly a method for preparing 3, 3-dimethyl butyraldehyde by the reaction of 3, 3-dimethylbutyric acid and phosphorus trichloride. A synthesizing method of 3, 3-dimethyl butyraldehyde with simple process, simple and convenient operation, high safety, low production cost and small influence to environment is provided. The method comprises the steps: the 3, 3-dimethylbutyric acid is added in a reactor and stirred, the phosphorus trichloride is added, then reaction is carried out after the temperature is raised to reaction temperature, after reaction, the reaction system is cooled to room temperature and stands for layering; and the lower layer of orthophosphorous acid divided after standing is taken as byproduct, the crude product of acyl chloride is adopted to carry out vacuum distillation under the absolute pressure of 20KPa and the distillate at 79 to 81 DEG C is collected, therefore the 3, 3-dimethyl butyraldehyde product is obtained.