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800 results about "Phosphoryl chloride" patented technology

Phosphoryl chloride (commonly called phosphorus oxychloride) is a colourless liquid with the formula POCl₃. It hydrolyses in moist air releasing phosphoric acid and fumes of hydrogen chloride. It is manufactured industrially on a large scale from phosphorus trichloride and oxygen or phosphorus pentoxide. It is mainly used to make phosphate esters such as tricresyl phosphate.

Poly-phosphate flame retardant containing DOPO side-chain structure and preparation method thereof

The invention discloses a poly-phosphate flame retardant containing a DOPO side-chain structure and a preparation method thereof, belonging to the technical field of polymeric organic phosphorus flame retardant structures and the preparation method thereof. The flame retardant is characterized by comprising the following repeating unit structure: wherein n=5-50. The preparation method of the poly-phosphate flame retardant comprises the following steps of: reacting an intermediate I containing the DOPO structure with phosphorus oxychloride to obtain an intermediate II containing phosphorus oxychloride, and fusing and polymerizing the intermediate II and a bisphenol compound to obtain the poly-phosphate flame retardant containing the DOPO side-chain structure. The preparation method is simple, and through adjusting Ar categories and ratios, the phosphorus content can be controlled at 11.5-15.5% and the sulfur content can be controlled at 0-5.9%. The flame retardant has the characteristics of favorable thermal stability, high decomposition temperature, favorable char-forming property, and the like, and can be used for flame retardance modification of materials, such as polyester, polyamide, polycarbonate and blends thereof, and the like, with higher processing temperature.
Owner:DALIAN UNIV OF TECH

Intumescent flame retardant functional silicate and preparation method thereof

The invention discloses an intumescent flame retardant functional silicate and a preparation method thereof. According to the invention, the preparation method comprises the following two methods: one method comprises the steps of first preparing silane coupling agent organic functional silicate, and then preparing the intumescent flame retardant functional silicate on the basis of the former step; and the second method comprises the steps of first preparing a modified silane coupling agent containing phosphorus and nitrogen flame retardant elements, and then modifying inorganic silicate by using the modified silane coupling agent on the basis of the former step. According to the invention, the intumescent flame retardant functional silicate comprises an organic part B and an inorganic part A, wherein the organic part B is grafted to the inorganic part A in such a way that a silanol group formed by after a silane coupling agent containing amino has dehydration reaction with hydroxyls on the surface and between layers of the inorganic part A; and the organic part B is formed in such a way that a phosphoryl chloride compound has elimination reaction with an amino silane coupling agent. The intumescent flame retardant functional silicate disclosed by the invention is integrated with reinforcing, flame retardant and smoke suppressing functions.
Owner:SOUTH CHINA UNIV OF TECH +1

Method for preparing combustion inhibitor bisphenol A bis(diphenyl phosphate)

The invention relates to a preparation method for flame retardant bisphenol A bi(diphenyl phosphate). The preparation method comprises the following steps: taking phosphorus oxychloride, bisphenol A and phenol as raw materials, adopting anhydrous zinc chloride or anhydrous aluminum chloride as a main catalyst, and adopting anhydrous calcium chloride or calcium phosphate as a promoter; adding the phosphorus oxychloride, the main catalyst and the promoter into a reactor for intensive stirring, when the materials are heated up to 73 to 78 DEG C, continuously adding bisphenol A, after the addition of bisphenol A is completed within 2.5 to 3 hours, heating up to and maintaining the temperature of 110 to 115 DEG C, and continuing the reaction for 1.5 to 2 hours; leaking out excessive phosphorus oxychloride under the normal and reduced pressure; and cooling down the intermediate product to 100 DEG C, continuous dropping phenol into the intermediate product, heating up to 140 DEG C 2 hours later, carrying out the reaction for 3 to 4 hours, monitoring the content of phenol through the liquid chromatography, and complementing phenol till the phenol content in the crude product is less than 0.5 percent. The yield reaches 98 percent; the content of triphenyl phosphate is less than 1.5 percent; and the acid number is 0.03mgKOH/g.
Owner:BC P INC CHINA NAT PETROLEUM CORP +1

Bromine-containing pentaerythritol phosphoester retardant and preparation method thereof

InactiveCN101921407AToxicBring health risksGroup 5/15 element organic compoundsBulk chemical productionTribromoneopentyl alcoholQuaternary ammonium cation
The invention relates to a bromine-containing pentaerythritol phosphoester fire retardant and a preparation method thereof. The bromine-containing pentaerythritol phosphoester fire retardant is pentaerythritol double-spiro phosphoryl double-tribromo neopentyl alcohol ester. The preparation method of the novel bromine-containing pentaerythritol phosphoester comprises the following steps of: 1, reacting pentaerythritol with phosphorus oxychloride to generate an intermediate pentaerythritol double-spiro double-phosphorus oxychloride; and 2, reacting the pentaerythritol double-spiro phosphorus oxychloride with tribromo neopentyl alcohol to generate the pentaerythritol double-spiro phosphoryl double-tribromo neopentyl alcohol ester, wherein in the reaction, quaternary ammonium salt cation ionic liquid serves as a solvent and a catalyst. The invention discloses a new synthesis method of the bromine-containing pentaerythritol phosphoester fire retardant. The ionic liquid serves as the solvent, so the synthesis yield is improved; and a phosphorus-bromine synergistic flame retardant technique is adopted in the design of a molecular structure, so the anti-flaming efficiency of the flame retardant for high molecular materials is improved.
Owner:DONGHUA UNIV

Polymeric phosphorus-containing flame retardant with DOPO as lateral group and preparation method thereof

The invention discloses a polymeric phosphorus-containing flame retardant with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide as a lateral group and a preparation method thereof. The preparation method is characterized by comprising the following steps: placing aromatic dihydric phenol and pentaerythritol diphosphate diphosphoryl chloride (or bromine) which are modified by the 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in an anhydrous acetonitrile solvent based on reaction mol ratio, heating the obtained mixture to 80 DEG C in an inert atmosphere, agitating and reacting until no halogen hydride is released, cooling the obtained mixture to the room temperature, and depressurizing the mixture to remove the solvent. The obtained product has high phosphorus content, very good expansibility and char formation, and good flame retardation effect. When flame retardation is performed on epoxy resin, the limiting oxygen index of the obtained product is greatly improved and the vertical burning scale reaches V-0 level; and the polymeric phosphorus-containing flame retardant has the advantage of overcoming the disadvantages of low thermal decomposition temperature, poor compatibility with polymer matrix and easy migration in the existing micromolecular phosphorus flame retardants. The preparation method has the advantages of being simple and feasible, using no catalyst and simple post-treatment process.
Owner:UNIV OF SCI & TECH OF CHINA

Anti-mud type phosphate modified polycarboxylate superplasticizer and preparation method thereof

The invention discloses an anti-mud type phosphate modified polycarboxylate superplasticizer and a preparation method thereof. The method specifically comprises the following steps: performing oxidation-reduction free radical polymerization reaction on unsaturated carboxylic acid micro-monomer and unsaturated polyether macro-monomer in the presence of an initiator, a reducing agent and a chain transfer agent, thereby acquiring a carboxyl-containing polycarboxylate superplasticizer prepolymer; with diphenyl phosphoryl chloride, modifying the carboxyl-containing polycarboxylate superplasticizer prepolymer partially, thereby acquiring a phosphate based copolymerization product; after completing the reaction, regulating the pH value to 6-7 and adding water, thereby acquiring the polycarboxylate superplasticizer. According to the invention, the side chain of the polycarboxylate superplasticizer is modified into a phosphate group containing two benzene rings and the phosphoric acid functional group enters into the carminate element of the polycarboxylate superplasticizer, so that the sulfate radical resisting capacity and anti-mud capacity of the polycarboxylate superplasticizer are promoted. The introduction of the benzene rings can greatly increase the physical size of the side chain of the polycarboxylate superplasticizer and the polycarboxylate superplasticizer is unlikely to be inserted into the layered structure of clay, so that the anti-mud effect can be achieved and the intrinsic function of the polycarboxylate superplasticizer is not influenced.
Owner:JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD

Phosphorus-nitrogen-silicon intumescent flame retardant containing triazine ring and cage structure and synthesis method of intumescent flame retardant

The invention relates to a phosphorus-nitrogen-silicon intumescent flame retardant containing a triazine ring and a cage structure and a synthesis method of the intumescent flame retardant. The synthesis method comprises the steps as follows: a solvent is added to a container, phosphorus oxychloride is added and stirred to be dispersed, PEPA (1-oxy phospha-4-(hydroxymethyl)-2,6,7-trioxabicyclo[2.2.2]octane) and an acid-binding agent are dropwise added step by step, and a PEPA-containing unitary substituent is obtained; substances with diamine or dihydric alcohol are added to the other container and mixed with the solvent and the acid-binding agent, the PEPA-containing unitary substituent is slowly dropwise added, and a phosphorous-containing diamine intermediate is obtained after separation; the solvent is added to a container provided with a reflux condenser and the like, cyanuric chloride is added and stirred to be dispersed, an amino silane coupling agent and the acid-binding agent are dropwise added step by step, and a silicon-containing unitary substituent is obtained; the mixture of the phosphorous-containing diamine intermediate and the acid-binding agent is slowly dropwise added, cooling, washing and drying are performed, and a powdery solid, namely, the phosphorus-nitrogen-silicon intumescent flame retardant containing the triazine ring and the cage structure, is obtained. The phosphorus-nitrogen-silicon intumescent flame retardant has the advantages that the flame retardant has certain polymerization degree, high molecular weight, higher charcoal forming amount and better thermal stability, the proportion of acid sources, carbon sources and gas sources in molecular structures is relatively proper and the like.
Owner:SHUNDE POLYTECHNIC

Reactive phosphorus triazine flame retardant for dyeing, and preparation method and application thereof

The invention discloses reactive phosphorus triazine flame retardant for dyeing, and a preparation method and application thereof, which belong to the technical field of flame retardants and relate to flame retardant for cotton. A molecular structure of the reactive phosphorus triazine flame retardant for dyeing is OPO3OCLO3OO3PO. The preparation method includes: mixing pentaerythritol with dioxane under protection of inert gases, dropwise adding phosphorus oxychloride at 80 DEG C for two hours, adding two to three drops of triethylamine, allowing for reaction for 4-10 hours, cooling, filtering, vacuum-drying to obtain PEPA after rinsing; and mixing cyanuric chloride with reaction solvent, adjusting the temperature to 10-20DEG C, initially dropwise adding the PEPA and acid-binding agent, allowing for continuous reaction for 6 hours, dropwise adding again the PEPA and the acid-binding agent, allowing for reaction for 6 hours, adding precipitant for precipitation after cooling, filtering, rinsing, and drying to obtain the fished product. The preparation method is simple, the prepared flame retardant has a carbon source, an acid source and a gas source integrated and is higher in thermal stability and better in carbon forming performance, and the PEPA and the triazine structure are complemented while both being given to full play to the advantages.
Owner:ZHONGBEI UNIV

Hexaphenyl phosphate ester melamine salt fire retardant and method for preparing same

InactiveCN102190814ALess physical and chemical propertiesLittle impact on physical and chemical propertiesGroup 5/15 element organic compoundsFiltrationPhosphate
The invention relates to a hexaphenyl phosphate ester melamine salt fire retardant and a method for preparing the same. Based on the molar ratio, the reaction ratio of diphenyl phosphorus oxychloride to melamine is (3.0-3.6):1.0, and the diphenyl phosphorus oxychloride comprises components of phenol, phosphorus oxychloride and anhydrous magnesium chloride in a ratio of (2.0-2.5):(1.0-1.4):(0.01-0.03). The preparation method comprises the following steps of: adding phosphorus oxychloride, anhydrous magnesium chloride and phenol respectively, performing continuous stirring reflux during reaction, and performing vacuum distillation after the reaction to obtain diphenyl phosphorus oxychloride; and adding the diphenyl phosphorus oxychloride and melamine, performing stirring reflux, and after the reaction, cooling the obtained product in an ice bath, and performing suction filtration, water washing and drying on the product to obtain the hexaphenyl phosphate ester melamine salt. The hexaphenyl phosphate ester melamine salt fire retardant prepared by the method has the advantages of low toxicity, less smoke, harmlessness, high efficiency, environmental friendliness and the like and leads the development trend of intumescent fire retardants in the future.
Owner:WUHAN INSTITUTE OF TECHNOLOGY

Method for preparing rivastigmine hydrogen tartrate and application thereof

The invention relates to a method for preparing rivastigmine hydrogen and tartrate thereof, which comprises the following steps: taking metamethoxyacetophenone as an initial raw material, and obtaining 1-(3-methoxyphenyl)ethanol by the reduction; then performing the chlorination to obtain 1-(chloroethyl)-3-methoxyphenyl; then reacting the1-(chloroethyl)-3-methoxyphenyl with dimethylamine hydrochloride to obtain 1-(3-methoxyphenyl)-N, N-dimethylethanamine; demethylating the reaction product to obtain 3-[1-(dimethylamino)ethyl]phenol; then performing salt formation resolution with (s)-(+)-camphor-10-sulfonic acid, recrystallizing, and dissociating to obtain (s)-3-[1-(dimethylamino)ethyl]phenol; then taking ethylamine as a raw material to react with ethyl formate to obtain formylethylamine; then reacting the formylethylamine with phosphorus oxychloride to obtain an imine intermediate; reducing the imine intermediate by sodium borohydride to obtain ethyl methyl amine; then reacting the ethyl methyl amine with triphosgene to obtain N-methyl-N-ethylformyl chloride; and finally using (s)-3-[1-dimethylamino)ethyl]phenol to condensate with the N-methyl-N-ethylformyl chloride, and then performing salt formation with levotartaric acid to obtain the rivastigmine hydrogen tartrate. The method has the advantages of easily-obtained raw materials, simple and convenient operation, low cost, high yield and small pollution, and is a brandnew synthesis route at present.
Owner:SHENYANG PHARMA UNIVERSITY

Symmetrical double-rhodamine B fluorescent probe for detecting mercury ion and preparation method of fluorescent probe

InactiveCN103254893AEnables visualization of fluorescence imagingFluorescent signal enhancementOrganic chemistryFluorescence/phosphorescenceFluorescenceAcyl group
The invention relates to a symmetrical double-rhodamine B fluorescent probe for detecting a mercury ion and a preparation method of the fluorescent probe. The structural formula of the symmetrical double-rhodamine B fluorescent probe RBSRB (rhodamine B-symmetrical-rhodamine B) is as shown in the specification. The preparation method comprises the following steps: adding rhodamine B and phosphorus oxychloride into a solvent for reflux reaction for 20-24h at 85-90 DEG C, obtaining rhodamine B acyl chloride, dissolving rhodamine B acyl chloride and 2-bromine ethylamine in the solvent, stirring for reaction for one night at room temperature, purifying to obtain rhodamine B acyl-2-bromine ethylamine, adding rhodamine B acyl-2-bromine ethylamine and sodium sulfide into the solvent for reflux reaction for 5-8h at 80-85 DEG C, and purifying to obtain the fluorescent probe. The fluorescent probe is symmetrical double-rhodamine B amide connected by a sulphur atom; only alcohol under 1% is introduced as a cosolvent during an experiment; the fluorescent probe is high in selectivity, and has high selectivity to the mercury ion; other common ions do not interfere with the fluorescent probe obviously; and the fluorescent probe has an application prospect in bioluminescence imaging.
Owner:DONGHUA UNIV

Reactive epoxy resin flame-retardant curing agent containing phosphorus and nitrogen and preparation method thereof

The invention relates to a chemical synthesis agent and a preparation method thereof and provides a reactive epoxy resin flame-retardant curing agent containing phosphorus and nitrogen and a preparation method thereof. Raw materials for preparation of the curing agent comprise pentaerythritol, phosphorus oxychloride and 4,4-diamino diphenyl sulfone (DDS). The preparation method for the curing agent comprises the following two steps: step 1, reacting pentaerythritol (PER) with phosphorus oxychloride (POCl3) under certain conditions so as to produce a phosphorus-containing intermediate, i.e., pentaerythritol bisphosphorate diphosphoryl choloride (SPDPC); and step 2, subjecting SPDPC and DDS to a stirring reaction for a certain period of time under the condition of introduction of inert gas and subjecting a product to filtration, washing, drying and the like so as to obtain a white powder which is a phosphorus-nitrogen intumescent flame retardant. The reactive epoxy resin flame-retardant curing agent has high heat stability, expansibility and char yield and can be used as a flame retardation additive to a plurality of polymer materials so as to improve the flame retardant property of the polymer materials. The preparation method provided by the invention has the advantages of simple production conditions, high product purity, high yield and simple and convenient post treatment.
Owner:SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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