38 results about "Dichlorophenylphosphine" patented technology

A synthetic method of a phosphorus-nitrogen intumescent flame retardant relates to a synthetic method of a flame retardant, which comprises the following steps: respectively dissolving raw materials of dichlorophenylphosphine and 4,4'-diaminodiphenylmethane in solvents, introducing inert gas, stirring, slowly and dropwisely adding the 4,4'-diaminodiphenylmethane solution into the dichlorophenylphosphine solution, after dropwise addition, performing reflux reaction for 2-10 hours, cooling, performing suction filtration, washing, and drying to obtain the light yellow powdery phosphorus-nitrogen intumescent flame retardant; the phosphorus-containing monomer and the nitrogen-containing monomer are combined into one compound through condensation polymerization reaction, and thus the flame retardant not only has good flame retardation, but also has the greatest advantage of good compatibility with polymer due to its large molecular weight. The compound can be used as a flame retardant additive for various polymers to improve the flame retardation of the polymers. According to the invention, the production process condition is simple; the product purity and yield are high; and the post-treatment process is simple.

The invention relates to reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and its synthetic method and application and belongs to the field of preparation of a flame retardant. The synthetic method comprises the following steps: using glacial acetic acid as a solvent, adding para amino benzoic acid into glacial acetic acid, slowly dropwise adding dichlorophenylphosphine oxide into an acetic acid solution of para aminobenzoic acid, continuously stirring and reacting at 85-95 DEG C for 4-6 h, and absorbing hydrogen chloride discharged by the reaction by the use of aqueous alkali; and cooling a reaction product after the end of the reaction, carrying out suction filtration, washing and drying to obtain white powdery bis-(p-aminocarboxyphenyl)phenylphosphine oxide. The bis-(p-aminocarboxyphenyl)phenylphosphine oxide flame retardant has advantages of low toxicity, low smoke, innocuousness, high efficiency and the like, is a reactive flame retardant integrating a carbon source, an acid source and a gas source, and is applied in inherent flame retarding of nylon or thermoplastic polyester copolymer.

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.

A preparation method of a phosphorus-nitrogen intumescent flame retardant relates to a preparation method of a flame retardant, and the method comprises the following procedures: respectively dissolving raw materials of dichlorophenylphosphine and p-phenylenediamine in solvents, introducing inert gas, stirring, slowly and dropwisely adding the p-phenylenediamine solution into the dichlorophenylphosphine solution, after dropwise addition, performing reflux reaction for 2-10 hours, cooling, performing suction filtration, washing, and drying to obtain the light purple powdery phosphorus-nitrogen intumescent flame retardant; the compound can be used as a flame retardant additive for various polymers to improve the flame retardation of the polymers. According to the invention, the production process condition is simple; the product purity and yield are high; and the post-treatment process is simple.

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.

The invention discloses a method for preparing a phenyl hypophosphite flame retardant, which comprises the following steps of: adding dichlorophenylphosphine into water at the temperature of between 40 and 100 DEG C within 1 to 6 hours in a reaction kettle with a stirring and refluxing device, and continuously stirring; keeping the temperature to be between 40 and 100 DEG C, and maintaining reaction for 1 to 6 hours; and reducing the temperature to room temperature, regulating the pH of reaction liquid to be between 6 and 8 by using an alkaline material, adding metal salt within 0.5 to 3 hours, maintaining reaction for 1 to 2 hours, filtering, and drying to obtain the phenyl hypophosphite flame retardant, wherein the molar ratio of the water to the dichlorophenylphosphine to the metal salt is 1L:(1-7mol):(1-5mol). Phenyl hypophosphite is prepared from a simple raw material, an intermediate product is not required to be separated, the method is simple, the reaction period is short, conditions are mild, cost is low, and the obtained product has high heat stability.

The invention relates to a curing agent and a preparation method thereof, and concretely relates to a dichlorophenylphosphine oxide and m-xylylenediamine epoxy resin curing agent and a preparation method thereof. Raw materials for preparing the dichlorophenylphosphine oxide and m-xylylenediamine epoxy resin curing agent comprise dichlorophenylphosphine oxide and m-xylylenediamine. The method for preparing the curing agent comprises the following steps; stirring and reacting dichlorophenylphosphine oxide (DCPPO) and m-xylylenediamine (MXDA) under the introduction of an inert gas for a certain period of time, and carrying out filtering, washing and drying treatment on the above obtained product to obtain a white solid. The above compound has good compatibility with epoxy resin, can be cured together with the epoxy resin, has small influences on the mechanical performances of a cured product, can be used as an epoxy resin curing agent, and also effectively improves the flame retardation performance of the epoxy resin. The method has the advantages of simple production conditions, high purity and high yield of the target product, and simple post-treatment process.

The present invention relates to a kind of method of producing phenyl phosphorus dichloride. Its technical scheme is: use chlorinated benzene, elemental phosphorus, and phosphorus trichloride as raw materials, and adopt reaction in a tubular reactor to prepare phenylphosphorus dichloride. The reaction equation is as follows: P 4 + 6C 6 h 5 Cl + 2PCl=6C 6 h 5 PCl. The beneficial effect is: since the main reaction of this method is carried out in a tubular reactor, without using a catalyst, the materials can directly reach the reaction conditions according to the ratio for rapid reaction, shorten the production cycle, and avoid the generation of a large number of by-products; at the same time It solves the potential safety hazards caused by high-temperature and high-pressure reactions in the past by using autoclaves; and there is no waste gas, waste residue, and waste water in the production process. Compared with the current process for preparing phenylphosphorus dichloride, it has greater cost advantages and environmental protection advantages.

The invention belongs to the organic chemical synthesis field and in particular relates to a synthesis method of benzo[b]phospholes. The synthesis method comprises the following steps: taking 1-substitued-2-bromoaryl-acetylene as a raw material, adding a dichlorophenylphosphine synthesis intermediate, and then generating a target compound through trace air catalysis. The synthesis method provided by the invention has the advantages that an oxidant, a catalyst and an additive do not need to be additionally added, and tolerance on different functional groups is good, so that the synthesis method is an environment-friendly synthesis method for a benzo[b]phospholes compound; the yield reaches more than 40%, so that the synthesis method has a good application prospect.

The invention provides a synthesis method for dichlorophenylphosphine oxide, relating to a synthesis method for a catalyst for chemical industry. The synthesis method comprises the following steps of taking benzene and phosphorus trichloride as raw materials and simultaneously adding sodium chloride and alchlor as the catalyst, reacting so as to produce mixed liquor of the dichlorophenylphosphine oxide, benzene and the phosphorus trichloride and solid residue, processing the solid residue with extracting agent and mixing with the mixed liquor, thus obtaining the pure dichlorophenylphosphine oxide through distillation under normal pressure and reduced pressure. The catalyst AlCl3*XNaCl complex can be recycled. Compared with traditional method, the synthesis method has the characteristics that the operation steps are simple, the production time is short, decomplexing agent is added no more in the steps, the synthesis method is easy to operate and control, the production cost is low, and the production steps are environment-friendly, and the like.

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.

The invention relates to a 2-[(2-dimethylaminophenyl)(phenyl)phosphino]-N,N-dimethylaniline copper iodide complex and a synthesis method and the application thereof. The synthesis method comprises thefollowing steps: firstly, enabling 2-bromoaniline and methyl iodide to be in a substitution reaction to produce N,N-dimethyl-2-bromoaniline, and then enabling the N,N-dimethyl-2-bromoaniline and n-butyllithium to be in reaction in a tetrahydrofuran solution to produce aryl lithium; continuing to enable the aryl lithium and dichlorophenylphosphine to be in reaction to produce a ligand 2-[(2-dimethylaminophenyl)(phenyl)phosphino]-N,N-dimethylaniline (ppda), and finally enabling the ppda and cuprous iodide to be in reaction in a dichloromethane solution to obtain a target product. When the synthesis method is used for synthesizing the target product, the yield is high and reaches 72%, and the synthesis method is simple and easy to operate; in addition, the target product has a dual-emissioncharacteristic, can be used as a light-emitting material for assembling an OLED, and has a good application prospect.

The invention discloses a method for synthesizing di-tert-butylphenylphosphonium tetrafluoroborate, and belongs to the field of organic synthesis. The method comprises the following steps: in the anhydrous and anaerobic atmospheres, taking dichlorophenylphosphine as a raw material, after the reduction of diisobutyl aluminium hydride, reacting with tertiary butanol under the catalytic action of boron trifluoride, and then carrying out hydrolysis to generate the di-tert-butylphenylphosphonium tetrafluoroborate. Compared with the prior art, the method is high in yield and simple in aftertreatment, and is more applicable for industrial production.

The invention discloses a method for preparing dicyanomethyl phenylphosphine, which comprises the following steps of: adding tetrahydrofuran and zinc powder into a reactor, adding dropwise the mixed solution of dichlorophenylphosphine, bromoacetonitrile and the tetrahydrofuran, performing reaction at the constant temperature of 20 to 70 DEG C for 0.5 to 3 hours, performing primary distillation under reduced pressure to recover the tetrahydrofuran and the bromoacetonitrile after the reaction is finished, continuing to add dichloromethane and water into the distilled reactor, performing demixing under stirring to obtain an organic layer, and performing secondary distillation under reduced pressure to remove the dichloromethane to obtain the dicyanomethyl phenylphosphine finished product. The dicyanomethyl phenylphosphine product prepared by the method has the purity of over 98 percent; and the production process is simple, the production is easy to control and the method is favorable for large-scale production.

The invention discloses a selenium atom-containing fluorescence probe, and a preparation method and an application thereof, and belongs to the field of functional materials. The structural general formula of above material is represented by formula (I) shown in the description; and in the formula (I), Ar is a carbazolyl or diphenylamino group, and Ph is a phenyl group. The preparation method of the material concretely comprises the following steps: reacting carbazole / diphenylamine with dichlorophenylphosphine / diphenylchlorophosphine to form a derivative containing an N-P structure, and carrying out chemical modification to introduce selenium atoms in order to form the selenium atom-containing fluorescence probe. The method has the advantages of simple synthesis steps, mild conditions, low production cost and high thermal stability. Se=O double bonds are formed through the reaction of the selenium atoms and hypochlorite radicals in order to generate fluorescence change. The selenium atom-containing fluorescence probe has the advantages of high sensitivity and high selectivity.

The invention provides a reactive phosphorus-containing epoxy resin flame-retardant curing agent and a preparation method thereof, and relates to a curing agent and a preparation method thereof. Raw materials for preparation comprise dichlorophenylphosphine oxide and m-xylylenediamine. The preparation method of the flame retardant comprises the following steps: reacting the dichlorophenylphosphine oxide (DCPPO) and the m-xylylenediamine (MXDA) with stirring for some time while inert gas is introduced; and performing filtration, washing, drying and other treatment on the product to obtain a white solid. The compound has favorable compatibility with epoxy resin, can be cured with the epoxy resin into a whole and has less influence on the mechanical properties of a cured product; and the compound can serve as the epoxy resin curing agent, and can effectively improve the flame retardancy of the epoxy resin. The process provided by the invention is simple in production conditions, high in product purity and yield and convenient in a posttreatment process.

The invention relates to a synthesis method of chloroanthraquinone. Firstly, chlorine is introduced into the mixed liquid of benzene phosphorus dichloride and phenyl phosphonyl chloride at the temperature lower than or equal to 30 DEG C to prepare chlorinating reagent 4-chlorophenyl phosphine, then raw material nitroanthraquinone is added to react for 4 to 6 hours at 160 to 180 DEG C, after the reaction is accomplished, cooling is performed and water is added for dilution, and NaOH solution is used for neutralization, and pH is neutralized to 6.5 to 7.5, then ethyl acetate is used for extraction separation, after extract phase is washed and dried, exsolution and concentration are performed, and finally freezing crystallization is separated, and the separated crystal is the chloroanthraquinone. The method has the advantages that the use of heavy metal is avoided, and the method is beneficial to improving the quality of products and protecting the environment.

The invention discloses a preparation method of aluminum phenylphosphinate. The preparation method comprises the following steps: a. preparing 0.1-1mol / L aluminum nitrate or aluminum sulfate solution; b. slowly dropping the aluminum nitrate or aluminum sulfate solution in dichlorophenylphosphine at 0-40 DEG.C; c. after dropping, heating and adjusting the pH value of the solution, reacting for 1-3 hours at 40-100 DEG.C to generate a target product aluminum phenylphosphinate. The method disclosed by the invention is used for preparing aluminum phenylphosphinate by adopting aluminum nitrate or aluminum sulfate solution and dichlorophenylphosphine to directly react under acidic condition in one-step method, the yield of the target product is 87-96%; the obtained aluminum phenylphosphinate is white powder, the color treatment is unnecessary, and the purity is high; the existing process rout is simplified, the reaction time is short, the environment-friendly is realized, the cost is low, and the method is more suitable for the industrial production.

The invention provides an ionic liquid modified silica gel loaded aluminum chloride catalyst for catalytic preparation of dichlorophenylphosphine. The preparation method comprises the following stepsof: a, uniformly mixing and stirring ionic liquid and silica gel, performing heating to 100-150DEG C, keeping the temperature, performing stirring for 1-2h, then conducting cooling to room temperature, and precipitating, filtering and drying the solid to obtain ionic liquid modified silica gel; and b, adding the ionic liquid modified silica gel obtained in the step a into ethanol, adding aluminumchloride under stirring, continuously performing stirring for 1-2h, removing ethanol under reduced pressure, heating the mixture to 120-160DEG C under the protection of nitrogen, and carrying out reaction for 5-10h to obtain yellow powder. The prepared catalyst has stable properties and high reaction activity, a high product yield (90% or above) can be achieved by using a very small amount of a catalyst in the preparation process of dichlorophenylphosphine, post-treatment of the catalyst is simple, the catalyst can be removed from the system only through filtration, and the catalyst can be reutilized after drying.

The invention discloses a phosphor-fluorine flame retardant and a preparation method thereof. The structure of the phosphor-fluorine flame retardant is shown in the description, wherein n is a positive integer of 1 to 50. The flame retardant is a condensed high polymer phosphor-fluorine flame retardant which is synthesized by taking bisphenol AF and dichlorophenylphosphine oxide as raw materials and has a phosphor-fluorine synergistic effect, has a better flame-retardant effect, and has the advantages of good weather ability, as well as lower toxicity and the like compared with a traditional flame retardant; after the phosphor-fluorine flame retardant is added into a high polymer material, a separation-out phenomenon is avoided.

The invention relates to a sulfur, nitrogen and phosphorus heterocyclic compound which has the structural formula as shown in the specification, wherein R1 refers to sulfur and R2 refers to one or hydrogen and methoxyl. The invention further relates to a preparation method and application of the sulfur, nitrogen and phosphorus heterocyclic compound. In the preparation method, sulfur powder is added to reactants, namely triphenyl triamine and dichlorophenylphosphine to react to obtain the sulfur, nitrogen and phosphorus heterocyclic compound. According to the preparation method, the synthesis procedure is short, reaction conditions are mild, operation is facilitated, yield is high, the sulfur, nitrogen and phosphorus heterocyclic compound has good heat stability and chemical stability and can be applied to manufacturing of field effect transistors, solar batteries or light emitting diodes, and the like.

The invention discloses a method for synthesizing di-tert-butylphenylphosphonium tetrafluoroborate, and belongs to the field of organic synthesis. The method comprises the following steps: in the anhydrous and anaerobic atmospheres, taking dichlorophenylphosphine as a raw material, after the reduction of diisobutyl aluminium hydride, reacting with tertiary butanol under the catalytic action of boron trifluoride, and then carrying out hydrolysis to generate the di-tert-butylphenylphosphonium tetrafluoroborate. Compared with the prior art, the method is high in yield and simple in aftertreatment, and is more applicable for industrial production.

The invention discloses a method for preparing a phenyl hypophosphite flame retardant, which comprises the following steps of: adding dichlorophenylphosphine into water at the temperature of between 40 and 100 DEG C within 1 to 6 hours in a reaction kettle with a stirring and refluxing device, and continuously stirring; keeping the temperature to be between 40 and 100 DEG C, and maintaining reaction for 1 to 6 hours; and reducing the temperature to room temperature, regulating the pH of reaction liquid to be between 6 and 8 by using an alkaline material, adding metal salt within 0.5 to 3 hours, maintaining reaction for 1 to 2 hours, filtering, and drying to obtain the phenyl hypophosphite flame retardant, wherein the molar ratio of the water to the dichlorophenylphosphine to the metal salt is 1L:(1-7mol):(1-5mol). Phenyl hypophosphite is prepared from a simple raw material, an intermediate product is not required to be separated, the method is simple, the reaction period is short, conditions are mild, cost is low, and the obtained product has high heat stability.

A preparation method of a polymeric phosphorus-nitrogen flame retardant relates to a preparation method of a flame retardant, and the method comprises the following procedures: respectively dissolving dichlorophenylphosphine and m-xylylenediamine in solvents, introducing inert gas, stirring, slowly and dropwisely adding the m-xylylenediamine solution into the dichlorophenylphosphine solution, after dropwise addition, performing reflux reaction for 2-10 hours, cooling, performing suction filtration, washing, and drying to obtain the white powdery polymeric phosphorus-nitrogen flame retardant; the compound can be used as a flame retardant additive for various polymers to improve the flame retardation of the polymers. According to the invention, the production process condition is simple; the product purity and yield are high; and the post-treatment process is simple.

The invention discloses a method for preparing dicyanomethyl phenylphosphine, which comprises the following steps of: adding tetrahydrofuran and zinc powder into a reactor, adding dropwise the mixed solution of dichlorophenylphosphine, bromoacetonitrile and the tetrahydrofuran, performing reaction at the constant temperature of 20 to 70 DEG C for 0.5 to 3 hours, performing primary distillation under reduced pressure to recover the tetrahydrofuran and the bromoacetonitrile after the reaction is finished, continuing to add dichloromethane and water into the distilled reactor, performing demixing under stirring to obtain an organic layer, and performing secondary distillation under reduced pressure to remove the dichloromethane to obtain the dicyanomethyl phenylphosphine finished product. The dicyanomethyl phenylphosphine product prepared by the method has the purity of over 98 percent; and the production process is simple, the production is easy to control and the method is favorable for large-scale production.

The invention relates to a new epoxy resin curing agent and a preparation method thereof. The new epoxy resin curing agent has a structural formula shown as the figure in the description. The preparation method comprises: in a condition at 105-430 DEG C, reacting dichlorophenylphosphine with diethyl phosphite at a mol ratio of 3:1, raising the temperature to 150-160 DEG C, and performing a reaction for 3-4 h to obtain the new epoxy resin curing agent. The provided new epoxy resin curing agent is quite stable at the room temperature and long in storage period, and is used to graft phosphorus-series molecules to an epoxy resin structure during curing of an epoxy resin system. The new epoxy resin curing agent is excellent in flame retardance and thermal resistance, is quite stable, and can reduce the curing temperature.

A preparation method of a polymeric phosphorus-nitrogen flame retardant relates to a preparation method of a flame retardant, and the method comprises the following procedures: respectively dissolving dichlorophenylphosphine and m-xylylenediamine in solvents, introducing inert gas, stirring, slowly and dropwisely adding the m-xylylenediamine solution into the dichlorophenylphosphine solution, after dropwise addition, performing reflux reaction for 2-10 hours, cooling, performing suction filtration, washing, and drying to obtain the white powdery polymeric phosphorus-nitrogen flame retardant; the compound can be used as a flame retardant additive for various polymers to improve the flame retardation of the polymers. According to the invention, the production process condition is simple; the product purity and yield are high; and the post-treatment process is simple.

The invention discloses a preparation method of 3, 7-dicarbazolyl-5-phenyl benzoxphosphine heteroindole, and belongs to the technical field of organic synthesis. The method comprises the following steps: carrying out a coupling reaction on 1, 4-difluoro-2-nitrobenzene under the catalysis of copper to obtain 4, 4 '-difluoro-2, 2'-dinitro-biphenyl, carrying out stannous chloride reduction and amido diazonium salt process conversion to obtain 4, 4 '-difluoro-2, 2'-diiodo-biphenyl, and carrying out 4, 4 '-difluoro-2, 2'-diiodo-biphenyl. The preparation method comprises the following steps: carrying out lithium-iodine exchange on 2, 2 '-diiodo-biphenyl, carrying out nucleophilic substitution reaction on the 2, 2'-diiodo-biphenyl and dichlorophenylphosphine to generate phenylphosphine heterobenzoindole, oxidizing the phenylphosphine heterobenzoindole to form phenylphosphine oxide heterobenzoindole, and carrying out substitution reaction on carbazole and aryl fluoride to synthesize the phosphine oxide type organic small molecular luminescent material with fluorescence activity. The 3, 7-dicarbazolyl-5-phenyl benzoxphosphine heteroindole synthesized by the method not only can be used as a photocatalyst in the field of organic synthesis, but also can be used as an organic photoelectric material.

The invention discloses a preparation method of a symmetric phosphine oxide type TADF organic photoelectric material, and belongs to the field of organic functional materials. 2, 2 '-dinitro-biphenyl is subjected to stannous chloride reduction, amido acylation, electricity-rich aromatic ring bromination reaction and acid deacylation of a protecting group to form free amido, the amido is converted into 5, 5'-dibromo-2, 2 '-diiodo-biphenyl through a diazonium salt process, then the 5, 5'-dibromo-2, 2 '-diiodo-biphenyl is converted into 5, 5'-dibromo-2, 2 '-diiodo-biphenyl, and the 5, 5'-dibromo-2, 2 '-diiodo-biphenyl is converted into 5, 5 The preparation method comprises the following steps: carrying out lithium-iodine exchange on 2, 2 '-diiodo-biphenyl, carrying out nucleophilic substitution reaction on the 2, 2'-diiodo-biphenyl and dichlorophenylphosphine to generate phenylphosphine heterobenzoindole, oxidizing the phenylphosphine heterobenzoindole to form phenylphosphine oxide heterobenzoindole, and carrying out coupling reaction on brominated aromatic hydrocarbon and heteroaromatic hydrocarbon under the catalysis of copper to synthesize the small organic molecule luminescent material with fluorescent reactive oxygen species. The 2, 8-diphenothiazinyl-5-phenyl benzoxphosphine heteroindole synthesized by the method has the potential of becoming an organic micromolecule electroluminescent material and being used as a photosensitizer for organic photoreaction, and fits the development trend of multifunctional application of organic micromolecule materials.