36 results about "Phosphonous Acids" patented technology

The invention discloses an alpha-hydroxy unsaturated alkylphosphonic acid compound as well as a preparation method and application of the alpha-hydroxy unsaturated alkylphosphonic acid compound. The alpha-hydroxy unsaturated alkylphosphonic acid compound has the structural formula I as shown in the specification. The preparation method comprises the steps: subjecting 2-ethyl-2-hexenal and hypophosphorous acid or hypophosphite to addition reaction in the existence of an acid catalyst to generate 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphorous acid; subjecting 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphorous acid and an oxidizing agent to reaction to generate 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphonic acid. 30-600g / t of 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphonic acid is used as a flotation collector for bauxite, ilmenite, rutile, scheelite, wolframite, rare earth ores, tin ores, fluorite ores or lithium ores, and the pH value of a flotation solution is controlled at 4-12, so that a target ore and a gangue mineral can be effectively separated.

The polyamide resin of the present invention is produced by polycondensation of a diamine component comprising 70 mol % or more of m-xylylenediamine and a dicarboxylic acid component comprising 70 mol % or more of a C4-C20 α, ω-straight-chain aliphatic dicarboxylic acid in the presence of at least one phosphorus compound selected from the group consisting of phosphinic acid compounds and phosphonous acid compounds and in the presence of an alkali metal compound of a weak acid. The weak acid has a dissociation constant lower than a first dissociation constant of a dicarboxylic acid mainly constituting the polyamide resin. The polyamide resin satisfies the following requirements (A), (B) and (C):14000≦a≦40000  (A)b≦1.000  (B)0.9930≦b−1.1a2×10−11+3.2a×10−7≦0.9980  (C)wherein a and b are as defined in the disclosure.

N, N-bis(2-hydroxyethyl) aminomethylphosphonic diethylester is concerned with preparation of aminomethylphosphonic diester. It includes: (1) reaction of formaldehyde water solution with diethanol; (2) decompression distilling to produce 3 - (2 -hydroxyethyl) - 1,3, - oxaazapentane; (3) adding anhydrous solid acid catalysts and phosphonous acid diester; (4) filtrating and recovering the catalysts to get yellow transparency products with yields of above 98% and 94%-94% contents of N, N-bis(2-hydroxyethyl) aminomethylphosphonic diethylester. It is prepared simply, and highly yields with more effective content. The product is reactive fire-retardant for environmental protection, capably used in plastics, especially in foamed polyamine ester.

The invention discloses a synthetic method for alkyl group phosphorous acid diester compounds or alkyl group phosphinic acid ester compounds. According to the synthetic method, alcohols which are cheap, easy to get, wide in source, stable and low in toxicity serve as alkylating reagents, iodine salt which is cheap and easy to get serves as catalysts, no solvent is needed, and the alkyl group phosphorous acid diester compounds can be selectively directly obtained after a reaction. The reaction method is simple, the condition is mild, no organic solvent is needed and operation is simple. According to the method, the requirements for reaction conditions are low, various types of alcohols such as a benzyl group type, an allyl type and a fat type can be utilized as the alkylate reagents to implement the synthesis of different types of substituted alkyl group phosphorous acid diester, and the method can be further expanded to the synthesis of the alkyl group phosphinic acid ester compounds through the reaction between the substituted phosphonous acid diester and the alcohols.

A methylene phosphocarboxylic acid as water quality stabilizer is prepared from carboxy-contained amine, PCl3 (or phosphonous acid and concentrated hydrochloric acid) and water through heating and adding solution of formaldehyde. It has high output rate.

A polycarbonate resin composition which contains: 100 parts by mass of a resin component that is composed of (A) 60-95% by mass of an aromatic polycarbonate resin, (B) 2-30% by mass of a polyolefin resin and / or a polyolefin elastomer, each of which contains an epoxy group or a glycidyl group and (C) 1-38% by mass of a polyolefin resin other than the component (B); and (D) a phosphorus-containing compound. In this polycarbonate resin composition, the component (D) is composed of component (D1) and / or component (D2) described below. (D1) 0.01-0.5 part by mass of at least one compound that is selected from the group consisting of phosphite compounds and phosphate compounds, wherein at least one alkoxy group is bonded to a phosphorus atom (provided that in cases where the compound has an aryloxy group bonded to a phosphorus atom, hydrogen atoms are at all the ortho positions of the aryloxy group) (D2) 0.001-0.1 part by mass of at least one acid that is selected from the group consisting of phosphoric acid, phosphorous acid, phosphonic acid and phosphonous acid

The invention relates to a synthesis and purification method of methyl phosphinate compounds. The method concretely comprises the following steps: adding brine to a solution containing a methyldialkyl phosphinate and magnesium chloride mixture in an inert solvent at a low temperature, and separating to obtain methylalkyl phosphinate or methyldialkyl phosphinate. The method solves the post-treatment and purification difficulties of a Grignard reagent method, and has the advantages of industrial production, effective reduction of the generation of methyl phosphonous acid, mild process conditions, and excellent reaction yield and product quality.

An improved regiospecific synthesis of organic phosphonous acids, comprising of hydrophosphorylation of an olefin with hydrophosphorous acid in the presence of an inorganic persulfate, which acts as a source of free radicals at a pH ranging from 4.5 to 7.0, in which the orientation of addition is anti-Markonikoff. The process enables production of organic phosphonous acids at lower temperature and atmospheric pressure under milder pH conditions for better regioselectivity in hydrophosphorylation and obtain the phosphonous acid with good yield and purity following simple isolation procedure. Phosphonous acids obtained by the process are commercially valuable as effective detergents and wetting agents, lubricants and lubricant additives, plasticizers for plastics and resins, corrosion inhibitors, chemicals including insecticides and pesticides, cobalt extractants and as key intermediates for preparation of commercially important angiotensin converting enzyme (ACE) inhibitors.

A two-phase system is composed of polyethylene glycol (PEG), phosphine ligand containing PEG chain and non-polar organic solvent. It features that when the reaction is taking place at high temp, all reactants are mixed to become one phase, and when the reaction is finished, the PEG phase is automatically separated from the resultant.

The invention discloses a method for preparing (Z)-2-(tert-Methoxycarbonyl Methoxyimino)-2-(2-Aminothiazol-4-yl)Acetic Acid active ester, which includes that: in an organic solvent system and at -10 DEG C to 50 DEG C, 1.0mol of (Z)-2-(tert-Methoxycarbonyl Methoxyimino)-2-(2-Aminothiazol-4-yl)Acetic Acid (MICA Acid) and 1.0mol to 1.4mol of rubber accelerator DM (MBTS) are mixed; then 1.0mol to 1.3mol of organic amine and 0mol to 0.1mol of pyridinium derivative as a catalyst are added in; 1.1mol to 1.5 mol of phosphonic acid triethyl ester is dripped in within 1h to 8h at -10 DEG C to 50 DEG C;and the temperature is preserved for 1h to 6h, then the (Z)-2-(tert-Methoxycarbonyl Methoxyimino)-2-(2-Aminothiazol-4-yl)Acetic Acid active ester is obtained. The method adopts cheaper raw materials and a phase transfer catalysis technique; thus shortening reaction period, reducing production cost and having super high industrial application value.

The present invention relates to phosphonous acid monoalkyl ester compound synthesis method. The method is ::adding salicylal and organic amine in 95% ethanol, heating and making it reflux for 3-4 hours, adding diethyl phosphite ethanol solution for continuous reflux for 36-70 hours, filtering white solid, washing it with ethanol, mol ratio of salicylic acid, aromatic amine and diethyl phosphite being 1:1:1. The structure of phosphonous acid monoalkyl ester compound is indicated as formula (I). The inventive method is simple and yield is high.

The invention discloses a method for preparing clodronate disodium. The method comprises the following steps of: performing methylenation, chlorination, acid hydrolysis and salification on triethyl phosphate and dibromomethane which serve as raw materials to obtain the clodronate disodium. According to the method, the clodronate disodium is produced by taking triethyl phosphite is used as the raw materials, so that the cost of the raw materials is reduced substantially, the method is easy to operate, and industrial production is easy to implement; derosination reaction of an intermediate II is performed by an acid hydrolysis method, the reaction condition is mild, the reaction time is shortened to 1 to 3 hours from 10 hours, and the production efficiency is improved greatly; the purity of the product and the clarity of a solution are high, so the clodronate disodium can be used for preparing high-quality clodronate disodium injections and clodronate disodium capsules, and the risk of clinical medication is reduced; and hydrochloric acid and other organic solvents which are used in the process can be recycled, so the method is environment-friendly.

[Object]It is intended to obtain a polyamide resin composition that is excellent in heat aging resistance and exhibits suppressed metal corrosive properties and copper-depositing properties.[Means of solving the problems]A polyamide resin composition comprising a polyamide resin (A), a copper compound (B), a bromide of an alkali metal and / or a bromide of an alkaline earth metal (C), and at least one phosphorus compound (D) selected from the group consisting of phosphite compounds represented by the following general formula (1), and phosphonite compounds represented by the following general formula (2):phosphite compound: (RO)mP(OH)3-m  (1) andphosphonite compound: (RO)nO(OH)2-n(R)  (2)wherein m represents 1, 2, or 3; n represents 1 or 2; R represents an alkyl group, a phenyl group, or a partially substituted alkyl group or phenyl group; and if each of m and n is 2 or more, a plurality of (RO) groups in the general formulas (1) and (2) are the same or different from each other.

The invention discloses a method for preparing optically-active alpha-amino phosphonate derivatives by chiral spiro phosphate catalysis. Chiral spiro phosphate serves as a catalyst, imine and dialkyl phosphate are stirred in an organic solvent at room temperature, and high-purity optically-active alpha-amino phosphonate derivatives are prepared by a simple post-treatment purification process. The method is mild in reaction condition, simple in process and convenient in operation. The catalyst is high in stability and can be reused. The prepared optically-active alpha-amino phosphonate derivatives are high in potential biological activity and can be used as organic synthesis intermediates.

The invention relates to a synthesis method and a synthesis device of diethyl methylphosphite. The synthesis method comprises the following steps: (1) mixing methyl phosphine dichloride, absolute ethyl alcohol and a solvent to carry out a synthesis reaction; (2) carrying out reduced pressure deacidification treatment on the reaction solution obtained in the step (1); and (3) separating and purifying the deacidified reaction solution obtained in the step (2) to obtain diethyl methylphosphite. According to the synthesis method, an acid-binding agent is not needed, hydrogen chloride gas generatedby the synthesis reaction can be discharged through reduced-pressure deacidification treatment, the generation of solid waste residues containing acid-binding agent hydrochloride is avoided, the separation and treatment of the solid waste residues are reduced, and the dosage of ethanol is reduced by adding a solvent, so that the ethanol does not need to play a role as a solvent, the energy consumption is reduced, the resources are saved, the process is high in yield, simple to operate and environment-friendly, and the atom economy is good.

An ionic liquid composition having the following generic structural formula:wherein R1, R2, R3, and R4 are equivalent and selected from hydrocarbon groups containing at least three carbon atoms, and X− is a phosphorus-containing anion, particularly an organophosphate, organophosphonate, or organophosphinate anion, or a thio-substituted analog thereof containing hydrocarbon groups with at least three carbon atoms. Also described are lubricant compositions comprising the above ionic liquid and a base oil, wherein the ionic liquid is dissolved in the base oil. Further described are methods for applying the ionic liquid or lubricant composition onto a mechanical device for which lubrication is beneficial, with resulting improvement in friction reduction, wear rate, and / or corrosion inhibition.

The invention discloses a phosphonate-base polymer with high adaptability and slump retaining properties, and a preparation method and application thereof. The phosphonate-base polymer has the following structural characteristics: the side chain is an ether type chain segment; and the polymer has two stages of adsorption groups, the primary adsorption group is a phosphonate or phosphite functional group, the secondary adsorption group is carboxyl, and the two functional groups are connected by an ester bond or amido bond. The weight average molecular weight of the phosphonate-base polymer with high adaptability and slump retaining properties is 10000-50000. The phosphonate-base polymer has a novel molecular structure, and thus, has the advantages of low doping amount, high water reducing rate, excellent slump retaining properties, and high sulfate and clay interference resistance. The preparation technique can implement industrialization, and thus, has broad market application space.

The invention relates to the technical field of compound purification, and particularly provides a purification method of dialkyl methylphosphite. The purification method comprises the following steps: adding a weak polar solvent into a reaction solution containing dialkyl methylphosphite, magnesium chloride and an ether solvent, conducting cooling to -10 DEG C to 40 DEG C, adding a nitrogen-containing organic alkali compound, carrying out a heat preservation reaction, and conducting filtering to obtain magnesium chloride and a filtrate; and rectifying the filtrate to obtain a dialkyl methylphosphite product. According to the purification method provided by the invention, the purity and the yield of the dialkyl methylphosphite are improved, the obtained magnesium chloride does not containcrystal water, the nitrogen content in the magnesium chloride is 0.01-0.5%, and the purity of the anhydrous magnesium chloride can reach 97% or above; and the purity of the obtained dialkyl methylphosphite product can reach 97% or above, and the yield can reach 85% or above. The method has the advantages of simple process, no need of special equipment, mild reaction conditions and no need of high-temperature distillation or low-temperature brine treatment process, and is suitable for large-scale industrial production.

An ionic liquid composition having the following generic structural formula:wherein Z is N or P, and R1, R2, R3, and R4 are independently selected from hydrogen atom and hydrocarbon groups having one to four carbon atoms with optional interconnection to form a cyclic group that includes Z, and wherein R1, R2, R3, and R4 are all hydrocarbon groups when Z is P, and X− is a phosphorus-containing or carboxylate anion, particularly an organophosphate, organophosphonate, or organophosphinate anion, or a thio-substituted analog thereof containing hydrocarbon groups with at least three carbon atoms. Also described are lubricant compositions comprising the above ionic liquid and a base lubricant, wherein the ionic liquid is dissolved in the base lubricant. Further described are methods for applying the ionic liquid or lubricant composition onto a mechanical device for which lubrication is beneficial, with resulting improvement in friction reduction, wear rate, and / or corrosion inhibition.

The invention discloses an alpha-hydroxy unsaturated alkylphosphonic acid compound as well as a preparation method and application of the alpha-hydroxy unsaturated alkylphosphonic acid compound. The alpha-hydroxy unsaturated alkylphosphonic acid compound has the structural formula I as shown in the specification. The preparation method comprises the steps: subjecting 2-ethyl-2-hexenal and hypophosphorous acid or hypophosphite to addition reaction in the existence of an acid catalyst to generate 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphorous acid; subjecting 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphorous acid and an oxidizing agent to reaction to generate 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphonic acid. 30-600g / t of 1-hydroxyl-2-ethyl-2-hexenyl-1-phosphonic acid is used as a flotation collector for bauxite, ilmenite, rutile, scheelite, wolframite, rare earth ores, tin ores, fluorite ores or lithium ores, and the pH value of a flotation solution is controlled at 4-12, so that a target ore and a gangue mineral can be effectively separated.

The invention discloses a preparation method of diethyl methylphosphonite, aiming to solve the problem that in the existing method, when ammonia gas is used as the acid-binding agent, the pH value of the reaction solution needs to be controlled between 7.0-8.5, accurately It is very difficult to control the pH value, and when the pH value is lower than that, a large amount of ethyl methylphosphinate by-products will be generated, and the use of organic amines as acid-binding agents has high toxicity, high price, and cumbersome recovery process. The problem of low recovery rates. The present invention uses methyl phosphine dichloride, ethanol and calcium oxide as main raw materials to prepare diethyl methyl phosphinate, which is a lower-cost diethyl methyl phosphonite suitable for industrial production. Methods of Esters Preparation. In the preparation of diethyl methylphosphonite, the present invention uses cheap calcium oxide instead of ammonia or organic amine as the acid-binding agent for the first time, which effectively reduces the production cost, and the calcium oxide is non-toxic, environmentally friendly, and has relatively Good economic value and social value.

The invention relates to the technical field of mineral processing, and specifically discloses a flotation method for copper oxide ore. The flotation method of copper oxide ore is to mix the original ore of copper oxide ore with inhibitor, and then grind the ore to obtain a floatable pulp; and 2 times of scavenging, and then 4 times of beneficiation, the ore in each operation returns to the previous operation in sequence, and finally flotation to obtain copper oxide concentrate products, in which the collectors used are α-hydroxyarylphosphonous acid and alkyl Mixed collectors for xanthates. The copper oxide ore flotation method provided by the invention simplifies the treatment process of the copper oxide ore, and improves the grade and recovery rate of the obtained copper oxide concentrate product.

The invention relates to a method for producing poly aluminum chloride by using a byproduct of diethyl methylphosphonate production. The method comprises the following steps: (1) slowly adding a byproduct sodium tetrachloraluminate, rich in sodium tetrachloraluminate and obtained in a production process of diethyl methylphosphonate, into a dissolving kettle for dissolution, and collecting the solution; (2) adding ferric trichloride and hydrochloric acid; (3) sequentially adding aluminum hydroxide and calcium metaaluminate for polymerization reaction; (4) controlling the temperature to be 100 DEG C, and performing thermal reaction for 75min; and (5) cooling, and performing solid-liquid separation, wherein the filtrate is the product of the invention. The method disclosed by the invention has the advantages of simple process, high efficiency, low consumption, energy conservation, greenness and environmental friendliness and low cost.

The present invention relates primarily to a process for producing particular phosphinates (phosphonous acid monoesters) and use thereof for producing biologically active substances which may be used in the pharmaceutical or agrochemical sector, preferably for producing phosphorus-containing amino acids.

The invention provides a method for high-selectivity synthesis of phosphinic acid ester / phosphorous acid ester / phosphoric acid ester derivatives containing different substituted functional groups; a metal salt is used as a catalyst, a P(O)-OH-containing compound and aryl boronic acid are used as reactants, and an alkali, an additive and an organic solvent are added into the reaction system. The method has the advantages that the catalyst is cheap and easy to obtain; the reaction conditions are mild, and the method is safe and reliable; the selectivity of the obtained target product is close to 100%, and the yield is as high as 90% or more. The method solves the deficiency that traditional synthetic phosphinic acid ester / phosphorous acid ester / phosphoric acid ester compounds have poor reaction selectivity, complex reaction steps and low yield and need to use reagents harmful to the environment, and has a good prospect in industrial application. The invention also provides the corresponding phosphinic acid ester / phosphorous acid ester / phosphoric acid ester derivatives correspondingly containing different substituted functional groups.

The invention provides a method for resource utilization of diethyl methylphosphonite rectification high boilers. The method comprises mixing the high boilers of diethyl methylphosphonite rectification with hydrochloric acid, and performing a hydrolysis reaction. Finally, the ethanol is recovered by distillation to obtain the feed liquid A; the obtained feed liquid A is mixed with an alkyl alcohol, and reacted under heating and reflux conditions until anhydrous is generated to obtain the feed liquid B; the obtained feed liquid B is rectified to obtain methyl sulfide Alkyl phosphonates. The method can reduce waste discharge in the production process of diethyl methylphosphinate, protect the environment, has mild reaction conditions, does not need to add a catalyst, has low treatment cost, hardly generates waste liquid in the process, and is economical and environment-friendly.

A methylene phosphocarboxylic acid as water quality stabilizer is prepared from carboxy-contained amine, PCl3 (or phosphonous acid and concentrated hydrochloric acid) and water through heating and adding solution of formaldehyde. It has high output rate.

The invention discloses a spirobidihydrobenzosilole phosphorous acid monoester compound as well as a preparation method and application of the spirobidihydrobenzosilole phosphorous acid monoester compound. The invention specifically discloses a compound as shown in a formula I. The compound can be used for catalyzing a hydrosilicification reaction of allene or a hydroformylation reaction of terminal olefin, and has one or more advantages as follows: the operation is simple and convenient; the catalytic activity is high; the enantioselectivity of the product is high.