- Method for producing 2-carboxethyl phenylphosphinic acid without wastewater
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The invention relates to a method for producing 2-carboxethyl phenylphosphinic acid without wastewater. According to the technical solution, dichlorophenylphosphine, acyclic acid and water are taken as raw materials, dichloropropane is taken as a solvent, and the method comprises the following steps of fully reacting the dichlorophenylphosphine and the acyclic acid to generate an acyl chloride intermediate; dropwise adding water into mixed liquor of the acyl chloride intermediate and dichloropropane according to a reaction mole ratio, and performing hydrolysis to generate the 2-carboxethyl phenylphosphinic acid. A required amount of water is added dropwise in reaction, so that production of a large amount of acidic wastewater is avoided, and moreover, a high-quality byproduct hydrochloric acid is recycled; the dichloropropane is taken as the solvent, so that the problem that conventional process wastewater contains 2-carboxethyl phenylphosphinic acid is solved, and yield is increased; the dichloropropane can be distilled for continuous use after being recycled for many times, so that the production cost is reduced, and the problem of existence of a large amount of wastewater in a conventional production process is solved.
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Paragraph 0023; 0024
(2016/12/01)
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- Process for the preparation of 2-carboxyalkyl(aryl)phosphinic acid and corresponding anhydride(s)
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An improved hydrolysis process comprising a process for the preparation of 2-carboxyalkyl(aryl)phosphinic acid using a controlled addition of water to an acrylation reaction mixture, and control of the temperature. Preparation of 2-carboxyalkyl(aryl)phosphinic acid cyclic anhydride is disclosed using a controlled addition of water, wherein up to about one mole of water per mole of dichloro(aryl)-phosphine charged to the acrylation reaction is added, and temperature is controlled.
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- Method for preparation of 3-(hydroxyphenyl phosphinyl)-propanoic acid
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The present application relates to a method for the preparation of 3- (hydroxyphenylphosphinyl) -propanoic acid by the condensation of phenylphosphonous dichloride and acrylic acid and the hydrolysis of the condensate, in which, under a pressure of greater than 1 atm, acrylic acid is added at 65～110 °C at an amount more by 10～25 mole% than that of phenylphosphonous dichloride and the condensation is carried out at a temperature of 70～100 °C under at greater than 1 atm.
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- Method for preparing 3-(hydroxyphenylphosphinyl)-propanoic acid
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Disclosed is a method for the preparation of 3-(hydroxyphenylphosphinyl)-propanoic acid which is commonly used as a flame retardant for polyester resins. The preparation of 3-(hydroxyphenylphosphinyl)-propanoic acid is accomplished by reacting phenylphosphonous dichloride with phenylphosphinic acid to give a hydrophosphoryl compound, reacting the hydrophosphoryl compound with acrylolyl chloride to give 3-(chlorophenylphosphinyl)-propionyl chloride, the acryloyl chloride being present at an amount more by 5-30 mole % than the amount of the hydrophosphoryl compound, and hydrolyzing the 3-(chlorophenylphosphinyl)-propionyl chloride to the 3(hydroxyphenylphosphinyl)-propanoic acid. This method enables 3-(hydroxyphenylphosphinyl)-propanoic acid to be produced at high yields with good color through low temperature reactions. In addition, the method is economically favorable because the remainder of the acryloyl chloride after the addition reaction can be collected and recycled with ease.
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- Production of 2-carboxyalkyl (phenyl)phosphinic acid
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Processes for producing 2-carboxyalkyl(phenyl)phosphinic acid comprising hydrolyzing the reaction mixture produced from the reaction of dichloro(phenyl)phosphine with a carboxylic acid in the presence of water, wherein the hydrolysis is conducted with reduced levels of water.
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- Method for preparation 3-(hydroxyphenylphosphinyl)-propanoic acid
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Disclosed is a method for the preparation of 3-(hydroxyphenylphosphinyl)-propanoic acid which is commonly used as a flame retardant for polyester resins. The preparation of 3-(hydroxyphenylphosphinyl)-propanoic acid is attained by the condensation of phenylphosphonous dichloride and acrylic acid and the hydrolysis of the condensate. In the condensation, the mole ratio of phenylphosphonous dichloride to acrylic acid is within the range of 1:1.1 to 1:1.25. Under a pressure of greater than 1 atm, acrylic acid is added at 65 DIFFERENCE 110 DEG C. at an amount more by 10 DIFFERENCE 25 mole % than that of phenylphosphonous dichloride and the condensation is carried out at a temperature of 70 DIFFERENCE 100 DEG C. under at greater than 1 atm, to produce 3-(hydroxyphenylphosphinyl)-propanoic acid at high yields with desired color.
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- Process for producing ogranophosphorus ester compound and reactive flame retardant
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1 A process for producing a purified organophosphorus alkyl ester compound in which the reaction mixture obtained by reacting a dichlorophosphine derivative with (meth)acrylic acid is esterified with a lower monool, and the resulting reaction mixture is neutralized with an alkali metal hydroxide or alkaline earth metal hydroxide either in a solid form or in the form of an aqueous solution and purified; 2 a process for producing a purified organophosphorus hydroxyalkyl ester compound or an alkylene glycol solution thereof which comprises subjecting the purified organophosphorus alkyl ester compound obtained by process 1 to transesterification with an alkylene glycol; 3 a reactive flame retardant comprising the purified organophosphorus alkyl ester compound obtained by process 1; and 4 a reactive flame retardant comprising the purified organophosphorus hydroxyalkyl ester compound or alkylene glycol solution obtained by process 2.
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- Method of producing a phosphinyl-carboxylic acid derivative
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A phosphine derivative of the following general formula ( I ): STR1 (wherein R1 is an alkyl group having 1 to 18 carbon atoms or an aryl group having 6 to 18 carbon atoms, and the aryl group may have an alkyl group having 1 to 18 carbon atoms or an alkenyl group having 2 to 18 carbon atoms) is reacted with acrylic acid or methacrylic acid in the presence of a catalyst selected from the group consisting of an organic peroxide and an azo-compound, and the resulting reaction product is hydrolyzed with water, thereby to obtain a phosphinyl-carboxylic acid derivative of the following general formula (III): STR2 (wherein R1 is as defined above, and R2 is a hydrogen atom or a methyl group). Based on the reaction above-mentioned, ester of free acid and a cyclic acid anhydride can also be obtained. Accordingly, the target compound can be obtained at a relatively low reaction temperature in a short period of time with high yield. The reaction proceeds substantially quantitatively, thus enhancing the productivity and facilitating the purification.
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