- Production process of diethylenetriaminepenta(methylene-phosphonic acid)
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The invention discloses a production process of diethylenetriaminepenta(methylene-phosphonic acid). The production process comprises the following specific operation steps: (1) adding metered hydrochloric acid, diethylenetriamine and phosphorous acid into a reactor in order, performing continuous stirring in the reactor, and maintaining the temperature at =50 DEG C; (2) performing heating to a certain temperature, adding a part of a formaldehyde aqueous solution dropwise at different flow rates, after the addition is completed, performing heat preservation, and performing concentration; and (3) adding hydrochloric acid, performing heating to 110-120 DEG C, adding the remaining formaldehyde aqueous solution dropwise, after the addition is completed, performing heat preservation for a reaction, performing evaporation, performing dilution, performing cooling, and adjusting the pH to obtain the qualified finished product. The method accelerates the reaction rate, not only effectively inhibits the production of by-product hydroxymethylphosphonic acid, improves the conversion rate and product yield of the effective active component diethylenetriaminepenta(methylene-phosphonic acid), butalso shortens the total reaction time, and reduces the production costs; and the method is simple, safe, and easy to operate, and is beneficial to industrial production.
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Paragraph 0018-0021
(2020/02/27)
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- PROCESS FOR PRODUCING HIGH-PURITY AMINOMETHYLENE PHOSPHONIC ACID
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PROBLEM TO BE SOLVED: To provide a method for producing a high purity amino methylene phosphonic acid, by which unreacted formaldehyde existing in amino methylene phosphonic acid can be removed at high yield, with simple method and with simple equipment without generating a dangerous material.SOLUTION: The method for producing the high purity amino methylene phosphonic acid includes a step of adding water to a distillation still during distillation when a coarse amino methylene phosphonic acid solution having a moisture content of 35-60 wt.% is distilled by using a batch-type distiller. The total amount of water to be added is at least 0.5 time the charge weight of the coarse amino methylene phosphonic acid.
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Paragraph 0047-0051
(2017/05/18)
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- A second ethylene triamine penta methylene phosphonic acid continuous production process
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The invention relates to a continuous production process for HTPMP. The process comprises the following steps: adding a certain mole ratio of diethylenetriamine, phosphorous acid, formaldehyde and hydrochloric acid into a mixing kettle, and uniformly mixing under 35 DEG C; pumping into a tubular reactor; after reaction, entering a thermal insulation kettle for thermal insulation and full reaction; after detecting that the phosphorus content is qualified, reducing pressure and externally evaporating formaldehyde; finally, dropwise adding hydrochloric acid for lowering the temperature and diluting to the needed active matter content. The production process adopts continuous feeding and continuous discharging, overcomes the defects of low rate of production, large energy consumption and the like of the current intermittent single-kettle mixing production process, and increases the rate of equipment utilization. The production cycle is shortened, the capacity is increased, the comprehensive energy consumption is reduced, and the large industrial scale production is easily realized.
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Paragraph 0025-0030
(2017/01/09)
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- METHOD FOR THE SYNTHESIS OF AMINOALKYLENEPHOSPHONIC ACID
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The present invention is related to a method for the synthesis of an aminoalkylenephosphonic acid or its phosphonate esters comprising the following steps: a) forming, in the presence of an aldehyde or ketone and an acid catalyst, a reaction mixture by mixing a compound comprising at least one HNR1R2 moiety or a salt thereof, with a compound having one or more P-O-P anhydride moieties, said moieties comprising one P atom at the oxidation state (+III) and one P atom at the oxidation state (+III) or (+V), wherein the ratio of moles of aldehyde or ketone to N-H moieties is 1 or more and wherein the ratio of N-H moieties to P-O-P anhydride moieties is 0.3 or more and, b) recovering the resulting aminoalkylenephosphonic acid comprising compound or its phosphonate esters.
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Paragraph 0078
(2014/02/15)
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- METHOD FOR THE SYNTHESIS OF ALPHA-AMINOALKYLENEPHOSPHONIC ACID
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The present invention is related to a new method for the synthesis of alpha-aminoalkylenephosphonic acid or its phosphonate esters comprising the steps of forming a reaction mixture by mixing a P-O-P anhydride moiety comprising compound, having one P-atom at the oxidation state (+111) and the other P-atom at the oxidation state (+111) or (+V), an aminoalkanecarboxylic acid and an acid catalyst, wherein said reaction mixture comprises an equivalent ratio of alpha-aminoalkylene carboxylic acid to P-O-P anhydride moieties of at least 0.2, and recovering the resulting alpha-aminoalkylene phosphonic acid compound or an ester thereof from the reaction mixture.
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Page/Page column 23
(2014/02/15)
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- Method for the Manufacture of Aminoalkylene Phosphonic Acid
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A method for the manufacture of amino alkylcnc phosphonic acids is disclosed. Pure P4O6 is hydrolyzed in the presence of a homogeneous Brocnstcd acid catalyst whereby the pH of the reaction medium is maintained below 5 and the free water content of said reaction medium is, after the P4O6 hydrolysis has been completed, from 0 to 40 %. The required amine component can be added before, during, or in one preferred execution, after the P4O6 hydrolysis has been completed. Formaldehyde is then added and the reaction mixture containing the P4O6 hydrolysate, the amine and the formaldehyde is reacted in presence of a Broensted acid catalyst selected from homogeneous and heterogeneous species. The amino alkylene phosphonic acid reaction product can then be recovered in a manner known per sé.
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Page/Page column 11
(2009/11/30)
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- Process for the manufacture of aminopolyalkylene-phosphonic acid compounds
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A beneficial method for the manufacture of amino polyalkylene phosphonic acids, under substantial absence of hydrohalogenic acid, is disclosed. The method, in essence, is based on reacting narrowly defined ratios of phosphorous acid, an amine, a formaldehyde in presence of specific ranges of an acid catalyst having a pKa equal or inferior to 3.1. The inventive method is capable of yielding economically and quality operational/capacity advantages, in particular significantly reduced one-step cycle duration under exclusion of corrosion disadvantages and also is environmentally friendly without requiring, in that respect, anything more than nominal capital expenditures.
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Page/Page column 9-11; 14
(2008/06/13)
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