113 results about "Methylphosphinic acid" patented technology

The invention relates to a preparation method of a fire retardant, in particular to a dialkyl metal phosphinate and a synthesis process of a fire retardant thereof. The dialkyl metal phosphinate has a structural formula described in the specification, wherein R1 represents alkyl, M represents metal ions, n represents an integer from 1 to 3, and R2 represents olefin of aliphatic series. The preparation method comprises the steps of: reacting alkylphosphonous dichloride with alcohol to obtain monoalkyl phosphate; carrying out radical reaction on the monoalkyl phosphate with olefin to obtain dialkyl ester phosphinate; and reacting the dialkyl ester phosphinate with lewis acid to obtain the dialkyl metal phosphinate fire retardant. The invention has mild reaction condition; the prepared product has good thermal stability and high yield, wherein the yield can reach 87.6 percent by the count of methyl butyl ester phosphate; and the preparation method is suitable for industrialized production.

Solvent extraction of one or more metal ions from an aqueous solution in the presence of hydrocarbon-soluble aminomethylenephosphonic acid derivatives.

The invention relates to a new preparation method for herbicide glufosinate. The method comprises the following steps of: performing Bucherer-Bergs cyclization reaction on a methylphosphonate derivative type compound (II), ammonium carbonate and cyanide serving as raw materials to obtain a compound shown by a formula (III); and then hydrolyzing to prepare glufosinate compound shown by a formula (I). According to the preparation method, hemiacetal or acetal is used as a raw material, and the Bucherer-Bergs cyclization reaction is performed to obtain a glycolylurea derivative, so that high yield, easiness for detection and mild condition are guaranteed; and after glycolylurea is cyclihydrolyzed, a product has high purity, and ammonium salt can be removed without multiple recrystallization processes.

The invention provides a method or preparing a glufosinate ammonium salt. The method comprises the following steps: 1, taking a proper amount of methylphosphonate, adding the taken methylphosphonate to a sodium cyanide, ammonium chloride and ammonia water mixed solution, and reacting at 5-45DEG C for 2-8h to generate aminonitrile phosphine ester; 2, slowly adding an acid to the aminonitrile phosphine ester, and reacting to obtain a glufosinate ammonium salt mixture; 3, adding R<1>OH to the glufosinate ammonium salt mixture, heating and refluxing the obtained solution, introducing ammonia gas after the above reaction ends, cooling after ammonia gas introduction ends, and filtering and separating out ammonium chloride to obtain an alcohol solution of glufosinate ammonium ester; and 4, carrying out reduced pressure alcohol removal on the obtained alcohol solution of glufosinate ammonium ester, adding an alkali, reacting, carrying out reduced pressure concentration after the reaction ends, carrying out alcohol precipitation, filtering the obtained solution, and drying the obtained precipitate to obtain the glufosinate ammonium salt. Cheap and easily available ammonia gas is used to substitute flammable, explosive and cancerigenic propylene oxide in traditional methods, so the method provided by the invention has the advantage of economy, safe operation and high industrialization prospect.

The invention relates to a preparation method of low-trimethylene-content amino trimethylene phosphonic acid, which comprises the following specific processing steps: adding ammonium chloride, an amino trimethylene phosphonic acid mother solution and formalin into a reaction kettle, and increasing the temperature to 90 DEG C; dropwisely adding formaldehyde and phosphorous acid, and keeping refluxing while controlling the temperature; after the dropwise addition, performing refluxing reaction while keeping the temperature; detecting the phosphite content, supplementing formaldehyde, and further performing refluxing reaction while keeping the temperature; performing negative pressure outer evaporation to remove the ammonium chloride, the formaldehyde and hydrogen chloride; and cooling, and adding reverse osmosis water to regulate the active matter content. According to the invention, the provided amino trimethylene phosphonic acid has the characteristic of low trimethylene content (the active matter content is 50+/-2%, and the trimethylene content is 24-26%); and compared with the common commercially available amino trimethylene phosphonic acid, the provided amino trimethylene phosphonic acid has better compatibility with zinc corrosion inhibitor, and can regulate the amount of zinc corrosion inhibitor in a compound product in a wider range. Besides, the invention widens the application range of the amino trimethylene phosphonic acid in different water bodies.

This invention discloses the method for separating cerium and recovering fluorine and preparing ultramicro-powder cerium trifluoride. In this invention method, bastnasite ore or the mixture containing bastnasite ore and eremite ore is used as raw material mixed with sulfuric acid or nitric acid or the mixture containing both in optional ratio. The extractant is the mixture containing EXTR1 and EXTR2. Said EXTR1 is trialkyl phosphine oxide or dimethyl heptyl methyl-phosphonate or tritutyl phosphate; and said EXTR2 is di(2-ethylhexyl) phosphate, or mono 2-ethyl-hexyl 2-ethyl-hexyl-phosphonate, or di (2,4,4-trimethyl pentyl) phosphonate. The diluent is paraffine or sulfonated kerosene. The products of Ce3+ and cerium trifluoride are obtained after the loading organic phase is proceeded washing and back-extraction. The purity of the cerium trifluoride is 99.9-99.999%, and the grain size distribution is 40-300nm, the recovery rate of cerium is greater than 95%, and fluorine than 98%.

The invention discloses a preparation method of glufosinate-ammonium. The method comprises the steps that methylphosphonate compound (II) and benzylidene glycine ester compound (III) are reacted, so as to obtain benzylidene phosphonic butyric ester compound (IV); the benzylidene phosphonic butyric ester compound (IV) is further hydrolyzed, so as to obtain hydrochloride (V); finally, the target product glufosinate-ammonium (I) is obtained. The method has the advantages that the utilization of extremely toxic substance cyanide is avoided, the reaction condition is mild, monitoring is easy, and repeated recrystallization is not required for removing inorganic salt. (img file='DDA0000501075940000011.TIF' wi='1408' he=' 672' /).

The invention discloses a novel sensor, and specifically discloses a molecularly-imprinted photonic crystal (MIPC) which is used for detecting organophosphorus toxicants timely and quickly. The MIPC employs methylphosphonic acid and ethylphosphonic acid as imprinting templates. An intensity of a reflectance spectrum of the corresponding imprinted photonic crystal decreases significantly with the increase of the concentration of a target compound or with the absorption time. The MIPC also shows some practical application values, and shows effects of low detection limit and high sensitivity in detections for the organophosphorus toxicants such as sarin, soman, VX and R-VX prototypes.

The invention discloses a preparation method of glufosinate-ammonium and derivatives thereof. The method comprises the following steps: (1) by using a substituted hydantoin and methylphosphonate compounds as a raw material, adding alkali, carrying out nucleophilic substitution reaction at the reaction temperature of 20-100 DEG C in a reaction solvent to obtain a hydantoin derivative, and tracing product generation condition by high performance liquid chromatography in the reaction process to judge the reaction endpoint, wherein the molar ratio of the methylphosphonate compounds, substituted hydantoin and alkali is 1:(1.0-5.0):(1.0-4.0); (2) carrying out reflux reaction for prepared hydantoin derivative prepared and an inorganic acid in water for 30-60 hours; after reaction, adding ammonia water to adjust the pH of the liquor to 12; spirally distilling to remove the solvent; adding absolute methanol for reflux for 30-60 minutes; filtering; spirally drying the mother liquor; adding methanol for recrystallization to obtain pure glufosinate-ammonium shown in formula (I) or derivatives thereof, wherein the molar ratio of the hydantoin derivative and inorganic acid is 1.0:(4.0-9.0).

The invention discloses a preparation method and use of an organic aluminum phosphate fire retardant. The method comprises: hydrolyzing dimethylmethylphosphonate under the action of sodium hydroxide or potassium hydroxide to form the sodium or potassium salt of dimethylmethylphosphonate, wherein the molar ratio of the dimethylmethylphosphonate to the sodium hydroxide or potassium hydroxide is 1:1; and reacting the aqueous solution of the sodium or potassium salt of dimethylmethylphosphonate with aluminum sulfate under heating and violently stirring CONDITIONS according to a molar ratio of 6:1 to form aluminum methyl methyl phosphonate. The aluminum methyl methyl phosphonate prepared by the invention only is formed by only reactions both of which are performed by using water as reaction medium, the process is simple and the efficiency is high. The thermal decomposition temperature of the aluminum methyl methyl phosphonate prepared by the method is above 325 DEG C, and the aluminum methyl methyl phosphonate can be used as V-0 grade fire retardant for thermoplastic plastics such as poly butylenes terephthalate (PBT) resin, poly(ethylene terephthate) (PET) resin, polyamide PA66 resin and poly(p-phenylene oxide) (PPO) resin.

The invention belongs to the technical field of nuclear waste treatment and recycling, and relates to a method for extracting and recycling neptunium from spent fuel aftertreatment waste liquid. The method comprises following optional order-replaceable repeatable steps, and water phase back-extraction matte is finally collected. The steps comprise 1, neptunium in a neptunium-containing water phase solution is oxidized to be hexavalent, and an organic solvent containing dimethyl phosphonate (1-methyl heptyl) ester is added under the strong acid condition for extraction; organic phases are collected, a reducing agent is added, reextraction is carried out under the dilute acid condition, and therefore hexavalent neptunium in the organic phases is selectively reduced to be pentavalent and reextracted to enter a water phase; 2, a reducing agent is used for reducing neptunium in the water phase solution to be tetravalent, and an organic solvent containing dimethyl phosphonate (1-methyl heptyl) ester is added under the strong acid condition for extraction; and organic phases are collected, reextraction is carried out under the dilute acid condition, and therefore tetravalent neptunium in the organic phases is reextracted to enter the water phase. By means of the method, a neptunium nitrate solution with standard purity can be prepared.

The present invention relates to a method for improved removal of cations, preferably alkaline earth metals, in particular calcium and barium, from aqueous solutions using chelating resins having aminomethylphosphonic acid groups and iminodimethylphosphonic acid groups having high dynamic absorption capacity for cations at a low residual content of the cations and high regeneration efficiency, and a markedly lengthened loading duration of the chelating resin, to the chelating exchangers themselves, and also to uses thereof.

The invention discloses a process for preparing methyl ethylphosphinate and methyl ethylphosphinate aluminum salt, and belongs to the technical field of flame-retardant materials, aiming to solve thedifficulty in realization of industrial production of the methyl ethylphosphinate in the prior art. The process for preparing the methyl ethylphosphinate and the methyl ethylphosphinate aluminum saltincludes taking sodium iodide as a catalyst, and reacting methyl diethylphosphinate at the temperature of 80-180 DEG C to generate the methyl ethylphosphinate; reacting the methyl ethylphosphinate with aluminum trichloride in a solvent to obtain the methyl ethylphosphinate aluminum salt. The process has the advantages that the low-purity methyl diethylphosphinate serves as a raw material, the methyl ethylphosphinate is obtained under a moderate condition and at high yield, and industrialization is realized easily; methyl ethylphosphinate aluminum flame retardants with high phosphorus content are further obtained, and are environment-friendly halogen-free flame retardants for polymer materials.

The invention discloses an amino trimethylene phosphonic acid (ATMP) with content of greater than or equal to 90 percent and process for preparation, wherein the product comprises (by weight percentage) amino trimethylene phosphonic acid 90-98%, unavoidable impurity substance 1-2%, and balancing water. The production process comprises the steps of stock preparation, charging sodium acetate as crystal nucleon, agitating, charging anhydrous alcohol as crystallizing aid agent, dewatering, and drying.

The invention discloses a thorium and uranium separating and recovering method. The method comprises the following steps: 1) taking aqueous acid containing thorium and uranium as material liquid, taking an organic solvent containing methylphosphonic acid di(1-methyl) heptyl ester, taking the aqueous acid as washing liquid for fractionation and extraction; 2) taking the organic solvent containing methylphosphonic acid di(1-methyl) heptyl ester as an extraction supplement agent, taking the aqueous acid as the washing liquid, and performing fractionation and extraction on an organic extract phase containing thorium and uranium, the extraction supplement agent, and the washing liquid; and 3) performing back extraction on the organic extract phase containing uranium and strip liquor in a multistage counter current mode. Under conditions of low feeding acidity, organic phase/water phase flow ratio and less extracting stage number, separating and recovery of thorium and uranium are realized, high thorium and uranium recovery rate can be obtained, and the impurity metal ion decontamination coefficient is obtained.

The present invention provides methods and compositions for detecting, identifying and measuring the abundance of chemical nerve agents. Methods and compositions of the present invention are capable of providing selective detection of phosphorous based nerve agents, such as nerve agents that are esters of methyl phosphonic acid derivatives incorporating a moderately good leaving group at the phosphorus. Selectivity in the present invention is provided by a sensor composition having an alpha (α) effect nucleophile group that undergoes specific nucleophilic substitution and rearrangement reactions with phosphorus based nerve agents having a tetrahederal phosphorous bound to oxygen. The present invention includes embodiments employing a sensor composition further comprising a reporter group covalently linked to the alpha effect nucleophile group allowing rapid optical readout of nerve agent detection events, including direct visual readout and optical readout via spectroscopic analysis.

The invention discloses a method for measuring the residual quantity of glufosinate, glyphosate and metabolite aminomethyl phosphonic acid thereof in tea. A liquid chromatography-tandem mass spectrometry method for measuring glufosinate, glyphosate and metabolite aminomethyl phosphonic acid thereof in tea is established by virtue of pure water extraction, dichloromethane liquid-liquid extraction and SHS-SAX solid phase extraction column purification and enrichment. The method is simple and fast, has high sensitivity and good reproducibility, and is successfully applied to daily inspection of tea samples.

The invention provides an arylmethyl phosphonate preparation method. The method includes the following steps that arylmethyl ester, triethyl phosphate and a catalyst are sequentially added into a reactor and reacted for 5-8 h at the temperature of 100-200 DEG C after full stirring, and after excessive triethyl phosphate is distilled off through decompression, the mixture continues to be reacted for 3-7 h at the temperature of 100-200 DEG C; then, the mixture is cooled to the room temperature, a product is extracted through a mixed solvent, and arylmethyl phosphonate is obtained after the mixed solvent is removed. The catalyst is one or more of tetramethyl ammonium bromide, tetraethylammonium bromide, tetrabutyl ammonium bromide, benzyltrimethyl ammonium bromide, cetyl trimethyl ammonium bromide, cetyltrimethyl ammonium chloride, ammonium chloride, sodium iodide and potassium iodide. Arylmethyl phosphonate is synthesized through a one-step method, other solvents are not added, operation is easy, and the product yield is high and can be 85.3% at maximum.

The invention relates to a preparation method of a self-reproducing activated carbon filter element and belongs to the technical field of preparation of water purifying materials. An enzymolysis filtrate and crushed coconut shells are blended and fermented, a reaction filter cake is carbonized and then is mixed with potassium thiocyanate and amino trimethyl phosphonic acid for a reaction, finally,a product is mixed with polyethylene for membrane casting and firing, and the self-reproducing activated carbon filter element is obtained. Firstly, an enzymatic hydrolysate containing rich amino acid is obtained through enzymolysis, the enzymatic hydrolysate and the crushed porous coconut shell particles are mixed and sealed to be fermented under the action of rich microorganisms, then, coconutshells containing carboxyl and amino groups and an iron salt solution are mixed for a reaction, activated carbon is obtained, the activated carbon, potassium thiocyanate and amino trimethyl phosphonicacid are blended, part of metal ions in the activated carbon are removed, the oxidability of the prepared activated carbon is greatly improved due to holes, the activated carbon and water react to produce hydroxyl free radicals .OH with very high oxidability, the self-reproducing purpose is finally achieved, and the activated carbon filter element has broad application prospects.

The invention relates to a transparent flame-retardant organic glass plate and a preparation method thereof. The transparent flame-retardant organic glass plate is prepared from the following raw materials in parts by weight: 60-80 parts of methyl methacrylate, 2-35 parts of tris (2-chloroethyl) phosphate, 2-20 parts of dimethyl methylphosphonate, 0.01-0.5 part of azodiisoheptonitrile, 0.01-0.5 part of azodiisobutyronitrile and 0.01-0.5 part of stearic acid. Compared with the prior art, the transparent flame retardant organic glass plate with flame retardant performance reaching UL 94V2 to UL94V0 grade and the transparence over 92% is prepared by adding a phosphorus flame retardant, a plasticizer, a high temperature initiator, a low temperature initiator and a release agent into the methyl methacrylate.