175 results about "Methylphosphonic 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.

A process for extracting RE from the RE contained phosphorite is disclosed, which features that its immersing liquid is nitric acid, its salting-out agent is ammonium (or sodium) nitrate, its extractant is dimethylheptyl methylphosphonate (P350) or 2-ethylhexyl phosphonate-bis(2-ethylhexyl) ester (P502), its diluent is n-heptane or kerosene, its washing liquid is the solution of sodium (or ammonium) nitrate, its backextractant is the solution of nitric acid or hydrochloric acid, and its preciptant is oxalic acid. Its advantage is high purity (more than 95%) and high output rate (more than 98%) of RE.

The invention relates to a synthesizing method for pesticide glufosinate, i.e., ((D,L)-2-amino-4-(hydroxyl(methyl)phosphinyl)butyrate) and a salt of an acid or an alkali thereof. In the synthesizing method, the pesticide glufosinate is prepared by undergoing a strecker reaction, and an intermediate compound, i.e., (3-nitrile-3-hydroxy)propyl methyl phosphonic acid directly reacts with carbon dioxide and ammonia gas in an aqueous solution to synthesize the pesticide glufosinate and a salt of an acid or an alkali thereof. The method comprises the following specific steps of: adding the intermediate compound, i.e., (3-nitrile-3-hydroxy) propyl methyl phosphonic acid into a high-pressure kettle; adding carbon dioxide, ammonia gas and water, wherein ammonium bicarbonate or ammonium carbonate and the like can be used for replacing carbon dioxide carbon and ammonium, the molar ratio of the intermediate to the carbon dioxide is between 1 and 12, and the ratio of the ammonia gas to the carbon dioxide is between 0.5 and 5; adding 15-75 times of water; heating to 120-180 DEG C; reacting for about 4-20 hours; and after the reaction, cooling, taking the reaction liquid out, and concentrating to directly obtain an ammonium salt of glufosinate. The yield is over 80 percent.

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 a non-combustible solid polymer electrolyte and a secondary lithium battery containing the solid polymer electrolyte. The preparation method comprises the following steps of uniformly mixing an epoxy-terminated methyl phosphonate oligomer, a lithium salt and a battery additive which are in the mass ratio of (60 to 100): (10 to 44): (0 to 14), then, injecting the mixture between positive and negative pole pieces of the battery, and carrying out in-situ polymerization curing under the condition of heating so as to prepare the non-combustible solidpolymer electrolyte. According to the preparation method, in-situ polymerization curing is carried out in the battery by using a mixed solution of the low-molecular-weight liquid epoxy-terminated methyl phosphonate oligomer, the lithium salt and the battery additive as a solid electrolyte precursor, so as to prepare the non-combustible solid polymer electrolyte; by adopting methyl phosphonate as aconstruction unit, the polymer full-solid electrolyte has excellent flame retardance and safety performance, and the safety performance of energy storage batteries, particularly high-capacity batteries and battery packs is greatly improved.

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).

Methods of coating seeds with polymers and seeds coated with such polymers are disclosed herein. The polymers can be phosphonates, sulfonates, polymers of ethylenically unsaturated carboxylic acids, polyaminopolyethermethylene phosphonate, polysuccinic oligomers, acrylic acid/2-acrylamido-2-methylpropane sulfonic acid, blends of acrylic acid/2-acrylamido-2-methylpropane sulfonic acid with polyaminopolyethermethylene phosphonate, sulfomethylated acrylic acid/acrylamide, blends of sulfomethylated acrylic acid/acrylamide with polyaminopolyethermethylene phosphonate, polymaleic acid, acrylic acid/acrylamide copolymers, polyacrylic acid, trimethylglycine hydrochloride, blends of polyaminopolyethermethylene phosphonate with trimethylglycine hydrochloride, and any combination or salt of such polymers. Methods of monitoring, determining, and controlling the concentration of scale inhibitors in an agricultural irrigation system are also disclosed herein.

The invention relates to a circulating water scale inhibitor, which comprises the following components by weight portion: 2. 5 to 2.8 portions of PASP (polyaspartic acid), 1 to 1.2 portions of ATMP (amino trimethylene phosphonic acid), 2.4 to 2.6 portions of HPMA (hydrolyzed polymaleic anhydride), 1.2 to 1.4 portions of AA/AMPS (acrylic acid and 2-acrylamide-2-methyl propane sulfonic acid copolymer), 1.1 to 1.3 portions of PAA (polyacrylic acid), and 0.7 to 1.8 portions of water. The scale inhibitor prepared by the formulation is environment-friendly, has the characteristics of safety and reliability, easy preparation, convenient use and the like, and is suitable to be used as medicaments for preventing scale on circulating water systems in the fields of electric power, chemical engineering, medicine, petroleum, and the like.

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 invention relates to an intumescent flame retardant and a preparation method thereof. The intumescent flame retardant is polymethylene ammonium phosphonate which at least contains three methylammonium phosphonate groups -CH2P(O)(ONH4)2 in one molecule, and the intumescent flame retardant is prepared from polymethylene phosphonic acid and an ammonium source through a reaction, wherein the mole ratio of phosphonate groups PO3H2 to amino groups NH2 is 1:(2-2.5), a water solution is prepared from the ammonium source and water in the mass ratio being 1:(0.01-5) and dropwise added to polymethylene phosphonic acid while being stirred after complete dissolution, the reaction temperature is controlled to be 20-130 DEG C, the mixture is continuously stirred to react for 0.5-1.5 h after the water solution is dropwise added, evaporation concentration, cooling crystallization, filtration, washing, filtrate recovery for preparation of an ammonia source solution, filter cake drying and crushing are performed, and a product is obtained. The flame retardant is excellent in performance, good in stability and compatible with a polymer material, raw materials used in the preparation method are easily sourced, the cost is lower, and the process is simple, safe and environment-friendly.

The invention belongs to the technical field of nuclear material extraction and recovery, and relates to a method for extracting and recovering plutonium from a plutonium-containing nitric acid solution. The method comprises the following steps: oxidizing plutonium in the spent fuel reprocessing plutonium-containing nitric acid solution to tetravalent with an oxidant, adding an organic solvent containing DMHMP, Di(1-methyl heptyl)methyl phosphonate for extraction under strong acidic conditions, collecting organic phase, adding a reducing agent, performing back extraction under dilute acidic conditions to selectively reduce the tetravalent plutonium in the organic phase to trivalent, and performing back extraction to form the aqueous phase. The method for extracting and recovering plutoniumfrom the plutonium-containing nitric acid solution can efficiently separate plutonium from other impurities, such as uranium, fission product elements of plutonium, strontium, and cesium, and concentrate plutonium to obtain the plutonium nitrate product solution with standard purity.

The invention relates to a chromium-free metal surface treatment composition. The composition is characterized by comprising the following components: A) hydroxy-terminated water-soluble polydimethylsiloxane, B) silane coupling agent with alpha-functional group, C) bivalent or high-valent metal ions of Zr<2+>, Ca<2+>, Ce<3+> or Mo<6+> selected from at least one of Zr(CH3COO)2, Ca(CH3COO)2, Ce(NO3)3 and (NH4)6Mo7O24, D) pH regulator selected from at least one of hydroxyethylidene-1,1-diphosphonic acid, 2-phosphonic acid butane-1,2,4-tricarboxylic acid and amino trimethylene phosphonic acid, and E) deionized water, wherein the concentration range of the component A) is 50 to 100 g/L, the concentration range of the component B) is 2 to 10 g/L, the concentration range of the component C) is 0.2 to 5 g/L, and E) the balance of the component shown in the specification.

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 relates to a scale cleaning agent for a cinder flushing water system of an iron-making plant. The scale cleaning agent contains the following components in percentage by mass: 5%-45% of S-carboxyethyl thiosuccinic acid, 1%-45% of polyether polyamino methylene phosphonate N-oxide, 6%-40% of an acrylic acid-hydroxypropyl acrylate copolymer, 20%-35% of hydrochloric acid, 1%-25% of diethylenetriamine pentamethylene phosphate and 0.1%-3% of diisooctyl cis-butenedioate sulfonate, wherein the mass concentration of hydrochloric acid is 30%-36%. The invention further relates to a cleaning method for the cinder flushing water system of the iron-making plant. According to the scale cleaning agent, scale of equipment and pipelines in the cinder flushing water system of the iron-making plant can be effectively cleared; the scale cleaning agent has the advantages that the pertinence is strong, a formula is environment-friendly, the cost is low, and the preparation is simple; and the cleaning method has the advantages that the operation steps are simple and feasible, the cleaning is flexible, and use equipment is few.

The invention discloses a process for preparing tenofovir. The method is characterized by comprising the steps: with adenine, (R)-propylene carbonate and p-toluenesulfonyloxy methyl phosphonic diester as raw materials, adopts a one-pot process to prepare an intermediate 2, and followed by hydrolyzing the intermediate 2 by an inorganic acid to obtain tenofovir, wherein the following reaction formula is shown in the description. With utilization of the process, the purpose that high-purity tenofovir is synthesized with utilization of cheap and easily available raw materials and with simple operation, mild reaction conditions, low cost and high yield is achieved; and the process has the advantages of energy saving and environmental protection, is suitable for large scale production, and has practical value in realization of industrial production of tenofovir.

The present invention sets forth an improved method of microetching a metal substrate by contacting the substrate with an aqueous composition comprising a sodium persulfate or hydrogen peroxide oxidizing agent, acid, and one or more additives. When the oxidizing agent is sodium persulfate, the one or more additives generally comprise an aliphatic saturated dicarboxylic acid. When the oxidizing agent is hydrogen peroxide, the one or more additives generally comprise a stabilizer and amino tris(methylene phosphonic acid).

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.