254 results about "Diethyl phosphate" patented technology

The invention relates to a low-odour polypropylene compound, the compound comprises (by weight ratio) polypropylene 55-95, talcum powder 0-40, fatty acid ester compound 0.5-3, nano zinc oxide 0.5-3, nano titanium oxide 0.5-3, heat stabilizer DSTP 0.1-1.0, heat stabilizer 3114 0.1-1.0, heat stabilizer 618 0.1-0.5, wherein the fatty acid ester compound being C25-C45 long-chain fatty acid ester, the heat stabilizer DSTP being octadecyl thiodipropionate, the heat stabilizer 3114 being 3,obtaining 5-ditert-butyl-4-hydroxy benzylphosphonate diethylate, the heat stabilizer being dioctadecyl pentaerythritol diphosphite.

The invention relates to a synthesis technique of tenofovir, and relates to the field of medicinal chemistry. Using natural (R)-lactate as the starting material, chiral R-1,2-propanediol is obtained through reduction, and then reacted with diethyl carbonate under the action of alkali to obtain the key reaction intermediate R-propylene carbonate ester. Use adenine and R-propylene carbonate to prepare R-9-(2-hydroxypropyl)adenine; Gained R-9-(2-hydroxypropyl)adenine and diethyl p-toluenesulfonyloxyphosphate Under the catalysis of magnesium tert-butoxide, the condensation reaction is carried out to obtain R-9[(diethylphosphorylmethoxy)propyl]purine; the obtained R-9[2-(diethylphosphorylmethoxy) Propyl]purine is hydrolyzed to obtain Tenofovir. The process has short reaction steps, short required reaction time, high quality yield and good product quality, and is suitable for industrialized production.

The invention relates to a method for synthesizing argatroban. The method comprises the following steps that nitryl L-arginie and quinoline sulfonchloride are condensed, and undergo amidation with piperidine ethyl formate, followed by hydrolysis and hydrogenation to obtain argatroban; the amidation is to make carboxylate (c-v) and (2R, 4R) 4MPE (Z-VII) react in an organic solvent in the presence of condensing agent, or the presence of both condensing agent and dehydration promoter, in which the molecular ratio of carboxylate (c-v): (2R, 4R) 4MPE (Z-VII): condensing agent: dehydration promoter is 1: 0.8-1.2: 0.8-1.2: 0-1.2. The condensing agent adopted by the invention is diphenylphosphoryl azide, diethylthiophosphoryl, chlorophosphoric acid diethyl or bromophosphoric acid diethyl. The invention has simplified operation, lowered cost, decreased pollution, increased yielding rate, and is suitable for large-scale industrialized production of argatroban.

The invention provides conjugate polyether, comprising 6-8 parts of polyether polyol EP-330N, 2-4 parts of polyether polyol SU-450L, 0.06-0.15 parts of non-hydrolytic surface active agent, 1.5-2 parts of water, 0.8-1.5 parts of nonyl phenol polyoxyethylene ether NP-10, 0.03-0.05 part of foaming catalyst PC52, 0.3-0.5 part of foaming catalyst NE300 and 1.3-2 parts of ethyl diethyl phosphate. The invention further provides a polyurethane raw material composition, polyurethane foams and applications thereof. Compared with the conventional polyurethane foams, the polyurethane foams in the invention have low density, low mass, proper aperture ratio, good sound-proofing effect, and good heat insulating effect, and compared with the polyurethane foams with middle and high density, the cost of the polyurethane foams in the invention is lower. While the polyurethane foams in the invention have low density, the polyurethane foams can reach the application standards of thermal insulation materials, sound-proofing materials, sandwich panels for construction, spraying materials for ceilings of automobiles or filling materials and the like. The conjugate polyether is a total-moisture foaming system, has no damage to ozone layer and has the advantage of environmental protection.

The invention relates to the technical field of cable materials, in particular to a modified high-flame-retardation weather-resistant polyurethane cable material and a preparing method thereof. The modified high-flame-retardation weather-resistant polyurethane cable material comprises modified polyurethane elastomer, ethylene-vinyl ethylene copolymer, nitrile rubber, chlorinated polyethylene, antimony trioxide, calcium chloride, ethyl phosphoric acid diethyl ester, a lubricating agent, a dispersing agent, an antioxidant, a rat-proof master batch, a termite-proof master batch and an ultraviolet light absorber. The modified polyurethane elastomer is formed by anionic polyurethane of lateral chain band sulfonic group or/and carboxylic group, tetra-n-butyl titanate, organic solvent, deionized water and a catalyst. According to the preparing method of the modified high-flame-retardation weather-resistant polyurethane cable material, as the modified polyurethane elastomer is used as the main raw material, the modified polyurethane cable material prepared by the method has high flame retardation and weather resistance.

The invention provides a synthesis method for glufosinate shown as a formula (V) and an analogue thereof. The method comprises the following steps of: preparing an intermediate such as methyl diethyl phosphate by Grignard, disproportionation and coupling and with phosphorus trichloride, triethyl phosphate and chloromethane as initiative raw materials; condensing the methyl diethyl phosphate, anhydride and acrolein substances; performing Strecker reaction and hydrolysis and thus obtaining the glufosinate and the analogue thereof. In the synthesis method, the reaction condition is mild; safety is high; and yield is obviously increased.

The invention provides efficient neutral formaldehyde capture agent, which consists of deionized water, melamine, formalin solution, methyl salicylate, isoamyl alcohol, polysorbate, diethyl phosphate, sodium dodecyl benzene sulfonate and activated carbon. The invention further provides a method for preparing the efficient neutral formaldehyde capture agent. The efficient neutral formaldehyde capture agent can rapidly react with formaldehyde to form innocuous and unpoisonous colorless transparent liquid with excellent stability, and can not produce secondary pollution for environment at the same time. The efficient neutral formaldehyde capture agent is low in cost of raw materials, simple and easy in production process, and simple and convenient to use.

The invention discloses polyurethane sponge and a processing method thereof. Polyether polyol with a flame retardant function is directly added to a material A, and a diethyl ethylphosphonate fire retardant is selectively added to a material B, so that the polyurethane sponge does not contain halogen, is low in viscosity and very stable in a two-component system of the material A and the material B, and a product is endowed with good fireproof and flame-retardant properties while the process is simple. The product is endowed with good mildew-proof and antibacterial effects through an antibacterial agent and a mildew preventive added to the material B; and through addition of nanoscale inorganic material tourmaline powder, the product has the function of lastingly emitting anions. The production technology and the formula are relatively simple on the premise that all performance indexes reach the expected requirements; the production process and the formula are relatively simple; the processes such as heating or refrigerating do not need to be specifically carried out in the production process and foaming and curing in a natural state can be carried out; the production success rate of sample post-detection is very high; the produced polyurethane sponge has obvious fireproof and flame-retardant functions, antibacterial and anti-mildew functions and continuous anion release function, and is beneficial to improvement of the competitiveness of the product.

The invention discloses a concise glufosinate ammonium synthesizing method and aims at solving the problem that an existing method needs to use toxic sodium cyanide to synthesize glufosinate ammonium.Being different from an existing method of using diethyl methyl phosphite to prepare the glufosinate ammonium, the concise glufosinate ammonium synthesizing method disclosed by the invention can effectively avoid using toxic chemicals; thus, the problem of using the sodium cyanide is solved. By means of the synthesizing method, use of toxic chemicals is reduced, operation steps are simplified, equipment investment is reduced, the amount of three wastes is reduced, a requirement for clean production is met, and more environmental friendliness is achieved. Meanwhile, the synthesizing method disclosed by the invention not only can synthesize racemate glufosinate ammonium, but also can synthesize optical pure-chirality glufosinate ammonium, so that the synthesizing method has obvious progressive significance. According to the synthesizing method disclosed by the invention, technique connection is orderly, no solid material is used, convenience in operation is achieved, a technological process is simple, automatic production is achieved, labor intensity of workers is greatly reduced, and a production efficiency is improved; thus, the synthesizing method has a better application prospect and is worth of popularizing and applying in a large scale.

The invention discloses antibacterial and mothproof silk composite fibers. The antibacterial and mothproof silk composite fibers are characterized by comprising the following materials in parts by weight: 17-20 parts of mulberry silk, 10-13 parts of tencel, 12-15 parts of chicken feather down fibers, 4-7 parts of acrylic fibers, 6-9 parts of aloe fiber, 7-10 parts of kawo kawo fiber, 1.2-3.2 parts of chitin fibers, 2-3 parts of epoxidized soybean oil, 0.3-0.5 part of calcium carbonate, 0.1-0.3 part of sodium sec-alkyl sulfonate, 1-3 parts of mica powder, 100-110 parts of 1-butyl-3-methylimidazole dibutyl phosphate, 120-125 parts of 1-ethyl-3-methylimidazole diethyl phosphate, 1.2-3.2 parts of folium cortex eucommiae, 1-3 parts of rhizoma corydalis, 2-4 parts of radix rubiae, 2-5 parts of additives and a proper amount of water. Due to addition of the multiple plant fibers and Chinese herbal medicines, the silk composite fibers have good antibacterial, mothproof, breathable, moisture-absorbing and heat-preserving functions, and the prepared silk composite fibers are also high in elasticity, strength and washing durability.

The invention discloses a cardanol-based phosphatefire-retardant plasticizer and a preparation method thereof. The preparation method comprises the following steps: with cardanol and diethyl chlorophosphate as main raw materials, carrying out substitution reaction in the presence of an acid binding agent to synthesize cardanol-based diethyl phosphate; further with cardanol-based phosphoric acid as a raw material, in the presence of a peracetic phosphotungstate phase transfer catalyst, adding a peracetic source dropwise for epoxidation to prepare crude epoxy cardanol-based diethyl phosphate, and filtering, washing and dehydration to obtain a finished epoxy cardanol-based glycidyl ether plasticizer. According to the cardanol-based phosphatefire-retardant plasticizer and the preparation method disclosed by the invention, as the cardanol is taken as the raw material, the cost is low, and the source is wide; the preparation process is simple, the energy consumption is low; the product is low in toxicity, is environmentally friendly, is capable of endowing a polymer substrate with excellent flame retardancy and flexibility and has good application prospect.

The invention discloses a synthesis method for resveratrol, including (1) discharging hydrogen bromide gas to benzene solution of p-methoxy benzyl alcohol to obtain p-methoxy benzyl bromide, (2) carrying out reaction of p-benzyl bromide with triethyl phosphate to obtain diethyl p-methoxy benzyl phosphate, (3) carrying out reaction of diethyl p-methoxy benzyl phosphate with sodium amide and 3,5-dimethoxybenzaldehyde to obtain (E)-3, 4', 5-trimethoxystilbene, and (4) carrying out reaction of (E)-3, 4', 5- trimethoxystilbene with aluminum iodide to obtain the final product. The invention has the advantages of raw materials easy to get, lowered cost, mild reaction conditions, simplified operation, and enhanced yield.

The invention provides salts of 5-Aminolevulinic acid (ALA) of formula (I):

• • wherein RY is an organic acid moiety; Y is selected from the group consisting of a sulfonic acid residue, mono- or di-phosphoric acid residue, mono- or di-carboxylic acid residue and R is selected from the group consisting of saturated, unsaturated, straight or branched C₂-C₂₀ chains, aryl, aralkyl or naphthyl. In preferred embodiments, RY is selected from benzenesulfonic acid (besylate), 2-naphthalene sulfonic acid (napsyate), p-toluenesulfonic acid (tosylate), diethyl phosphate, dibenzyl phosphate, di-(2-ethylhexyl) phosphate, caproic or stearic acids. The invention also provides methods for preparing the ALA salts of the invention, pharmaceutical compositions containing the ALA salts of the invention, and use of the ALA salts of the invention in photodynamic therapy (PDT).

The invention provides a method for preparing aluminum polychlorid from byproducts generated in methyl diethyl phosphate production. The method comprises the following steps: (1) dispersing byproductsolid dregs into a solvent, analyzing, and collecting a solution; (2) cooling the solution with water, and separating aluminum chloride hydrate crystal; (3) hydrolyzing and polymerizing the aluminum chloride hydrate crystal, and aging, thereby obtaining the aluminum polychlorid. By adopting the method, solid dregs rich in sodium tetrachloroaluminate are adopted as a raw material, an inorganic polymeric flocculant, namely the aluminum polychlorid, is successfully prepared through steps of simple processes, and not only is the problem of waste disposal solved, but also a high additional value product can be successfully made.

The invention discloses a method for preparing a mimic enzyme molecularly imprinted polymer microsphere for hydrolyzing organophosphorus. A paraoxon transient state analogue (4-nitro benzyl) phosphoric acid diethyl ester serves as a template molecule, 1-vinyl imidazole and methacrylic acid are functional monomers, a molecular imprinting technology is used, a precipitation polymerization method is adopted, and therefore the mimic enzyme molecularly imprinted polymer microsphere for hydrolyzing the organophosphorus is prepared, wherein the mimic enzyme molecularly imprinted polymer microsphere for hydrolyzing the organophosphorus is good in dispersibility and uniform in particle size. The paraoxon hydrolytic enzyme activity of the prepared molecularly imprinted polymer microsphere and the paraoxon spontaneous hydrolyzing are compared, the hydrolyzing efficiency can be improved by 188 times to the maximum and is also improved by 2.3 times compared with the catalyzing efficiency of a non-imprinted polymer synthesized under the condition of not adding template molecules, a measured Km value and a measured Vmax value are 0.064 mmol/L min and 2.41 mmol/L respectively, and Kcat is 0.237/S. The prepared mimic enzyme molecularly imprinted polymer microsphere for hydrolyzing the organophosphorus can be used for efficiently hydrolyzing organophosphorus pesticide and can also be used for degrading and destroying organophosphorus nervous toxic agent chemical weapons.

Belonging to the technical field of medicine synthesis, the invention relates to a method for synthesis of PMPA by combining a biological technique and a chemical technique. The method comprises: taking chlorinated acetone as a starting raw material, conducting yeast fermentation reduction so as to obtain chiral chloropropanol (I), then subjecting the chiral chloropropanol (I) and diethyl p-toluenesulfonyloxyphosphonate to a condensation reaction under the action of alkali so as to obtain a reaction intermediate (II); preparing R-9-(2-hydroxypropyl)adenine (III) from adenine and the reaction intermediate (II); and hydrolyzing the obtained R-9[2-(diethylphosphonomethoxy)propyl]purine, thus obtaining the PMPA (IV). The method combines the biological technique and the chemical technique and obtains a key chiral alcohol by means of a biological means, i.e. fermentation. The method has the characteristics of short reaction process, short reaction time, high mass yield, and can produce products with good quality, thus being suitable for industrialized production.

The invention discloses a preparation method of baricitinib and belongs to the technical field of drug preparation. The method comprises that 4-chloropyrrolopyrimidine as a starting raw material is subjected to amino protection, the product, hydrazine hydrate and acrolein undergo a one-pot displacement reaction and a cyclization reaction to produce an intermediate 4, a starting raw material 1, 3-dibromoacetone and ethylene glycol undergo a condensation reaction to produce an intermediate 5, the intermediate 5 and ethyl sulfonamide undergo a condensation reaction to produce an intermediate 6, the intermediate 6 and diethyl cyanomethylphosphonate undergo a reaction under action of a strong base to produce an intermediate 7, the intermediate 4 and the intermediate 7 undergo an addition reaction under the action of a catalyst, and the product undergoes a deprotection reaction to produce a desired product 1. The preparation method needs mild reaction conditions. The intermediate purification method is simple and easy, has a total yield of 40-55% and is suitable for industrial production.

The invention discloses an organophosphorus active flame-proof epoxide resin solidifying agent amino phosphonate ester and the preparing method. The amino phosphonate ester comprises the following parts: 3:1:1:1 absolute ethyl alcohol, phsophorus trichloride, organic amine (the structural formula is H2N-R-NH2)and acetone. The organic amine is diethylenetriamine, triethylene tetraamine, tetraethylene pentamine or 4, 4-diaminodiphenylmethane. The method comprises the following steps: 1, synthesizing diethyl phosphate with alcohol and phsophorus trichloride; 2, generating ketoimine with acetone and the organic amine by adding the anhydrating agent; 3, generating amino phosphonate with diethyl phosphate and ketoimine. The oxygen index of the product is more than 20 and less than 34.6. The invention is provided with the simple method and the simple operation.

An industrial production process of tenofovir, the production process steps are as follows: add R-1,2-propylene glycol, diethyl carbonate and sodium ethylate into the reaction kettle; add absolute ethanol and diphosphite Ethyl ester, stirring, after the stirring is completed, put in paraformaldehyde and triethylamine, after the reaction is complete, add anhydrous sodium sulfate, dry, filter, and distill out, the distilled product is diethyl p-toluenesulfonyloxymethylphosphonate Fine product; add adenine, R-propylene carbonate, DMF and NaOH in the reaction kettle, after the reaction is complete, add magnesium tert-butoxide, drop diethyl p-toluenesulfonyl phosphate, after the reaction is complete, add acetic acid, Concentrate under reduced pressure, add hydrochloric acid, filter, filter out the solid and dry under normal pressure to obtain PMPA fine product. The method has the advantages of high yield, high product purity and low impurity content, and can be fully industrialized.

The invention discloses a method for continuously synthesizing diethyl phosphite in a microchannel reactor, and belongs to the technical field of organic synthesis processes. More specifically, the method is a method for generating diethyl phosphite by a continuous reaction in a microchannel continuous flow reactor using anhydrous ethanol and phosphorus trichloride as a substrate and chloroform asa solvent, wherein the mixed solution of the chloroform and the phosphorus trichloride is a material A, the anhydrous ethanol solution is a material B, and the material A and the material B simultaneously enter a microchannel through a metering pump. According to the method, the efficient mass transfer and heat transfer efficiency of the microchannel reactor are utilized to effectively strengthenthe mass transfer rate between two-phase materials, and the safety and operability of an experiment are greatly improved.

The invention discloses a method for recovering useful constituents such as tetrahydrofuran, methyl diethyl phosphate, triethyl phosphate and trimethylbenzene in a mixed waste solvent during a process of producing glufosinate ammonium by an integrated rectification process. The method comprises the following steps: using an integrated rectification process of discharging and rectifying in a single-tower side line and then connecting a single tower to rectify, directly extracting tetrahydrofuran from the top of the rectification tower in the side line and obtaining trimethylbenzene from the bottom of the tower; extracting the mixed solution of methyl diethyl phosphate and triethyl phosphate from the side line simultaneously, conveying the mixed solution to the rectification tower and carrying out single-tower separation, thereby obtaining methyl diethyl phosphate from the top of the tower and obtaining triethyl phosphate from the bottom of the tower. According to the method disclosed by the invention, the useful constituents in the mixed waste solvent during the glufosinate ammonium production process are recovered by the integrated rectification process, the total recovery rate of the mixed solvent exceeds 98%, and the quality achieves reuse standards. Compared with the conventional three-tower rectification method, the equipment cost and energy consumption of the method disclosed by the invention are obviously lowered.

The invention discloses polyurethane foam with heat conductivity coefficient enhanced by hollow glass beads. The polyurethane foam is prepared from, by weight, 150-160 parts of diphenyl-methane-diisocyanate, 100-105 parts of propoxylated glycerin, 100-110 parts of castor oil, 5-6 parts of glycerol, 40-43 parts of diethyl phosphate, a proper amount of 1 mol/L sodium hydroxide solution, 13-15 parts of diatomite, 5-6 parts of distilled water, 2-3 parts of triethanolamine, 3-4 parts of dibutyltin dilaurate, 4-5 parts of polyacrylamide, 3-4 parts of ethoxylated lauryl alcohol sulfate, 6-7 parts of hollow glass beads, 20-23 parts of cyclohexane, 0.2-0.22 part of n-propylamine, 0.6-0.7 part of silane coupling agent KH550 and a proper amount of deionized water. The prepared foam can be foamed on the spot, has the characteristics of being uniform in foaming, high in cell density and low in heat conductivity coefficient, is used for sealing of a switch cabinet, and is high in binding strength, good in sealing and excellent in heat preservation performance.

The invention discloses a method for synthesizing a glufosinate ammonium salt. The method comprises the following steps that (1) methyldiethoxyphosphine and n-butanol are used as raw materials to produce an intermediate I by hydrolysis and transesterification; (2) the intermediate I is subjected to a free radical addition reaction with acrolein cyanohydrin acetate to form an intermediate II; (3) the intermediate II is subjected to an aminolysis reaction with ammonia gas to form a mixture of an intermediate III and an intermediate IV; (4) the intermediate III and the intermediate IV are subjected to acid hydrolysis with hydrochloric acid to form an intermediate V; and (5) the intermediate V is neutralized, purified and crystallized to obtain the glufosinate ammonium salt. The method does not need to use toxic raw materials, avoids the large-scale use of ammonia water and ammonium chloride, not only greatly reduces the safety hazard, but also reduces the quantity of by-products and the amount of waste water generated, and the environmental protection risk is greatly reduced; and the purification process is simple, the product content and the yield coefficient are obviously increased,and the method is suitable for industrial scale production.