126 results about "Dimethyl phosphite" patented technology

The invention relates to a cyclic production method of glyphosate, belonging to the technical field of pesticide production techniques. The production method comprises steps as follows: the raw material dimethyl phosphite is subjected to an alkyl ester method to obtain glyphosate and a glyphosate mother solution; the glyphosate mother solution is treated to obtain a secondary alkali mother solution; the secondary alkali mother solution is subjected to catalytic preoxidation, high-temperature high-pressure air electrocatalytic degradation and liquid membrane extraction to obtain a liquid membrane concentrated solution and a saliferous liquid membrane diluted solution; the liquid membrane concentrated solution is subjected to active carbon decoloration, concentration by evaporation, and high temperature polymerization to obtain sodium tripolyphosphate; the saliferous liquid membrane diluted solution is filtered by a nanofiltration membrane to obtain a membrane concentrated solution and a membrane diluted solution; the membrane concentrated solution returns to the catalytic preoxidation step to be recovered; the membrane diluted solution enters an MVR (mechanical vapor recompression) system to be subjected to concentration by evaporation, thereby obtaining sodium chloride crystal, distilled water and a mother solution; and the sodium chloride crystal, distilled water and mother solution are respectively utilized. The invention lowers the production cost, enhances the utilization ratio of the product, reduces the discharge of waste liquor in the glyphosate production procedure, is environment-friendly, and has obvious comprehensive economic benefit and social benefit.

A Si-contained phosphonate as fire retarding agent used for fabrics is prepared through proportionally mixing methylvinyl dichlorosilane with solvent, stirring, adding dimethyl phosphite and catalyst, stirring under protection of N2, heating, reflux, collecting fraction, cooling, adding water, stirring, oil-water separating, and distilling water phase to obtain fire retarding agent SP.

The invention discloses a recovery method of monochloro methane, which comprises the following steps: washing tail gas which is generated in the preparation process of glyphosate acid or dimethyl phosphite, adsorbing through a molecular sieve, and condensing, wherein the adsorption temperature of the molecular sieve is 10-50 DEG C. The method disclosed by the invention effectively overcomes the defects that waste acid can be generated and an organic solvent is used in the existing technique for purifying and recovering monochloro methane. In addition, the molecular sieve selected in the invention can effectively adsorb methylal, thereby reducing a great deal of washing water and effectively relieving the pressure on environmental protection. The invention has favorable economic benefit and environmental benefit, avoids the trouble of filling concentrated sulfuric acid, lowers the cost, avoids the generation of the waste sulfuric acid, and solves the problems of emission and treatment of the waste sulfuric acid, thereby realizing environmental-protection production in deed; and meanwhile, the invention can effectively enhance the adsorption efficiency of the molecular sieve, and lower the energy consumption and production cost.

The invention relates to a novel process for producing 2-phosphonobutane-1,2,4-tricarboxylic acid co-production methyl chloride. The process comprises the following steps: firstly, putting dimethyl maleate and dimethyl phosphite in a reaction kettle, and dripping sodium methoxide to prepare a semi-finished phosphono succinic acid tetramethylester; then adding methyl acrylate in the semi-finished phosphono succinic acid tetramethylester; cooling and dripping sodium methoxide to obtain a midbody 2-phosphonobutane-1,2,4-tricarboxylic acid pentamethyl ester; leading chlorine hydride gas into the midbody; carrying out circumfluence for hours to obtain a finished product 2-phosphonobutane-1,2,4-tricarboxylic acid; opening a methyl chloride recovering device to recover methyl chloride; discharging methyl chloride gas into a gas cabinet through a vacuum pump, and then discharging the methyl chloride gas after being dried to a condenser through a methyl chloride compressor; and finally, collecting liquid methyl chloride in a methyl chloride storage tank for standby selling. The process conforms to the environment protection requirement, can maximize the benefit of hydrochloric acid with low added value, obtains the methylated chemical product, i.e. the methyl chloride, and can reduce the cost and save energy.

The invention discloses a method for recycling methyl chloride in tail gas emitted by glyphosate/ dimethyl phosphite production, wherein, after gas-liquid separation, condensation, bathing, alkali cleaning, and drying are carried out on tail gas from the production technology of glyphosate/ dimethyl phosphite, arid methyl chloride is compressed by a compressor and then copiously cooled to obtain methyl chloride; partial non-condensable gas unable to be absorbed through a freezing method is fed in the compressor through methyl chloride filtered by an organic vapor membrane to be compressed again; the rest gas is discharged to the upper air. The method for recycling methyl chloride in tail gas emitted by glyphosate/ dimethyl phosphate production has the advantages that through the technology of combined copious cooling and organic vapor membrane recycling, the adoption of a DCS automatic air supply balanced system, and the core of a novel ripple packing tower, multi-level bathing, alkali cleaning, absorbing, and drying are carried out for repeatedly recycling methyl chloride gas, thus solving the problems of numerous gas production and unstable gas production of recycled methyl chloride, guaranteeing stable running of equipment, improving productivity effect, and improving recovery rate of methyl chloride from 93 percent to more than 99.5 percent; and environmental benefits and economic benefits are outstanding.

The invention discloses a preparation method of a retanned intumescent flame retardant, which comprises the following steps: adding a catalyst into dimethyl phosphite, evenly mixing, adding acrylamide, acrylonitrile and maleic anhydride for reaction, and obtaining colorless transparent liquid A; using alkaline solution for regulating the pH of the transparent liquid A to 5-7, dripping glyoxal, and carrying out reaction for obtaining light yellow liquid B; and adding melamine into the light yellow liquid B for reaction, and obtaining reddish brown retanned intumescent flame retardant C. A product synthesized by the preparation method not only has good flame resistance, which can lead leather to achieve the difficult-flammability by adding 3% of the weight of the leather of the product, but also has good compatibility with the leather, thereby improving the hand feel, the fullness, the softness and the mechanical performances of the leather.

The embodiment of the invention discloses a method for preparing N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide, which comprises the following steps of: leading acrylamide, dimethyl phosphite and a catalyst to react in a solvent to obtain dimethyl (3-amino-3-acyl propyl) phosphonate, wherein the catalyst is a nonacid compound of alkaline earth metal; leading dimethyl (3-amino-3-acyl propyl) phosphonate to react with formaldehyde to obtain the N-hydroxymethyl-3-(dimethoxyphosphoryl) propionamide. In the invention, the nonacid compound of alkaline earth metal is used as the catalyst. Because the nonacid compound of alkaline earth metal is solid matter, the reactants including acrylamide and dimethyl phosphite can be in good contact with the solid catalyst. Meanwhile, the surface of the solid catalyst has high catalyst concentration to ensure that the catalyst is easy to initiate the reaction. Thus, the preparation method provided by the invention ensures short reaction time and high reaction efficiency.

The invention discloses a method for preparing glyphosate preparation with 30 to 70 percent of effective ingredient by glyphosate mother liquid. The method comprises the following steps that: mother liquid containing 1 to 4 percent of glyphosate in production of the glyphosate is prepared by a dimethyl phosphite method, and enters a primary film separation device to separate light mother liquid and extract mother liquid, wherein the extract mother liquid contains 5 to 10 percent of the glyphosate, and has salt concentration less than 2.0 percent; the light mother liquid enters a secondary film separation device to separate thick mother liquid and secondary light mother liquid, and the thick mother liquid returns to the inlet of the primary film separation device; after the extract mother liquid is subjected to pretreatment, the extract mother liquid is added with glyphosate raw powder, accessory ingredient and ammonia (or one of isopropylamine, potassium hydroxide and potassium carbonate) to be prepared into 30 to 70 percent glyphosate preparation; the secondary light mother liquid is subjected to multieffect evaporation concentration, crystallization, centrifugal separation and dry recovery of a byproduct NaCl; and after the separated mother liquid is oxidized, the mother liquid is added with calcium hydroxide to remove phosphor and precipitate calcium phosphate. The method prepares the glyphosate preparation over 30 percent by the glyphosate mother liquid, recovers the byproduct in the mother liquid, and greatly reduces treatment amount of wastewater producing the glyphosate.

The invention relates to a durable flame-retardant finish method for a cotton fabric based on ultraviolet light curing reaction. The method comprises the following steps: washing a cotton fabric, then putting into an acidic 1-5wt% thiohydroxy-containing silane coupling agent solution, dipping to perform thiohydroxy modification, and drying to obtain a thiohydroxy modified cotton fabric; (2) taking 1,3,5-triacryloylhexahydro-1,3,5-triazine TAHT and dimethyl phosphite DP, adding 1,8-diazabicycloundec-7-ene DBU, and reacting over night while stirring to obtain flame retardant DHTP; and (3) preparing the flame retardant DHTP in the step (2) into a solution, dipping the thiohydroxy modified cotton fabric in the step (1) in the DHTP solution to perform ultraviolet light curing reaction, washing with water, and drying to obtain a flame-retardant cotton fabric. The method provided by the invention is simple and easy to implement; the cotton fabric can keep the original moisture absorption property and other excellent properties; and the cotton fabric is endowed with flame retardancy while the durability is improved, has the advantages of obvious flame-retardant effect, safety and long-lasting action, and can not do harm to human bodies and environments, thereby having favorable application prospects.

The invention provides a method and a device for applying dimethyl phosphite hydrogen chloride tail gas to synthesis of glyphosate. The method comprises the following steps: conveying dimethyl phosphite tail gas into a compressor through a pipeline, and carrying out primary pressurized condensation to obtain a high-boiling-point alcohol water solution and non-condensable gas; carrying out cryogenic treatment on the non-condensable gas in a secondary pressurized condenser, separating the product to obtain hydrogen chloride gas, and storing the hydrogen chloride gas in a hydrogen chloride gas cabinet; carrying out an acidolysis reaction on the hydrogen chloride gas and the synthesis liquid in a hydrolysis kettle, then carrying out heating desolvation and deacidification and feeding the product into a cooling crystallization process; and then carrying out solid-liquid separation through a washing device, and finally drying the product to obtain the glyphosate raw medicine. According to the method, the hydrogen chloride and the methyl chloride are separated through pressurization and condensation, then the methyl chloride enters a refining procedure, and the separated hydrogen chlorideis applied to the glyphosate production mode, so that the introduction of water in a reaction system can be reduced, the steam consumption during solvent recovery is reduced, and the wastewater amount is reduced. The water for glyphosate production is reduced, the wastewater treatment and energy consumption are reduced at the same time, and the economic and environmental benefits are remarkable.

The new process of preparing N-phosphonomethyl iminodiacetic acid (NPMIDA) as the intermediate for synthesizing glyphosate features the materials including alkyl phosphite and/or C1-C4 formaldehyde alcohol. Especially, the residual liquid produced in the dimethyl phosphite producing process and acetal produced in dimethyl phosphite process of producing glyphosate are used. In the same time, chloromethane for synthesizing methyl chlorosilane may be obtained.

The invention relates to an anionic fluorocarbon surfactant and a preparation method thereof. The structural formula of the anionic fluorocarbon surfactant is as follows: CF3CF2CF2C(CF3)2CH2C6H4PO(OM)2, wherein M is equal to Li, Na, K or NH4. The preparation method comprises the following steps: (1) reacting hexafluoropropylene dimer and p-Bromobenzyl bromide to generate a fluorine-containing intermediate compound 1; (2) coupling the fluorine-containing intermediate compound 1 with dimethyl phosphite to obtain a fluorine-containing intermediate compound 2; (3) hydrolyzing the fluorine-containing intermediate compound 2 to generate a fluorine-containing organic acid 3; and (4) neutralizing the fluorine-containing organic acid 3 with alkali to obtain a product. The method has the advantages of being, simple, low in cost and good in repeatability, and raw materials can be easily obtained. The surface tension performance of the product is good.

The invention discloses fireproof emulsion paint. The fireproof emulsion paint comprises acrylic acid emulsion, polyurethane emulsion, epoxy resin, a fire retardant, expanded perlite, titanium dioxide, nanometer silica sol, silicon powder, nanometer titanium dioxide, zinc trifluoroacetylacetonate, dodecafluoroheptyl methacrylate, a film forming auxiliary agent, sorbitan monopalmitate, lauric acid, an antifoaming agent, hydroxyethyl cellulose, methyl ethyl ketone, N-phenyl-N'-cyclohexyl p-phenylenediamine, potassium citrate, dimethyldiallylammonium chloride and water. The fire retardant comprises dimethyl phosphite, methylvinyldichlorosilane, 3-aminopropyltriethoxysilane, 5-ethyl-5-butyl-2-chloro-1,3,2-dioxaphosphorinane, potassium tripolyphosphate, cetyl pyridinium bromide, decabromodiphenyl ethane, aluminum dihydrogen phosphate, calcium borate, melamine and cyanuric acid. The fireproof emulsion paint has excellent flame resistance, good fire retardancy, good adhesion to a base material and good decorative effects.

The invention discloses a flame-retardant finishing agent and a use thereof. The flame-retardant finishing agent comprises, by weight, 30-60 parts of a boric acid derivative, 5-10 parts of a phosphorus-containing compound, 1-3 parts of melamine, 1-2 parts of a non-ionic osmotic agent and 200 parts of water. The boric acid derivative is one of 2-chlorophenylboronic acid, 3-chlorophenylboronic acid, 4-chlorophenylboronic acid, 3-bromophenylboronic acid and 4-bromophenylboronic acid. The phosphorus-containing compound is one of ammonium dihydrogen phosphate, dimethyl phosphite, monopotassium phosphate and monocalcium phosphate. The flame-retardant finishing agent is prepared from the boric acid derivative as a main raw material, the flame-retardant finishing agent is used for treating a textile so that a high flame resistance textile is obtained, and the high flame resistance textile has good flame resistance and outstanding flame retardation endurance and thus the flame-retardant finishing agent has a wide application prospect in a high flame retardation requirement material such as an outdoor tent.

The invention relates to a synthesis method of glyphosate, which comprises the following steps: (1) respectively pouring paraformaldehyde, methanol and triethylamine into a reaction kettle, controlling the temperature of the reaction kettle to be 30-50 DEG C, and reacting for 0.5-2h under stirring; (2) adding glycine into the reaction kettle, controlling the temperature of the reaction kettle to be 30-50 DEG C, and reacting for 0.5-2h under stirring; (3) adding dimethyl phosphite into the reaction kettle, controlling the temperature of the reaction kettle to be 55-65 DEG C, and reacting for 0.5-1.5h under stirring; (4) controlling the temperature of the reaction kettle to be 40-50 DEG C, adding hydrochloric acid into the reaction kettle, increasing the temperature of the reaction kettle to be 110-135 DEG C, and preserving the temperature and precipitating for 1-2h; and (5) after heat preservation and precipitating, cooling, crystallizing, carrying out suction filtration, and then, drying to obtain glyphosate raw powder. By increasing the temperature of condensation reaction, the invention shortens the synthesis time of the glyphosate and improves the yield of the glyphosate; and the obtained glyphosate raw powder has larger particles.

The invention provides a recovery method of a rectification residual liquid of dimethyl phosphite. The preparation process comprises steps as follows: methanol and phosphorus trichloride are sprayed to an esterification reaction kettle slowly; a proper amount of ammonia is added to crude dimethyl phosphite in a neutralization tank slowly for neutralization; materials in the neutralization tank are sent to a rectifying tower to be rectified, dimethyl phosphite is completely distilled off, and a rectification residual liquid of dimethyl phosphite is left; the rectification residual liquid of dimethyl phosphite is transferred to a reaction kettle; the rectification residual liquid is subjected to activated carbon decoloration; the decolored liquid is filtered; a proper amount of hydrochloric acid is dropwise added to the filtered liquid, the mixture is sufficiently stirred until acidolysis is sufficient; tail gas generated in the acidolysis process is sent to a chloromethane recovery pipeline in a workshop; after acidolysis is finished, a phosphorous acid water solution in the kettle is concentrated and crystalized. Clean production is realized, discharge of three wastes is reduced, the recovery rate of byproducts is increased, and the production cost is reduced.

The invention provides a production process of dimethyl phosphite, and its preparation process is as follows: first, methanol and phosphorus trichloride are sprayed into the esterification reaction kettle slowly and relatively in the form of mist, and at the same time, the upper half of the reaction kettle is filled with Nitrogen, the reaction is exothermic, and the condenser is used to condense. After the reaction is completed, the solid in the esterification reactor is crude dimethyl phosphite; secondly, slowly spray the crude dimethyl phosphite in the neutralization tank into atomized ammonia For neutralization, the material in the neutralization tank is a mixture of dimethyl phosphite and ammonium chloride; the material in the neutralization tank is sent to the rectification tower for rectification, all of which are distilled out, and the remaining rectification residue of dimethyl phosphite liquid; finally, the rectification raffinate is filtered through molecular sieves, and then the rectification raffinate is rectified. The invention can improve the purity of dimethyl phosphite, so that the purity of dimethyl phosphite is 95.6%.

The invention provides a technology for recovering chloromethane washing wastewater in glyphosate production. The technology comprises the following steps: paraformaldehyde and dimethyl phosphite are subjected to a condensation reaction under the actions of methyl alcohol and trimethylamine; glyphosphonic acid is generated under the action of hydrochloric acid, and a large amount of tail gas containing chloromethane is produced; the tail gas is washed through a water scrubber, and gas after washing is processed through a carbon tetrachloride absorption tower; wastewater after washing is transferred into a distillation tower, the temperature is increased to 58 DEG C, and evaporated gas is collected and cooled to 20 DEG C for storage; the distillation tower is heated to 75 DEG C, and evaporated gas is collected and cooled to 15 DEG C for storage. With adoption of the technology, the chloromethane washing wastewater is subjected to recovery treatment, so that consumption of methyl alcohol in production can be reduced, and the production cost can be saved.