19 results about "Dimethyl phosphite" patented technology

The invention relates to the technical field of organic synthesis, in particular to a trichlorfon production device and a trichlorfon production process, the device comprises a first-stage synthesis kettle, a first-stage synthesis kettle condenser, a second-stage synthesis kettle, a second-stage synthesis kettle condenser and a centrifugal machine; a trichloroacetaldehyde feeding hole, a dimethyl phosphite feeding hole and a precipitant feeding hole are formed in the top of the first-stage synthesis kettle, an overflow hole is formed in the upper part of the side wall of the first-stage synthesis kettle, and the top of the first-stage synthesis kettle is connected with a first-stage synthesis kettle condenser through a pipeline; the second-stage synthesis kettle is communicated with an overflow port of the first-stage synthesis kettle through an overflow pipe, and the top of the second-stage synthesis kettle is connected with a second-stage synthesis kettle condenser through a pipeline; and the centrifugal machine is communicated with an overflow port of the second-stage synthesis kettle through an overflow pipe. According to the invention, a continuous synthesis method is adopted, and solid trichlorfon is immediately precipitated and separated out by adding a precipitant; meanwhile, two stages of synthesis kettles are arranged, so that solid trichlorfon is precipitated and separated out more sufficiently while the reaction retention time is ensured, the trichlorfon content is greater than or equal to 98%, and the yield is greater than or equal to 90%.

This invention belongs to the field of inorganic nanoparticle technology, and discloses a silicon-phosphorus-containing inorganic nanoparticle, its preparation method, and its application. The silicon-phosphorus-containing inorganic nanoparticle is prepared from inorganic nanoparticles, a phosphorus-containing compound, and a silane coupling agent. The inorganic nanoparticles are selected from at least one of nano-ZrO2, nano-CaCO3, nano-SiO2, and nano-TiO2. The phosphorus-containing compound is selected from at least one of dimethyl phosphite, diethyl phosphite, and diphenyl phosphite. The silane coupling agent is selected from γ-glycidoxypropyltrimethoxysilane and / or γ-glycidoxypropyltriethoxysilane. The silicon-phosphorus-containing inorganic nanoparticles of this invention, due to surface modification, have significant steric hindrance, are not prone to aggregation, and can be well dispersed in a matrix. The inorganic nanoparticles contain silicon and phosphorus, and have a certain flame-retardant effect.

The application discloses modified cotton fabric and a preparation method and application thereof, and relates to the field of textile fabrics.In the preparation of the modified cotton fabric, chitosan is pretreated by 2-bromoisobutyryl bromide, then acrylic acid and methyl acrylate are grafted and polymerized by an atom transfer radical polymerization method to obtain pre-modified chitosan, then the pre-modified chitosan is sequentially reacted with oxalyl chloride and 4-hydroxybenzotriazole to prepare modified chitosan; cotton fabric is ultrasonically pretreated by a sodium dodecyl sulfate solution, then sequentially reacts with 6-chlorohexanoyl chloride and N,N-dimethylallylamine to prepare pre-modified cotton fabric, and finally, the pre-modified cotton fabric is reacted with a modified liquid prepared from modified chitosan, dimethyl phosphite and 1,4-butanediol to prepare the modified cotton fabric.The modified cotton fabric prepared by the application has excellent ultraviolet resistance, antibacterial property, wrinkle resistance and flame retardance.

The invention provides a method for reducing moisture of an addition liquid in glyphosate synthesis. The method comprises the following steps: carrying out a depolymerization reaction on paraformaldehyde and a catalyst A in methanol to obtain a depolymerization liquid; adding glycine, methanol and triethylamine into the depolymerization liquid for catalytic reaction to obtain addition liquid; trimethyl phosphite is added into the addition liquid, a hydrolysis reaction is carried out, and water in addition is consumed; after reacting for a period of time, supplementing dimethyl phosphite and triethylamine to obtain a condensation solution; and adding hydrochloric acid into the condensation liquid for acidolysis to remove chloromethane, hydrogen chloride, water or other light components, cooling, adding alkali to adjust pH, crystallizing, filtering and drying to obtain glyphosate. Hydrolyzate dimethyl phosphite and methanol can be applied to the next step of reaction, so that the consumption of dimethyl phosphite and methanol in the condensation reaction is reduced; the side reaction is reduced, the glyphosate yield is increased by 6% compared with that of the prior art, and the glyphosate content reaches 98.5% or above.

The invention relates to the technical field of chemical fertilizer anti-caking agents, and discloses an attapulgite-based chemical fertilizer anti-caking agent and a preparation method thereof.The preparation method specifically comprises the steps that urea, dimethyl phosphite, a formaldehyde aqueous solution, itaconic acid and tripotassium citrate serve as raw materials, and a Mannich reaction, a dehydration reaction and an esterification reaction are conducted in sequence to prepare an alkenyl nitrogen phosphorus potassium compound nutrition component; the preparation method comprises the following steps: carrying out ring-opening reaction on hydroxyl groups on the surface of attapulgite and epoxy groups in allyl glycidyl ether to prepare alkenylated attapulgite; the preparation method comprises the following steps: by taking alkenylated attapulgite and an alkenylated nitrogen-phosphorus-potassium compound nutrient component as main raw materials and N, N-methylenebisacrylamide as a cross-linking agent, preparing functionalized attapulgite by adopting a solution polymerization method under the action of an initiator; functionalized attapulgite and fatty alcohol-polyoxyethylene ether are used as raw materials and are mixed, ground and sieved to prepare the chemical fertilizer anti-caking agent. The fertilizer prepared by adding the chemical fertilizer anti-caking agent prepared by the invention shows excellent anti-caking performance.

Provided is a modified cellulose, a preparation method and application thereof. The modified cellulose includes a flame retardant cellulose ester film, and the preparation method includes: obtaining a homogeneous cellulose solution by adding a cellulose to an ionic liquid cosolvent system; obtaining a cellulose phosphite ester solution by adding dimethyl phosphite and a catalyst to the homogeneous cellulose solution for performing a transesterification; obtaining cellulose phosphite ester powder by regeneration solvent precipitation, washing, centrifugation, and drying of the cellulose phosphite ester solution; and obtaining the flame retardant cellulose ester film by evaporating solvent after dissolving the cellulose phosphite ester powder in dimethyl sulfoxide.

The application discloses a preparation method of an intrinsically flame-retardant high-elasticity styrene-acrylic emulsion, which comprises the following steps: preparing a phosphorus-nitrogen integrated functional compound by using glycine, polyformaldehyde and dimethyl phosphite as raw materials; performing acyl chloride modification on the phosphorus-nitrogen integrated functional compound by using sulfoxide chloride; preparing a high-flexibility flame-retardant monomer by reacting the acyl chloride modified phosphorus-nitrogen integrated functional compound with a phenolic hydroxyl cashew phenol; and finally preparing the flame-retardant high-elasticity styrene-acrylic emulsion by reacting the high-flexibility flame-retardant monomer, styrene, butyl acrylate and acrylic acid in a cationic etherified starch aqueous solution. The emulsion has the multiple advantages of flame retardation, high elasticity, soap-free, water resistance and the like, is green and environment-friendly, low in cost, and has a wide application value.

The invention belongs to the technical field of anion exchange membranes, and relates to a polyaryl piperidine or polyaryl quinine N-methylation reaction method. Dimethyl phosphite is adopted as a methylation reagent, and the method has the advantages of being low in cost, safe and simple in process. The preparation method comprises the following specific steps: (1) synthesizing a polyarylpiperidine / quinine polymer; (2) synthesizing and dispersing the prepared polyaryl piperidine / quinine polymer in an organic solvent, and methylating by taking dimethyl phosphite as a methylation reagent; the polyaryl piperidine quaternization polymer or the polyaryl quinine quaternization polymer is obtained.

The invention relates to the technical field of glyphosate production, and particularly discloses a synthesis method and application of a glyphosate intermediate, and during synthesis of the intermediate, the synthesis method comprises the following steps: S1, taking paraformaldehyde as a raw material, adding triethylamine and methanol, mixing, adding glycine, and heating until a solid is dissolved; s2, mixing the feed liquid obtained in the step S1 with dimethyl phosphite, then adding triethylamine to adjust the pH value, and carrying out heating reaction; s3, cooling the reaction liquid obtained in S2, adding a regulator which is weak acid or strong alkali weak acid salt, uniformly mixing, heating, and removing the solvent under negative pressure; and S4, cooling the feed liquid obtained in S3, adding hydrochloric acid, uniformly mixing, standing, crystallizing, filtering, washing, and drying to obtain the glyphosate intermediate. By synthesizing the intermediate, dynamic monitoring, real-time production guidance, yield improvement and cost reduction in the production process are facilitated.

The utility model discloses a low-energy-consumption system for synthesizing dimethyl phosphite, and belongs to the technical field of dimethyl phosphite synthesis. The low-energy-consumption system comprises a micro-channel reactor, a gas-liquid separation device, a normal-pressure tail gas washing tower and a vacuum deacidification device, the micro-channel reactor is connected with a methanol feeding pipe, and the micro-channel reactor is connected with a phosphorus trichloride feeding pipe; the micro-channel reactor is connected with the gas-liquid separation device, the gas-liquid separation device is connected with the normal-pressure tail gas washing tower, and the gas-liquid separation device is connected with the vacuum deacidification device; the vacuum deacidification device is connected with the vacuum tail gas washing tower; the vacuum deacidification device is connected with the dimethyl phosphite rectification system; a continuous path for synthesizing dimethyl phosphite is formed among the micro-channel reactor, the gas-liquid separation device, the vacuum deacidification device and the dimethyl phosphite rectification system. The low-energy-consumption system not only reduces the energy consumption, but also ensures the high efficiency and continuity of the related synthesis process, and can be well matched with the dimethyl phosphite synthesis process to meet the actual requirements.

The utility model discloses a negative-pressure treatment device for tail gas generated in dimethyl phosphite production. The negative-pressure treatment device comprises a vacuum part, a condensation part and an absorption treatment part, the vacuum part comprises a buffer tank A, a Roots vacuum pump unit and a buffer tank B, the buffer tank A is provided with a tail gas inlet A, a tail gas outlet A and a methanol collecting tank A, the tail gas outlet A is connected with the Roots vacuum pump unit through a gas inlet pipeline, the Roots vacuum pump unit is connected with the buffer tank B through a gas outlet pipeline, and the top of the buffer tank B is provided with a tail gas outlet B; a methanol collecting tank B is arranged at the bottom of the buffer tank B; the condensing part comprises a condenser and a methanol collecting tank C, the tail gas outlet B is connected with the condenser, and the lower end of the condenser is connected with the methanol collecting tank C; the absorption treatment part comprises a multi-stage water absorption tower and an alkali absorption tower, the condenser is connected with the multi-stage water absorption tower, the multi-stage water absorption tower is connected with the alkali absorption tower, and a tail gas output pipeline is arranged at the top of the alkali absorption tower; the device disclosed by the utility model has the advantages of low production cost, high recycling rate and good chloromethane product quality.

A fully-continuous flow synthesis method of glyphosate is provided, which is performed by using a fully-continuous system including a plurality of pumps, a micromixer, a plurality of microchannel reactors, a plurality of tubular reactors, two back pressure valves, a plurality of reaction vessels, and a plurality of continuous crystallizers. Paraformaldehyde is depolymerized in the presence of an organic base, and the resultant depolymerization product undergoes an addition reaction with glycine to yield N, N-dihydroxymethylglycine, which further undergoes esterification with dimethyl phosphite (added in two batches) to generate a glyphosate ester. The glyphosate ester is adjusted to be acidic, hydrolyzed, desolvated, neutralized with a base, and purified to obtain glyphosate.

This invention discloses a preparation process for a weather-resistant polyurethane coating material, relating to the field of coating material technology. In preparing the weather-resistant polyurethane coating material, sericite is pretreated and then reacted with cinnamaldehyde to obtain modified sericite; a high-efficiency flame retardant is prepared by reacting 3,5-diamino-1,2,4-triazole sequentially with p-methoxybenzaldehyde and dimethyl phosphite using a one-pot method; polytetrahydrofuran diol, benzoyl diols, and 4,4'-dicyclohexylmethane diisocyanate are polymerized to obtain polyurethane; the polyurethane, high-efficiency flame retardant, and modified sericite are mixed using DMF as a solvent to formulate a polyurethane coating, which is then dried to obtain the polyurethane coating material. The polyurethane coating material prepared by the process provided by this invention possesses the advantages of weather resistance, flame retardancy, and antibacterial properties.

The invention provides a synthesis method of glyphosate, which comprises the following steps: reacting glycine methyl ester hydrochloride with alkali in an organic solvent, and separating the generated product to obtain glycine methyl ester and salt; the method comprises the following steps: cyclizing glycine methyl ester and a formaldehyde solution under an alkaline condition to generate [1, 3, 5]-triazinane-1, 3, 5-trimethyl triacetate; the preparation method comprises the following steps: carrying out condensation reaction on [1, 3, 5]-triazinane-1, 3, 5-trimethyl triacetate and dimethyl phosphite to obtain a condensation solution; and carrying out acidolysis and crystallization on the condensation liquid to obtain glyphosate crystals. According to the technical scheme, during cyclization reaction, N atoms in glycine methyl ester can react with the same amount of formaldehyde to form a ring, the triazinane intermediate is generated, consumption of formaldehyde is greatly reduced, triethylamine is not introduced as a catalyst in the synthesis route any more, the environmental protection pressure is greatly reduced, and a new thought is provided for the glyphosate synthesis process.

Provided is a method for preparing a flame retardant cellulose ester film, and the method includes: obtaining a homogeneous cellulose solution by adding a cellulose to an ionic liquid cosolvent system; obtaining a cellulose phosphite ester solution by adding dimethyl phosphite and a catalyst to the homogeneous cellulose solution for performing a transesterification; obtaining cellulose phosphite ester powder by regeneration solvent precipitation, washing, centrifugation, and drying of the cellulose phosphite ester solution; and obtaining the flame retardant cellulose ester film by evaporating solvent after dissolving the cellulose phosphite ester powder in dimethyl sulfoxide.

The invention relates to the technical field of chemical engineering, and particularly discloses a method for improving glyphosate synthesis yield, which comprises the following steps: S1, carrying out depolymerization reaction by taking paraformaldehyde as a raw material, methanol as a solvent and anhydrous triethylamine as a catalyst to prepare a formaldehyde monomer and obtain a depolymerization solution, then adding glycine to carry out addition reaction to prepare N-hydroxymethyl glycine, and carrying out reduced pressure distillation to obtain N-hydroxymethyl glycine; an addition liquid is obtained; s2, carrying out reduced pressure distillation treatment on the addition liquid until the volume of the addition liquid is reduced by 25-45%; and S3, detecting the contents of methanol and triethylamine in the liquid obtained in S2, supplementing anhydrous triethylamine and absolute methanol, dropwise adding dimethyl phosphite, carrying out a reaction, and finally carrying out acidification, crystallization and separation post-treatment to obtain a glyphosate product. According to the method, reduced pressure distillation is introduced after depolymerization and addition, water is efficiently removed by utilizing the multi-element azeotropic characteristic of methanol-water-triethylamine, and meanwhile, a drying reagent is accurately supplemented, so that dual stabilization of the water content of a system and the concentration of a catalyst is realized, and the hydrolysis loss of dimethyl phosphite is reduced.

The invention discloses a resourceful treatment method and a control system for wastewater generated in production of dimethyl phosphite, and relates to the technical field of resourceful utilization of wastewater generated in production of dimethyl phosphite. The method at least comprises one of the following steps: a, carrying out oil-water separation treatment on vacuum pump wastewater generated in a deacidification section in dimethyl phosphite production, and after an oil phase is separated out, treating a gas phase generated in dimethyl phosphite production by using the remaining water phase; and b, using the vacuum pump wastewater generated in a rectification section in dimethyl phosphite production to treat a gas phase generated in dimethyl phosphite production, and meanwhile, providing a system suitable for the method, so that the wastewater treatment cost is remarkably reduced.

The invention relates to the technical field of heat-shrinkable sleeves, and discloses a heat-shrinkable sleeve material for new energy and a preparation method thereof.The heat-shrinkable sleeve achieves wear-resistant and flame-retardant effects by adding a modification enhancer and a silicon-phosphorus synergistic flame retardant into a polyethylene matrix, the modification enhancer is prepared by grafting tannin on the surface of kaolin, and the modification enhancer is prepared by grafting tannin on the surface of kaolin. Kaolin is high in hardness, grafted tannin can improve dispersity, tannin is combined with the compatilizer in the extrusion process, the interface bonding force of the tannin and the compatilizer is enhanced, the mechanical property of polyethylene is improved, and meanwhile tannin has the antibacterial property; hydroxyl-terminated dimethyl methyl vinyl (siloxane and polysiloxane) and dimethyl phosphite are introduced to a sodium alginate molecular chain to form a silicon-phosphorus synergistic flame retardant, a carbon layer and a silicon dioxide layer can be formed on the surface of the heat-shrinkable sleeve during combustion, and the carbon layer and the silicon dioxide layer synergistically play a role in isolating oxygen and a heat source to prevent further combustion.

The invention relates to a method for feeding dimethyl phosphite by adopting a microchannel reactor, a process system comprises a microchannel reaction unit, a primary deacidification treatment unit and a post-system treatment unit, a methanol material inlet and a phosphorus trichloride material inlet are respectively arranged on two branch channels at one end of a microchannel, the other end of the microchannel is a product outlet, and the other end of the microchannel is a product outlet. The product outlet is connected with a top feed port of a first-stage deacidification kettle of the first-stage deacidification treatment unit through a pipeline, a bottom discharge port of the first-stage deacidification kettle is connected with a rear system, a heat-conducting medium cavity is formed among an upper heat-insulating plate, a lower heat-insulating plate and a shell, the upper heat-insulating plate is provided with a heat-conducting medium inlet, and the lower heat-insulating plate is provided with a heat-conducting medium outlet; the technological process comprises the following steps: S1, conveying methanol and phosphorus trichloride raw materials; s2, carrying out a reaction between the materials; s3, carrying out deacidification treatment; s4, purifying the dimethyl phosphite; through the advantages of the micro-channel reactor, the reaction efficiency and the product purity are improved, side reactions are reduced, and the method has a good industrial application prospect.