61 results about "Dimethyl phosphite" patented technology

The invention discloses a preparation method of an intrinsically flame-retardant and toughened polystyrene copolymer. The preparation method comprises the following steps: firstly, preparing a phosphorus-nitrogen integrated functional compound from glycine, paraformaldehyde and dimethyl phosphite as raw materials; then carrying out acylating chlorination modification on the phosphorus-nitrogen integrated functional compound by using thionyl chloride; reacting the phosphorus-nitrogen integrated functional compound modified by acylating chlorination with phenolic hydroxyl cardanol to prepare a high-flexibility flame-retardant monomer; and finally, reacting the high-flexibility flame-retardant monomer with styrene to obtain the polystyrene copolymer. The copolymer has the dual advantages of flame retardance and toughening at the same time.

The invention belongs to the field of pesticide preparation, and particularly relates to an improved preparation method of 2-(2 '-bromomethyl phenyl)-2-carbonyl methyl acetate. 2-oxo-2-(o-tolyl) ethyl acetate is used as a raw material and is sequentially subjected to oximation reaction, structure transposition treatment, bromination reaction and polybrominated substance to monobromination reaction, and finally 2-(2 '-bromomethyl phenyl)-2-carbonyl methyl acetate is obtained. Wherein the structure transposition treatment comprises the following steps: by taking an oximation product as a substrate, introducing a catalyst under a system anhydrous condition to realize conversion from a Z configuration to an E configuration; the polybrominated substance to monobrominated product conversion reaction comprises the following steps: dissolving a brominated product in THF, then adding dimethyl phosphite and diisopropylethylamine, and carrying out a reaction to realize conversion of the polybrominated substance into a monobrominated product. According to the method, the conversion of polybrominated substance impurities into monobrominated products is optimized through process improvement, so that the yield of the target product is improved, and the method is simple to operate, few in by-products and suitable for industrial production.

The invention discloses a method for detecting specific pollutants in a pesticide production plot, which can simultaneously detect six specific pollutants including three organophosphorus pesticides including isocarbophos, isofenphos-methyl and profenofos. One pesticide degradation product is dimethyl phosphate; the intermediate product of one pesticide is dimethyl phosphite, and the production raw material of the other pesticide is dimethyl sulfate. The method comprises the following steps: carrying out freeze-drying and grinding on a soil sample, and sieving with a sieve with the aperture of 0.25 mm; uniformly stirring the soil sample and diatomite, and adding a substitute and an extracting agent for extraction treatment to obtain a sample extracting solution; carrying out dehydration treatment on the sample extracting solution; and performing concentration treatment on the sample extracting solution to obtain a to-be-detected sample solution containing six target objects. The method can be used for simultaneously detecting specific pollutants of 6 pesticide production plots, and the detection rate is high; by adding an interior label, the accuracy of the method is improved; and the qualification rate of sample detection is improved by adding a substitute.

The application discloses a platinum complex with controllable activity and a preparation method and application thereof, which is formed by coordination of vinyl siloxane, modified ligand and chloroplatinic acid; the modified ligand is prepared by reaction of maleic anhydride, allylamine and hydroxymethyl dimethyl phosphite. The application introduces amide groups and phosphite groups into the molecular chain of maleic anhydride, uses the groups as coordination compounds to coordinate with vinyl siloxane and platinum, and can improve the normal-temperature storage stability of the platinum catalyst while still keeping high catalytic activity of the platinum catalyst on the hydrosilylation reaction; when the platinum complex is used for catalyzing preparation of addition-type liquid silicone rubber, no inhibitor needs to be added, and the silicone rubber has good mechanical properties.

The invention relates to the technical field of organophosphorus flame retardant synthesis, and particularly discloses an organic polymer catalyst and a method for preparing a cyclic phosphate flame retardant by using the organic polymer catalyst, the organic polymer catalyst contains methyl benzenesulfonate and imidazole ion groups and has bifunctional catalytic sites, imidazole ions can catalyze Michaelis-Arbuzov rearrangement reaction, and the molecular weight of the imidazole ions can be reduced to a certain degree. Methyl benzenesulfonate can catalyze isomerization of dimethyl phosphite, the organic polymer can be recycled through simple treatment after the catalytic reaction is completed, and high catalytic efficiency can still be obtained after the organic polymer is repeatedly used for multiple times.

The invention belongs to the technical field of electrochemical energy storage, and provides a manufacturing method of an electrolytic zinc-manganese aqueous secondary large battery, which comprises a method for preparing a manganese dioxide (MnO2) positive electrode through in-situ electrochemical deposition; according to the electrolytic MnO2-Zn battery based on the Mn < 2 + > / MnO2 chemistry, higher theoretical capacity, high discharge voltage and good cycle stability are achieved, the hydroxymethyl dimethyl phosphite is adopted as an electrolyte additive, the hydrogen evolution reaction and dendritic crystal growth of a zinc negative electrode are effectively inhibited, and the service life of the battery is prolonged. The chemical reaction kinetics of an electrode-electrolyte interface is also improved, so that the cycle life and the safety of the battery are greatly improved, and meanwhile, the manganese-based positive electrode material is structurally modified, so that the problems of unstable structure and insufficient conductivity of the positive electrode material in long-term circulation are solved; therefore, the battery can still maintain a stable voltage platform and a relatively high capacity retention ratio after 3000 times of charge-discharge cycles, and the service life of the battery is remarkably prolonged.

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 utility model discloses a dimethyl phosphite reaction device, which comprises an esterification kettle, a phosphorus trichloride feed pipe and a methanol feed pipe are inserted into the esterification kettle and are connected with a nozzle of a hedging reaction area, and a bottom discharge port of the hedging reaction area is connected with a mixed reaction area. The device has the beneficial effects that (1) two raw materials can be fully contacted through atomizing and spraying, so that the yield of dimethyl phosphite reaches more than 96%; (2) chloromethane gas and other gas phases can be separated from dimethyl phosphite through a gas-liquid separator, so that the generation of monomethyl phosphite and phosphorous acid is reduced; (3) a mixing element is arranged in the mixing reaction area, so that phosphorus trichloride which is not completely reacted can be rapidly mixed and reacted, and gas is discharged from an exhaust hole; (4) the method has the advantages that the materials can fully react, tail gas is quickly separated, and the esterification vacuum degree requirement can be reduced from-0.09 Mpa to-0.05 Mpa; and (5) the total retention time of the materials is short, backmixing is avoided, the total amount of reaction liquid held in unit time is small, and the safety is good.

The invention discloses a perovskite light-emitting diode based on a novel anti-solvent and a preparation method thereof, and belongs to the technical field of light-emitting diodes. The perovskite light-emitting layer is prepared by spin coating of a perovskite precursor solution; an anti-solvent is dropwise added in the spin-coating process; the anti-solvent is a mixture of ethyl acetate doped with dimethyl phosphite (DPP) in a volume ratio of (5: 1)-(40: 1). According to the invention, the selected S-A self-adaptive solvent gives consideration to the unique advantages of an EA anti-solvent and DPP molecules, regulates and controls the growth and orientation of the Q-2D perovskite crystal, and reduces the number of grain boundary defects; the formation of low n phases is inhibited, and the energy transfer efficiency among different n phases is improved; the defects of the Q-2D perovskite are passivated, and the non-radiative recombination loss is reduced. The EQEmax of the prepared PeLEDs reaches 29.27%, and a new view angle is provided for preparation of the high-performance PeLEDs.

The utility model discloses a dimethyl phosphite rectifying device which comprises a rectifying still, a rectifying tower, a condensing device and a distributor, wherein the rectifying still is provided with a dual-heating structure, the top of the rectifying still is connected with a crude ester feeding pipeline, the bottom of the rectifying still is connected with a residual liquid tank, and the upper part of the rectifying still is connected with the rectifying tower through a first gas phase pipeline; the top of the rectifying tower is connected with a condensing device through a second gas phase pipeline, a condensate extraction pipeline is connected below the condensing device and connected with a distributor, the distributor is connected with a backflow pipeline and a refined ester extraction pipeline, the backflow pipeline is connected with a rectifying tower body, and the refined ester extraction pipeline is connected with a transfer tank. The transfer tank is connected with a vacuum device and a finished product tank, and a refined ester content analysis device is arranged on the refined ester extraction pipeline; in general, the rectification device has the advantages of high rectification efficiency, good finished product quality, convenience in remote control and analysis, safety and convenience.

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%.

The invention relates to the technical field of pesticide production, in particular to a glyphosate technical production system, which comprises a phosphorus trichloride process, a dimethyl phosphite process and a glyphosate process, and specifically comprises the following steps: S1, introducing chlorine into a chlorination kettle filled with yellow phosphorus, controlling the reaction temperature to obtain gas-phase phosphorus trichloride, and removing phosphorus to obtain liquid-phase phosphorus trichloride; s2, methanol and liquid-phase phosphorus trichloride are introduced into an esterification kettle for an esterification reaction, an esterification reaction material and esterification tail gas are obtained, and dimethyl phosphite is obtained after deacidification; and S3, adding paraformaldehyde into the synthesis kettle, adding methanol and triethylamine, heating, sequentially adding glycine, dimethyl phosphite and the composite catalyst, stirring for reaction, and dealcoholizing to obtain the solid glyphosate. The purity and yield of glyphosate are remarkably improved by controlling the feeding proportion and reaction conditions of the raw materials and using the composite catalyst.

The utility model provides a continuous automatic temperature control device for a dimethyl phosphite deacidification process, which comprises a primary deacidification kettle connected with a secondary deacidification kettle through a discharge pipeline. The secondary deacidification kettle is connected with a crude ester receiver I and a crude ester receiver II through a discharging pipeline; a jacket is arranged on the outer side of the first-stage deacidification kettle and is connected with a steam header pipe; and a jacket is arranged on the outer side of the secondary deacidification kettle and is connected with the hot water collecting tank. The first-stage deacidification kettle is provided with a temperature monitoring device, a steam outlet pipeline connected with the bottom of the jacket is provided with a steam stop valve and a drain valve and is connected with the jacket on the outer side of the second-stage deacidification kettle, and the steam stop valve and the drain valve are interlocked with the temperature monitoring device of the second-stage deacidification kettle.

The invention discloses a preparation method of a high-flexibility flame-retardant monomer. The preparation method comprises the following steps: firstly, preparing a phosphorus-nitrogen integrated functional compound by taking glycine, paraformaldehyde and dimethyl phosphite as raw materials; then carrying out acylating chlorination modification on the phosphorus-nitrogen integrated functional compound by using thionyl chloride; and reacting the phosphorus-nitrogen integrated functional compound modified by acylating chlorination with phenolic hydroxyl cardanol to prepare the high-flexibility flame-retardant monomer. The flame-retardant monomer has good flexibility, the reaction process is simple, operation is convenient and safe, popularization and application are easy, and the flame-retardant monomer has good industrial application value.

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 present invention relates to the technical field of deacidification, and discloses a deacidification device used in a dimethyl phosphite production process, comprising a kettle body and a perfusion pipe, wherein the perfusion pipe is coaxially mounted on the upper portion of the kettle body. The present invention drives a driving member to move during rotation of a trigger member, and the driving member converts the translation into a driving force required for the rotation of a perfusion head, thereby driving the perfusion head to rotate so as to connect the inner cavities of the perfusion pipe and the injection pipe, so that the dimethyl phosphite entering the perfusion pipe passes through the perfusion head and enters the injection pipe, and then enters an atomizing device through the injection pipe, and the dimethyl phosphite is atomized by the high-speed rotation of the atomizing device. As the trigger member rotates at high speed, the driving member is cyclically squeezed, thereby achieving intermittent driving of the perfusion head to connect the inner cavities of the perfusion pipe and the injection pipe to achieve intermittent material discharge, thereby avoiding the dimethyl phosphite from being introduced too quickly, resulting in the dimethyl phosphite not being atomized in time in the atomizing device and overflowing.

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 utility model provides an automatic cleaning device for a dimethyl phosphite Roots vacuum unit. A clear water pipe (1) and a cleaning agent pipe (2) are connected with a mixing tank (3); the mixing tank (3) is connected with a roots vacuum pump unit (8); the Roots vacuum pump unit (8) comprises a Roots vacuum pump (4), a heat exchanger (5) and a storage tank (6) which are connected in sequence; the mixing tank (3) is connected with the Roots vacuum pump (4); and the tail end of the cleaning agent pipe (4) is inserted into the bottom of the mixing tank (3). The Roots vacuum unit is automatically cleaned in the production process of dimethyl phosphite, and process fluctuation, equipment failure or safety risks possibly caused by manual cleaning are eliminated, so that stable operation of a production device is guaranteed, and the safety risks in production are reduced.

In order to reduce the use amount of raw material methanol, improve the atom utilization rate and reduce byproduct chloromethane and the like, the invention discloses a process, a system and a control system for efficiently preparing dimethyl phosphite, and belongs to the technical field of synthesis of intermediate dimethyl phosphite of pesticide glyphosate. Wherein water and methanol are jointly used as raw materials (one molecule of water is used for replacing one molecule of methanol), the use amount of methanol is reduced, meanwhile, the byproduct chloromethane is greatly reduced, and the atom utilization rate is increased; a continuous flow reactor, a gas-liquid separator and the like are adopted, so that the whole reaction system is in a state from normal pressure to micro-positive pressure, the negative pressure state of a traditional kettle type continuous reactor is replaced, the reaction system does not need to use a vacuum pump, and the power consumption is greatly reduced; in addition, by controlling temperature, pressure, flow and the like, continuity, orderliness and controllability of the preparation process are guaranteed.

The present application relates to the field of the manufacturing of flame-retardant thin films, in particular to a method for preparing a flame-retardant cellulose ester thin film. Dimethyl phosphite, which acts as a flame-retardant monomer, is subjected to transesterification using 1,8-diazabicycloundec-7-ene as a catalyst in a 1-butyl-3-methylimidazolium chloride / dimethyl sulfoxide cosolvent system to synthesize a phosphite cellulose ester, and then, a phosphite cellulose ester thin film is prepared in dimethyl sulfoxide by means of solvent evaporation. The residual carbon rate of the prepared phosphite cellulose ester thin film is 30.4-33.7%. The operation process is simple, the cellulose solvent used is green and environmentally-friendly, the prepared cellulose ester can be applied to flame-retardant coatings, and the cellulose ester thin film can be applied to packaging materials, so that the problems of flammability, etc. of existing cellulose-based products are solved.

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 discloses a preparation method of an intrinsic flame-retardant high-elasticity styrene-acrylic emulsion. The preparation method comprises the following steps: firstly, preparing a phosphorus-nitrogen integrated functional compound by taking glycine, paraformaldehyde and dimethyl phosphite as raw materials; then carrying out acylating chlorination modification on the phosphorus-nitrogen integrated functional compound by using thionyl chloride; reacting the phosphorus-nitrogen integrated functional compound modified by acylating chlorination with phenolic hydroxyl cardanol to prepare a high-flexibility flame-retardant monomer; and finally, reacting a high-flexibility flame-retardant monomer, styrene, butyl acrylate and acrylic acid in the cationic etherified starch aqueous solution to prepare the flame-retardant high-elasticity styrene-acrylic emulsion. The emulsion has multiple advantages of flame retardance, high elasticity, no soap, water resistance and the like, is green and environment-friendly, is low in cost and has wide application value.

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.

The invention discloses a synthesis process of a glyphosate active compound, which belongs to the technical field of glyphosate synthesis, and comprises the following steps: adding paraformaldehyde and methanol into a synthesis kettle, uniformly stirring and mixing, adding a catalyst I, and carrying out depolymerization reaction; after the depolymerization reaction is finished, adding a catalyst II, preserving heat, fully stirring, and then adding glycine for addition reaction; after the reaction is completed, adding dimethyl phosphite to carry out condensation reaction; after the reaction is finished, pumping into a hydrolysis kettle, dropwise adding hydrochloric acid, heating with steam to evaporate methanol and methylal, then carrying out reflux reaction, evaporating hydrogen chloride under reduced pressure, and then adding water into the kettle; and finally, putting the material in the hydrolysis kettle into a crystallization kettle, cooling, standing, filtering and drying to obtain solid glyphosate. The introduced catalyst not only has a very good catalytic effect, improves the yield of a glyphosate active compound, shortens the glyphosate synthesis time and improves the production efficiency, but also can prevent the formation of glyphosine impurities and other impurities, improves the economic benefits, and is energy-saving and environment-friendly.

The utility model discloses a control system for preparing dimethyl phosphite. The control system comprises a DCS (Distributed Control System) controller, a phosphorus trichloride flowmeter and a phosphorus trichloride regulating valve which are arranged on a phosphorus trichloride inlet pipe, a water flowmeter and a water regulating valve which are arranged on a water inlet pipe, a methanol flowmeter and a methanol regulating valve which are arranged on a methanol inlet pipe, and a liquid level meter and a pressure transmitter which are arranged on a gas-liquid separator; the pressure regulating valve is arranged on the gas phase outlet pipe, the lower liquid regulating valve is arranged on the lower liquid pipe I, the motor is connected with the distributor, and the temperature sensor II is arranged on the jacket; the phosphorus trichloride flow meter, the phosphorus trichloride adjusting valve, the water flow meter, the water adjusting valve, the methanol flow meter, the methanol adjusting valve, the liquid level meter, the liquid discharging adjusting valve, the pressure transmitter, the pressure adjusting valve, the motor and the temperature sensor II are all connected with the DCS controller. The automation of the dimethyl phosphite preparation process is realized, and the stability, controllability and traceability of the dimethyl phosphite preparation process are ensured.

The invention relates to a continuous production process and device for dimethyl phosphite. The process comprises the following steps: (1) adding a backing material into a primary deacidification kettle; (2) connecting the bottom of the primary deacidification kettle into an inlet of a circulating pump, feeding methanol into the circulating flow reactor from an outlet of the circulating pump, and feeding phosphorus trichloride into the circulating flow reactor from an inlet of the circulating flow reactor; (3) a reaction product generated in the step (2) sequentially enters a first-stage deacidification kettle and a second-stage deacidification kettle; (4) carrying out two-stage deacidification to obtain dimethyl phosphite; wherein in the step (1), the base material is methanol and / or crude dimethyl phosphite. The circulating flow reactor is adopted, phosphorus trichloride is added from an inlet of the circulating flow reactor in proportion and rapidly reacts with methanol through the micro distributor, the production efficiency can be effectively improved, and the reaction is controlled to be carried out in a milder mode.

The invention discloses a method for recycling glyphosate technical from glyphosate mother liquor. The method comprises the following steps: S01, absorbing hydrochloric acid tail gas generated in the production process of dimethyl phosphite by taking the glyphosate mother liquor as an absorbent; s02, fully mixing the glyphosate mother liquor absorbing the hydrochloric acid tail gas with hydrochloric acid, and storing for later use; s03, fully mixing the mixed solution stored for later use with the condensation solution, then stirring and controlling the temperature at 30-40 DEG C; s04, carrying out heating hydrolysis on the temperature-controlled mixed solution, and ensuring that the mass concentration of sodium chloride salt in hydrolysate is 5-8% after the hydrolysis reaction is finished; and S05, then carrying out cooling crystallization, and when the temperature is lower than 40 DEG C, separating the glyphosate mother liquor to obtain a glyphosate raw medicine wet product. According to the method, the glyphosate dissolved in the glyphosate mother liquor can be effectively recovered, and the yield of the glyphosate is increased.

The invention relates to the field of preparation of azamethiphos, and particularly discloses a method for preparing azamethiphos by a one-pot method, which comprises the following steps: S1, reacting sulfur with dimethyl phosphite to generate O, O-dimethyl phosphorothioate; s2, enabling the O, O-dimethyl phosphorothioate to react with bromoiodomethane or chloroiodomethane to generate S-(halomethyl) O, O-dimethyl phosphorothioate; s3, S-(halomethyl) O, O-dimethyl phosphorothioate and 6-chloro-oxazole [4, 5-b] pyridine-2 (3H) ketone react to generate azamethiphos, and the total yield of the target product reaches up to 80%. The synthesis process of the azamethiphos is short in reaction time, does not need to replace a container, does not need to filter, wash and distill to remove impurities in the midway, simplifies the production process, reduces the workload and time cost, and improves the production efficiency; the equipment cost and the site cost are reduced, so that the method for preparing the azamethiphos in the scheme is more suitable for industrial production.

The utility model discloses a deacidification device for producing dimethyl phosphite. The deacidification device comprises a deacidification kettle, a condensing device and an analysis and determination device, a servo variable frequency motor, a feeding port, a backflow port, a vacuum port, an on-line thermometer, an on-line vacuum meter, a radar liquid level meter, a searchlight and a sight glass are arranged on a kettle cover of the deacidification kettle, the on-line liquid level meter, a circulating water interlayer, a stirrer and a discharging port are arranged on a kettle body, and the feeding port and the discharging port are communicated with a feeding pipeline and a discharging pipeline through an on-line flowmeter and an electromagnetic valve respectively. The vacuum port communicates with a vacuum pipeline; the condensing device is arranged above the deacidification kettle and comprises two condensers which are connected in series, one condenser is connected with a vacuum pipeline, the other condenser is used for discharging condensed gas, and a condensate outlet is connected with the reflux inlet; the analyzing and measuring device comprises a crude ester content acidity measuring device A mounted on the feeding pipeline and a crude ester content acidity measuring device B mounted on the kettle cover; the device disclosed by the utility model has the advantages of high working efficiency, low product acidity, high production yield and high automation degree.

The invention discloses a bio-based polymer composite board and a preparation method thereof, and relates to the technical field of polymer materials. When the bio-based polymer composite board is prepared, 1, 3, 5, 7-tetramethylcyclotetrasiloxane reacts with 1, 3-bis (3-carboxyl propyl) tetramethyldisilane to prepare a carboxyl-terminated siloxane oligomer, and then the carboxyl-terminated siloxane oligomer, terephthalic acid and ethylene glycol are subjected to condensation polymerization to prepare organic silicon polyethylene glycol terephthalate. The preparation method comprises the following steps: reacting organic silicon polyethylene glycol terephthalate with hydroquinone monomethacrylate and p-formylbenzoic acid in sequence to prepare modified polyethylene glycol terephthalate; coating diatomite with chitosan to prepare modified chitosan; the modified polyethylene glycol terephthalate, the modified chitosan and dimethyl phosphite are mixed, extruded and subjected to compression molding to prepare the bio-based polymer composite board. The bio-based polymer composite board prepared by the invention has excellent flame retardance, aging resistance and impact resistance.