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669 results about "Methylamines" patented technology

Derivatives of methylamine (the structural formula CH3NH2).

Cyclic structure betaine and double-tailed hydrophobic association polymer fracturing thickening agent and preparation method thereof

The invention relates to a ring structure betaine and double-tailed hydrophobic association polymer fracturing thickening agent and a preparation method thereof. The thickening agent is formed by copolymerization of four monomers, namely acrylamide, 2-allyl methylamino sodium ethanesulfonate, methyl diallyl sulfoethyl betaine and hydrophobic monomer double-tailed long-chain alkyl methyl allyl ammonium chloride. The preparation method comprises the following steps: firstly adding distilled water, then sequentially adding acrylamide, 2-allyl methylamino sodium ethanesulfonate, methyl diallyl sulfoethyl betaine and a hydrophobic monomer double-tailed long-chain alkyl methyl allyl ammonium chloride, adjusting the total concentration, introducing N2 to remove oxygen, adding an initiator, and reacting to prepare an AM / AMES / MDASBA / DCnMAAC quadripolymer, namely the polymer fracturing thickening agent. The thickening agent provided by the invention has good water solubility, and shows good salt resistance in mixed brine with the mineralization degree of greater than or equal to 30000 mg / L. The prepared linear solution and gel formed after crosslinking have high viscosity retention capacity at the temperature of 150 DEG C and the shearing rate of 170 s <-1 >, and the actual construction requirement for fracturing yield increase with the on-site mineralization degree larger than or equal to 30000 mg / L is met.
Owner:HEBEI PETROLEUM VOCATIONAL & TECH UNIV

Perovskite ink, preparation method thereof and perovskite solar cell

The invention provides perovskite ink, a preparation method thereof and a perovskite solar cell. The perovskite ink comprises a precursor solution A and a precursor solution B. The precursor solution A comprises a solute A and a solvent A, the precursor solution B comprises a solute B and a solvent B, the solute A comprises at least one of halogenated methylamine, halogenated formamidine, cesium halide and lead halide, and the solute B comprises at least one of cesium halide, lead halide and halogenated methylamine. The perovskite thin film prepared by using the perovskite ink is higher in crystallinity, larger in grain size after annealing and free of pinholes, and the energy conversion efficiency of the prepared perovskite solar cell is higher than that of a traditional DMF + DMSO solvent system. The invention also provides a preparation method of the perovskite ink and a perovskite solar cell.
Owner:GUANGDONG MINGYANG FILM TECH CO LTD

Stable perovskite precursor solution and preparation method and application thereof

The invention provides a stable perovskite precursor solution and a preparation method and application thereof. The perovskite precursor solution comprises a solute, a solvent and a stabilizer; the stabilizer comprises a compound containing a reducing group and a hydrogen ion group capable of being ionized; the solute comprises bromomethylamine, formamidine iodide, chloromethylamine, cesium iodide, lead iodide and lead bromide. The preparation method comprises the following steps: mixing a solute and a solvent, adding a stabilizer into the mixture, and mixing to obtain the perovskite precursor solution. According to the invention, the specific composition of the perovskite precursor solution is designed, and a specific stabilizer is further used, so that the perovskite precursor solution with relatively high stability and a relatively good storage effect is prepared.
Owner:JIUJIANG ROUSHUO OPTOELECTRONICS TECH CO LTD

Betaine type double-tailed hydrophobic association polymer fracturing thickening agent and preparation method thereof

PendingCN119661772Aincrease viscosityGood temperature and salt resistanceDrilling compositionEthanesulfonic acidPolymer science
The invention relates to a betaine type double-tailed hydrophobic association polymer fracturing thickening agent and a preparation method thereof. The thickening agent is prepared by the following steps: copolymerizing four monomers, namely acrylamide, 2-allyl methylamino sodium ethanesulfonate, methyl diallyl hydroxypropyl sulfobetaine and double-tailed long-chain alkyl allyl sulfoethyl betaine to form gel, chopping, hydrolyzing, neutralizing and purifying. The preparation method comprises the following steps: firstly adding distilled water, adding acrylamide, 2-allylmethylamino sodium ethanesulfonate, methyldiallyl hydroxypropyl sulfobetaine and other remaining raw materials, adjusting the total concentration, introducing N2 to remove oxygen, adding an initiator, reacting to prepare gel, chopping the gel, and hydrolyzing to obtain the water-soluble polymer. The fracturing thickening agent has good water solubility and shows good salt resistance in mixed saline water with the mineralization degree larger than or equal to 30000 mg / L, a prepared linear solution and jelly formed after crosslinking have high viscosity retention capacity at the temperature of 150 DEG C and the shearing rate of 170 s <-1 >, and the actual construction requirement for fracturing yield increase with the on-site mineralization degree larger than or equal to 30000 mg / L is met.
Owner:HEBEI PETROLEUM VOCATIONAL & TECH UNIV

4 apos; application of-methylamine baicalein in preparation of anti-photoaging product

The invention discloses an application of 4 '-methylamine baicalein in preparation of an anti-photoaging product. Experimental results show that the 4 '-methylamine baicalein not only has very low toxicity to fibroblasts, but also can remarkably improve the multiplication capacity of the fibroblasts irradiated by the UVB and can remarkably inhibit senescence of the fibroblasts irradiated by the UVB, and the effect of the 4'-methylamine baicalein is remarkably superior to that of baicalein; therefore, at least one of 4 '-methylamine baicalein or pharmaceutically acceptable salts, tautomers, stereoisomers and precursor compounds thereof can be used as an active ingredient for preparing anti-photoaging products, and the compound has important significance and application value especially for solving the photoaging problem generated by UVB phototherapy.
Owner:HANGZHOU THIRD PEOPLES HOSPITAL (HANGZHOU HUIMIN HOSPITAL HANGZHOU THIRD AFFILIATED HOSPITAL OF ZHEJIANG UNIV OF TRADITIONAL CHINESE MEDICINE) +2

Organic wastewater treatment agent and preparation method thereof

The invention discloses an organic wastewater treatment agent and a preparation method thereof, and relates to the field of water treatment materials. When the organic wastewater treatment agent is prepared, nano silicon dioxide sequentially reacts with a silane coupling agent 4140, sodium periodate, p-phenylenediamine and dimethyl phosphite, and modified nano silicon dioxide is prepared; the preparation method comprises the following steps: reacting modified nano silicon dioxide with 2, 4, 6-triformyl phloroglucinol and 2, 4-diamino-6-methoxypyrimidine, so as to prepare functionalized nano silicon dioxide; the preparation method comprises the following steps: reacting microcrystalline cellulose with thionyl chloride, N-(glycidyl)-N-phenyl-ethylene oxide methylamine and thiourea in sequence to prepare modified cellulose; and reacting the modified cellulose with the functionalized nano silicon dioxide to prepare the organic wastewater treatment agent. The organic wastewater treatment agent prepared by the invention has the capabilities of resisting bacteria, adsorbing anionic pollutants, adsorbing cationic pollutants and photocatalytically degrading organic pollutants.
Owner:DAQING TENGHUI PETRO TECH & SERVICE CO LTD

Double-tailed hydrophobic association polymer oil-displacing agent with benzene ring structure and preparation method of oil-displacing agent

The invention relates to a double-tailed hydrophobic associated polymer oil-displacing agent with a benzene ring structure and a preparation method thereof. The oil-displacing agent is formed by copolymerizing three monomers, namely acrylamide, 2-allyl methylamino sodium ethanesulfonate and a hydrophobic monomer double-tailed long-chain alkyl methyl (p-3-carboxyl acrylamide benzyl) ammonium chloride with the benzene ring structure. The preparation method comprises the following steps: firstly adding distilled water, then adding acrylamide, 2-allyl methylamino sodium ethanesulfonate and a hydrophobic monomer double-tailed long-chain alkyl methyl (p-3-carboxyl acrylamide benzyl) ammonium chloride with a benzene ring structure, supplementing water, adjusting the total concentration, introducing N2 to remove oxygen, adding an initiator, and reacting at a certain temperature to prepare the terpolymer. The prepared polymer oil-displacing agent has good water solubility, temperature resistance and shearing resistance, shows good salt resistance in saline water with the mineralization degree larger than or equal to 30000 mg / L and shows a good oil-displacing effect in a heterogeneous core oil-displacing experiment, and the crude oil recovery rate can be increased by 10% or above.
Owner:HEBEI PETROLEUM VOCATIONAL & TECH UNIV

Halogen-free low-splashing environment-friendly solder wire and preparation method thereof

The invention discloses a halogen-free low-splashing environment-friendly solder wire and a preparation method thereof, and relates to the technical field of electronic welding materials, and the halogen-free low-splashing environment-friendly solder wire is prepared from the following raw materials in percentage by mass: 1-4wt% of halogen-free scaling powder and the balance of lead-free solder; the lead-free solder is composed of the following components of Cu, Bi, Al, Ga, Ir, Ca, In and Sn. The halogen-free scaling powder comprises the following components: (3, 6-diamino acridine-9-yl) boric acid, glycerol triabietate, 3-(N-morpholinyl)-2-hydroxy propanesulfonic acid sodium salt, 3-trihydroxymethyl methylamino-2-hydroxy propanesulfonic acid, hexahydro-1, 3-ethoxy-s-triazine, a functional copolymer, a surface active agent, a corrosion inhibitor, a halogen-free activity reinforcing agent, an antioxidant, a solvent and rosin resin. The solder wire is low in splashing rate, high in surface resistivity and welding spot reliability, free of obvious corrosivity and good in weldability.
Owner:GUANGDONG ZHONGSHI METAL CO LTD

Preparation method of perovskite active layer, perovskite battery and perovskite material

The invention discloses a preparation method of a perovskite active layer, a perovskite battery and a perovskite material, and belongs to the technical field of perovskite batteries. According to the invention, bisphosphonate is added when the perovskite active layer is prepared, and the bisphosphonate is obtained by carrying out a deprotonation reaction on 1-aminodecane-1, 1-diphosphonic acid and methylamine, formamidine iodine or cesium carbonate. The bisphosphonate can be anchored on the surface of the substrate and form a self-assembled monomolecular structure, a simple and effective coating process is realized, the bisphosphonate structure of the bisphosphonate is beneficial to anchoring on the substrate, the possibility and effectiveness of anchoring the substrate are increased, the combination of the perovskite active layer and the substrate is enhanced, the formation of nano-pores is reduced, and the photoelectric conversion efficiency is improved. In addition, the introduced cations MA < + >, FA < + > and Cs < + > not only can enhance the self-assembly capability of the bisphosphonate, but also can be used as nucleating agents to promote the growth of perovskite crystals and improve the quality of the perovskite crystals.
Owner:旗滨新能源发展(深圳)有限责任公司

Disulfonate hydrophobic association polymer oil-displacing agent with benzene ring structure and preparation method of disulfonate hydrophobic association polymer oil-displacing agent

The invention relates to a bisulfonate hydrophobic association polymer oil-displacing agent with a benzene ring structure and a preparation method thereof. The polymer oil-displacing agent is formed by copolymerization of three monomers, namely acrylamide, sodium 2-allyl methylamino ethanesulfonate and long-chain alkyl disulfoethyl (4-vinyl benzyl) betaine which is a hydrophobic monomer with the benzene ring structure. The preparation method comprises the following steps: firstly adding distilled water, sequentially adding acrylamide, 2-allylmethylamino sodium ethanesulfonate and long-chain alkyl disulfoethyl (4-vinyl benzyl) betaine, adding water to adjust the total concentration, introducing N2 to remove oxygen, adding an initiator, and reacting at a certain temperature to obtain the terpolymer. The polymer oil-displacing agent prepared by the invention has good water solubility and good temperature resistance and shear resistance, shows good salt resistance in saline water with the degree of mineralization being greater than or equal to 30000 mg / L, shows a good oil-displacing effect in heterogeneous rock cores, and can improve the crude oil recovery rate by 10% or above.
Owner:HEBEI PETROLEUM VOCATIONAL & TECH UNIV

Dry powder drag reducer for fracturing fluid and preparation method of dry powder drag reducer

The invention provides a dry powder drag reducer for fracturing fluid and a preparation method of the dry powder drag reducer, and belongs to the technical field of fracturing materials for well drilling, and the preparation method comprises the following steps: dissolving 4-bromobutyryl chloride and N-dodecyl methylamine in acetonitrile, heating and stirring for reaction, adding polyethylene glycol monomethyl ether acrylate and dichloromethane, stirring and purifying in a nitrogen atmosphere to obtain a dry powder drag reducer; a double-tailed hydrophobic monomer is obtained; uniformly mixing the core-shell SiO2 / Fe3O4 composite nanoparticles, an ethanol water solution, KH570 and an ammonia solution, stirring, and purifying to obtain modified SiO2 / Fe3O4; the preparation method comprises the following steps: adding acrylamide, acrylic acid, sodium 2-acrylamido-2-methylpropanesulfonate, a double-tailed hydrophobic monomer and modified SiO2 / Fe3O4 into water, uniformly mixing, adjusting the pH value, introducing nitrogen, mixing and stirring, adding an azo initiator, stirring, cooling, purifying, carrying out vacuum drying, and crushing into powder, thereby obtaining the dry powder drag reducer for the fracturing fluid. The drag reducer has certain heat resistance while achieving good drag reduction performance, and can be better applied to fracturing operation in the well drilling process.
Owner:SHAANXI LONGYU INT TECH GRP CO LTD

Methylamine rectification equipment, separation and purification assembly and purification process

The invention discloses methylamine rectification equipment, a separation and purification assembly and a purification process, and relates to the technical field of methylamine processing.The methylamine rectification equipment comprises a tower body, a skirt is arranged at the bottom of the tower body, a manhole is formed in the side face of the skirt, a drain pipe is arranged at the bottom of the tower body, a ventilation hole is formed in the side face of the skirt, and a steam ingress pipe is arranged at the bottom of the side face of the tower body; a liquid inlet pipe is arranged on the side face of the tower body, a backflow pipe and a tower body top hanging column are arranged on the two sides of the top of the side face of the tower body respectively, a steam guide-out pipe is arranged at the top end of the tower body, a gas-liquid separator is arranged on the top side of the interior of the tower body, and tower plate assemblies are vertically arranged in the tower body in a staggered mode. Moreover, when the tower plate leaks liquid, monitoring is carried out in time, process parameters are adjusted in time, in addition, the flow speed of liquid on the tower plate can be adjusted conveniently according to production requirements, and blockage clearing can be intervened in time conveniently when the tower plate is blocked.
Owner:HEALTHY HANGZHOU HUSBANDRY SCI-TECH CO LTD +1

Perovskite precursor solution, perovskite solar cell and preparation method thereof

The invention discloses a perovskite precursor solution, a perovskite solar cell and a preparation method of the perovskite solar cell. The perovskite precursor solution provided by the invention contains a perovskite precursor solute, a perovskite precursor solvent and an additive, the perovskite precursor solute contains lead halide, and further contains at least one of tin halide, formamidine halide, methylamine halide, cesium halide, dimethylamine halide and guanidine halide; the perovskite precursor solvent contains at least one of N, N-dimethyl formamide, dimethyl sulfoxide, N-methyl pyrrolidone, 2-methoxyethanol, valerolactone and acetonitrile, and the perovskite precursor solvent contains at least one of N, N-dimethyl formamide, dimethyl sulfoxide, N-methyl pyrrolidone, 2-methoxyethanol, valerolactone and acetonitrile; the additive contains an organic salt of trifluoromethyl acid. The opening voltage loss is reduced, the filling factor and the photoelectric conversion efficiency of the battery are improved, the precipitation of lead iodide is reduced in the crystallization annealing process, the volatilization of organic cations is inhibited, the non-uniform crystallization is improved, and the stability of the battery is improved.
Owner:UNIV OF SCI & TECH OF CHINA

Expanded polytetrafluoroethylene artificial blood vessel with anticoagulation coating as well as preparation and application of expanded polytetrafluoroethylene artificial blood vessel

According to the scheme, the expanded polytetrafluoroethylene artificial blood vessel with the anticoagulant coating and preparation and application are provided, firstly, groups such as carboxyl and amino are formed on the inner surface of the expanded polytetrafluoroethylene artificial blood vessel through co-auto-polymerization reaction of L-dopamine and polyethyleneimine in a Tris aqueous alkali, then epoxy chloropropane serves as a cross-linking agent, and the expanded polytetrafluoroethylene artificial blood vessel with the anticoagulant coating is prepared. Trihydroxymethyl methylamino propanesulfonic acid is cross-linked to the inner surface of the membrane, carboxyl and sulfonic acid groups on the surface of the membrane endow the expanded polytetrafluoroethylene artificial blood vessel with anticoagulation performance, meanwhile, the hydrophobic performance of the outer surface is reserved, anticoagulation finishing is conducted on the inner wall of the expanded polytetrafluoroethylene artificial blood vessel, and the hydrophobic performance of the outer wall of the blood vessel is reserved; the expanded polytetrafluoroethylene artificial blood vessel has an anticoagulation function and does not influence the growth of fiber cells and fiber connective tissues on the surface of the blood vessel.
Owner:ZHEJIANG SCI-TECH UNIV

Method for optimizing quality of perovskite layer through atmosphere annealing

The invention relates to a method for optimizing the quality of a perovskite layer through atmosphere annealing, and belongs to the technical field of perovskite layer quality optimization, and the method comprises the steps: preparing precursor materials: taking methylamine hydrochloride, cesium iodide, formamidine iodide and lead iodide as perovskite precursor materials; the preparation method comprises the following steps: preparing a solvent: mixing N-methyl pyrrolidone with dimethylformamide; solution preparation: mixing the precursor material with a solvent to prepare a precursor solution; stirring and filtering the solution; preparing a substrate: sputtering NiO serving as a hole transport layer material on the glass substrate; blade coating of a perovskite precursor solution: uniformly blade coating the precursor solution on the glass substrate coated with the NiO film; preliminary drying; vacuum annealing preparation: placing the glass substrate coated with the perovskite precursor film in a vacuum cavity; nitrogen atmosphere filling: filling high-purity nitrogen; in the nitrogen atmosphere, the temperature in the cavity is increased to a certain temperature range, annealing is conducted at the temperature, and the optimized annealing temperature and time are selected; and cooling and packaging.
Owner:FLAT GLASS GROUP CO LTD

Preparation method of energy-saving corrosion inhibition type decarburizing agent

The invention belongs to the field of biomass gasification catalysts, and particularly relates to a preparation method of an energy-saving corrosion inhibition type decarburizing agent. According to the invention, under the action of the catalyst, ethylene carbonate and methylamine are adopted as basic raw materials to synthesize N-methyldiethanolamine, and then 1, 3-propane sultone is adopted to modify N-methyldiethanolamine, so that the carbon dioxide absorption amount and absorption rate of N-methyldiethanolamine are improved; the activating agent is added into the energy-saving corrosion-inhibition type decarburizing agent, so that the absorption rate of the decarburizing agent on carbon dioxide can be effectively improved, and the desorption energy consumption of the carbon dioxide is reduced; and the corrosion inhibitor is added, so that the corrosion of metal equipment can be effectively reduced.
Owner:ZIBO KAIMEIKE IND & TRADE CO LTD

Three-layer multi-core structure catalyst for high-selectivity synthesis of monomethylamine and preparation method of three-layer multi-core structure catalyst

The invention belongs to the field of methanol conversion and utilization, and particularly relates to a three-layer multi-core structure catalyst for high-selectivity synthesis of monomethylamine and a preparation method of the three-layer multi-core structure catalyst. The core layer of the catalyst is gamma-aluminum oxide, the middle layer of the catalyst is a mordenite (MOR) molecular sieve, and the outer layer of the catalyst is porous SiO2. The preparation of the multi-core MOR layer adopts a steam-assisted crystallization method, the preparation method is simple, no organic waste liquid is generated, the preparation method is environment-friendly, the multi-core MOR layer can be used in a reaction for preparing methylamine through continuous gas phase catalytic amination of methanol after being modified by ammonium ion exchange and chemical liquid phase deposition (CLD), the methanol conversion rate reaches 98.6% under the reaction conditions that the temperature is 340 DEG C, the methanol liquid hourly space velocity is 1.5 h <-1 >, the ammonia-alcohol ratio is 3 and the pressure is normal, and the method is suitable for industrial production. The mass ratio of monomethylamine is greater than 60%, and the method has a good application prospect.
Owner:HE NAN NENG YUAN JI TUAN YAN JIU ZONG YUAN YOU XIAN GONG SI

Preparation method of anti-cracking modified EVA cable material

The invention relates to the technical field of high polymer materials, and discloses a preparation method of an anti-cracking modified EVA cable material.The preparation method comprises the steps that maleic anhydride, N, N-bis (2-aminoethyl) methylamine, benzyl chloride and HDPE serve as raw materials, antibacterial modified HDPE is prepared through a dehydration ring-closing one-step method and a solution method, and the anti-cracking modified EVA cable material is obtained; the preparation method comprises the following steps: taking antibacterial modified HDPE as a raw material, then taking benzotriazole, bis (2-chloroethyl) amine, 3-chloropropyltrimethoxysilane and magnesium hydroxide as raw materials, performing substitution reaction and polymerization reaction to prepare anti-ultraviolet modified magnesium hydroxide, and finally taking antibacterial modified HDPE, EVA, the anti-ultraviolet modified magnesium hydroxide, red phosphorus and the like as raw materials, and performing melting method to prepare the anti-cracking modified EVA cable material. The anti-cracking modified EVA cable material prepared by the preparation method disclosed by the invention has relatively good anti-cracking performance, antibacterial performance, flame-retardant performance and anti-ultraviolet performance.
Owner:ANHUI YANGZI IND CO LTD

Carbon fiber modified sizing agent as well as preparation method and application thereof

PendingCN121270863ACarbon fibresEpoxyFiber
The invention discloses a carbon fiber modified sizing agent as well as a preparation method and application thereof. The preparation method of the carbon fiber modified sizing agent comprises the following steps: (1) reacting 5-norbornene-2-methylamine with monofunctional epoxy resin to obtain slurry; and (2) dissolving the slurry prepared in the step (1) in an organic solvent to prepare the modified sizing agent. And then obtaining the modified carbon fiber through a dipping and sizing process. The method is simple in process, and the interface bonding strength of the carbon fibers and the polydicyclopentadiene can be greatly improved.
Owner:CHINA PETROLEUM & CHEMICAL CORP +1

Large-area methylamine-free perovskite photovoltaic module and preparation method thereof

The invention relates to a large-area methylamine-free perovskite photovoltaic module and a preparation method thereof. The photovoltaic module comprises a substrate, a hole transport layer, a perovskite active layer, an interface passivation layer, an electron transport layer and a metal electrode, the hole transport layer is a nickel oxide / organic hole material composite layer; the organic hole material comprises PTAA, P3HT, MoO3 or a self-assembled monomolecular layer. The perovskite solar cell provided by the invention has remarkable advantages in performance and stability, and especially has excellent long-term stability under high-humidity and high-temperature conditions.
Owner:NANKAI UNIV

Synthesis method of tilpotide

The invention provides a synthesis method of tilpotide, which comprises the following steps: dividing a target peptide chain into six fragments, and adopting bis (4-C18-C28 alkoxy phenyl) methylamine, 2, 4-bis (18-C28 alkoxy)-benzyl alcohol and NH2-Asp (OTAG)-OR1 as hydrophobic label carriers to assist synthesis. A side chain carboxyl group of aspartic acid is innovatively used as an anchoring position of a hydrophobic label, a new fragment connection route is designed, a full-protection tilpotide conjugate is synthesized through a multi-label synergistic effect, and finally a protecting group and a label are removed by using a TFA lysate. Compared with a solid-phase synthesis method, the method is carried out in a homogeneous reaction, the dosage of amino acid and the condensing agent is reduced to 1-1.2 times from 2-3 times, and the cost is remarkably reduced. Compared with an existing hydrophobic labeling method, the method has the advantages that multiple labels can be introduced to serve as protecting groups, the yield and purity of synthesis of medium-chain and long-chain polypeptides are improved, meanwhile, the problem of hydrophobicity attenuation caused by peptide chain extension is solved, and the green chemical process requirement is met.
Owner:ZHEJIANG UNIV OF TECH

Method for preparing rosuvastatin calcium intermediate

The invention relates to a method for preparing a rosuvastatin calcium intermediate, and belongs to the technical field of drug intermediate synthesis. The method comprises the following steps: under the protection of nitrogen, carrying out reflux reaction on raw materials including 4-fluorobenzaldehyde and ethyl 4-methyl-3-oxovalerate under the catalysis of piperidine acetate and a co-catalyst, and carrying out reduced pressure distillation recovery to obtain a compound shown as a formula V; dropwise adding 2-ethyl-2-isothiourea and a compound shown in a formula VI, carrying out cyclization reaction under a non-violent reflux condition, and then adding DDQ in batches for oxidation to obtain a compound shown in a formula IV; oxidizing the compound as shown in the formula IV, and immediately quenching by using saturated NaHCO3 after the reaction is finished to obtain a compound as shown in a formula III; the preparation method comprises the following steps: firstly, treating a compound shown as a formula III by using methylamine, and slowly dropwise adding methylsulfonyl chloride under ice bath temperature control to obtain a compound shown as a formula II; reducing the ester group of the compound shown in the formula II in anhydrous toluene by using DIBAL to obtain an alcohol intermediate; then, selective oxidation is performed to obtain a final product; the method integrally has the advantages of high product yield and purity, few byproducts and low production difficulty.
Owner:JIANGSU FURUI KANGTAI PHARM CO LTD

Preparation method of key intermediate of chlorantraniliprole

The invention provides a preparation method of a chlorantraniliprole key intermediate 2-amino-5-cyano-N, 3-dimethyl benzamide, which comprises the following steps: taking cheap and easily available o-methylaniline as a raw material, acylating an aniline substrate through Boc anhydride, carrying out ortho-lithiation on n-butyllithium, introducing carbon dioxide gas, and carrying out acid hydrolysis to obtain 2-amino-3-methyl benzoic acid, thereby obtaining the chlorantraniliprole key intermediate 2-amino-5-cyano-N, 3-dimethyl benzamide. The preparation method comprises the following steps: firstly, preparing an isatoic anhydride intermediate, then carrying out triphosgene ring closing to obtain an isatoic anhydride intermediate, carrying out bromine para-position halogenation, carrying out cuprous cyanide high-temperature Rosenmn-von Braun reaction, and finally carrying out methylamine ring opening to obtain the target product 2-amino-5-cyano-N, 3-dimethylbenzamide, and although the route is long, the yield is high, the continuity is good, few industrial three wastes are generated, and the cost is lower, so that the preparation method has great industrial production value.
Owner:SHANDONG LONGXI PLANT PROTECTION CO LTD

Flavonoid compound-meglumine co-amorphous substance and preparation method thereof

The invention belongs to the technical field of medicines, and particularly relates to a flavonoid compound-meglumine co-amorphous substance and a preparation method thereof. The flavonoid compounds comprise baicalein, hesperetin, naringenin, kaempferol, quercetin, isoliquiritigenin and the like, and the co-amorphous substance consists of a single flavonoid compound and meglumine and is prepared by adopting a melting shock cooling method or a rotary evaporation method. The miscibility of the flavonoid compounds and the meglumine is screened through Hansen solubility. The crystal diffraction characteristics, thermodynamic properties and intermolecular interaction of the co-amorphous substance are measured through PXRD, DSC and FTIR, and it is shown that the six flavonoid compounds and meglumine successfully form a co-amorphous system. The solubility and the dissolution rate of the six flavonoid compound-meglumine co-amorphous substance are obviously superior to those of flavonoid bulk drugs, and the physical stability of the formed co-amorphous substance is obviously superior to that of a single amorphous drug, so that the co-amorphous substance shows good patent medicine performance.
Owner:CHANGZHOU UNIV

Method for preparing trifluorobenzene pyrimidine

The invention belongs to the field of pesticide intermediates and product preparation, and particularly relates to a method for preparing trifluorobenzene pyrimidine. The method disclosed by the invention comprises the following steps: (1) in a first organic solvent, carrying out Schiff base condensation reaction on 2-aminopyridine and pyrimidine-5-formaldehyde under the action of a first moisture scavenger to generate N-2-pyridine-5-pyrimidine methylenimine; (2) in a second organic solvent, carrying out reductive amination reaction on the N-2-pyridine-5-pyrimidine methylenimine and hydrogen under the action of a catalyst to generate N-2-pyridine-5-pyrimidine methylamine; and (3) in a third organic solvent, carrying out cyclization reaction on the N-2-pyridine-5-pyrimidine methylamine and 2-(3-trifluoromethylphenyl) malonyl chloride in the presence of an acid-binding agent, so as to prepare the trifluorobenzene pyrimidine. According to the method disclosed by the invention, the post-treatment operation times and the reaction reagent consumption are greatly reduced, and efficient and green production is realized.
Owner:EAST CHINA UNIV OF SCI & TECH

Bisulfonate hydrophobic association polymer oil-displacing agent with cyclic structure and preparation method of bisulfonate hydrophobic association polymer oil-displacing agent

The invention relates to a bisulfonate hydrophobic associated polymer oil-displacing agent with a cyclic structure and a preparation method thereof. The oil-displacing agent is formed by copolymerization of four monomers, namely acrylamide, sodium 2-allyl methylamino ethanesulfonate, diallyl disulfoethyl betaine and long-chain alkyl dimethyl (p-3-carboxyl acrylamide benzyl) ammonium chloride which is a hydrophobic monomer with a benzene ring structure. The preparation method comprises the following steps: firstly, adding distilled water, then sequentially adding acrylamide, 2-allyl methylamino sodium ethanesulfonate, diallyl disulfoethyl betaine and a hydrophobic monomer long-chain alkyl dimethyl (p-3-carboxyl acrylamide benzyl) ammonium chloride with a benzene ring structure, supplementing water, adjusting the total concentration, introducing N2 to remove oxygen, adding an initiator, and stirring to obtain the water-absorbent polymer. And reacting at a certain temperature to obtain the quadripolymer. The prepared oil-displacing agent has good water solubility, temperature resistance and shearing resistance, shows good salt resistance in saline water with the mineralization degree larger than or equal to 30000 mg / L, shows a good oil-displacing effect in heterogeneous rock cores, and can improve the crude oil recovery rate by 10% or above.
Owner:HEBEI PETROLEUM VOCATIONAL & TECH UNIV

Preparation method of deuterated methylamine hydrochloride and solid-phase continuous flow synthesis system

The invention discloses a preparation method of deuterated methylamine hydrochloride and a solid-phase continuous flow synthesis system, and relates to the technical field of deuterated synthesis. The preparation method comprises the following steps: adding out-of-phase polykadexide into methyl trifluoromethanesulfonate and 1, 2-dichloroethane for heating reaction, then adding methanol for quenching reaction, washing and drying to obtain an out-of-phase polykadexide type methyl reagent; the method comprises the following steps: adding a heterophase polysulfide-type methyl reagent into a mixed solvent of a polar solvent and heavy water, and carrying out alkali treatment to complete deuteration conversion, so as to obtain a heterophase polysulfide-type deuterated methyl reagent; the preparation method comprises the following steps: dissolving o-phenylsuccinimide in acetonitrile, and adding a heterophase polysulfide deuterium methyl reagent and inorganic alkali to react, so as to obtain N-(1, 1, 1-trideuterium methyl) benzo-succinimide; the preparation method comprises the following steps: hydrolyzing N-(1, 1, 1-trideuterium methyl) benzo-succinimide and hydrochloric acid in an aqueous solvent to obtain deuterated methylamine hydrochloride. The preparation method is simple, the deuterium source is cheap, the atom utilization rate is high, the deuteration rate is high, and the production cost is low.
Owner:SHENZHEN UNIV

1-methylimidazole based on ionic liquid catalytic system and efficient synthesis process thereof

The invention relates to the technical field of 1-methylimidazole and synthesis thereof, in particular to 1-methylimidazole based on an ionic liquid catalytic system and an efficient synthesis process of the 1-methylimidazole, glyoxal, methylamine and formaldehyde are used as raw materials, and the ionic liquid catalytic system is prepared by compounding sulfonic acid group and carboxyl functionalized ionic liquid according to the ratio of 2: 1. The cocatalyst is formed by compounding transition metal salt and organic alkali according to the ratio of 1: 2, the molar ratio of the raw materials is 1: 2: 2, and the sulfonyl ionic liquid is subjected to microwave activation, carboxyl ionic liquid loading, transition metal salt ultrasonic pretreatment and organic alkali rectification purification to synergistically promote the reaction, so that efficient synthesis of 1-methylimidazole is realized, and the yield and purity of the product are improved. According to the process, a specially treated ionic liquid catalytic system and a cocatalyst are adopted, operations such as pulse stirring and multiple extraction are combined, efficient synthesis of 1-methylimidazole is achieved, the product purity exceeds 99%, the yield exceeds 90%, the cost is reduced, pollution is reduced, the green chemistry concept is met, and the application prospect is wide.
Owner:SHANDONG DYKE BIOTECHNOLOGY CO LTD

Preparation method of (S)-oxetane-2-methylamine

The invention provides a preparation method of (S)-oxetane-2-methylamine. The preparation method of (S)-oxetane-2-methylamine comprises the following steps: (1) carrying out ring closing reaction on a compound A under an alkaline condition to obtain a compound B; (2) reacting the compound B with dibenzylamine to obtain a compound C; (3) reacting the compound C with a reducing agent to obtain a compound D; (4) reacting the compound D with paratoluensulfonyl chloride to obtain a compound E; (5) reacting the compound E with alkali to obtain a compound F; and (6) carrying out a reaction on the compound F and palladium on carbon to obtain the (S)-oxetane-2-methylamine. According to the preparation method provided by the invention, ring expansion reaction using trimethylsulfoxide iodide in the prior art is avoided, the problem that residual sulfur elements cause poisoning of a palladium-carbon catalyst is solved, meanwhile, sodium azide is also avoided, and the preparation method is safe and reliable in process, high in chiral purity and yield and suitable for industrial large-scale production.
Owner:SHANGHAI KELY BIOPHARMACEUTICAL CO LTD +1

Heat-resistant polymethyl methacrylate, preparation method thereof and optical film

The invention discloses heat-resistant polymethyl methacrylate, a preparation method thereof and an optical film. The heat-resistant polymethyl methacrylate comprises a methyl methacrylate repetitive unit, a glutarimide repetitive unit and an N-methyl methacrylamide repetitive unit, and the sum of the number of the glutarimide constitutional unit and the number of the N-methyl methacrylamide constitutional unit is 1-20 mol% of the total number of the constitutional units. The glutarimide structural unit can be obtained by further cyclization reaction of an N-methyl methacrylamide structural unit, and the cyclization rate can be increased to 80-90% by adding a cyclization accelerator such as triethylamine, so that the thermal stability of the resin is improved, and the water absorption rate is reduced. The material can be used for preparing an optical film, has excellent heat resistance and moisture resistance, and is suitable for the field of optical display.
Owner:WANHUA CHEM GRP CO LTD