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706 results about "Tetrabutylammonium bromide" patented technology

Tetra-n-butylammonium bromide (TBAB) is a quaternary ammonium salt with a bromide counterion commonly used as a phase transfer catalyst. It is used to prepare many other tetrabutylammonium salts via salt metathesis reactions.

Microwave synthesis process for ZSM-11 molecular sieve

The invention relates to a microwave synthesis process for a ZSM-11 molecular sieve. The process uses aluminum source, alkali source, silicon source, tetrabutylammonium bromide and de-ionized water as the raw materials and adopts the heating mode of microwave radiation. The reaction mixture is crystallized for 1 to 8 hours under microwave radiation and self-generated pressure at 130 to 180 DEG C, solid is separated from the mother liquid, and then the product is washed by the de-ionized water until the pH value is 8 to 9, thus obtaining the raw powder of the ZSM-11 molecular sieve. The microwave synthesis process for the ZSM-11 molecular sieve has the advantages of replacing traditional water heating by microwave radiation heating and obtaining the ZSM-11 molecular sieve with the advantages of high crystallinity, pure crystal phase and controllable and wide range of grain size, and the process accelerates the nucleation rate and crystal growth speed obviously and shortens the crystallization time greatly by pre-placing crystal seeds.
Owner:DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI

Method for making PH value-sensitive polyvinylidene fluoride hollow fibre intelligent film and products thereby

Disclosed is a method for making pH sensitive PVDF hollow fiber intelligent film and products made thereby, wherein the making process comprises the steps of, (1) steeping the film in pure water for 24 hours, (2) preparing 10-20% alkali solution, and charging 3-4gl / L of tetrabutylammonium bromide, charging immersed film in alkali solution, heating by water bath, (3) preparing 1-2 mol / L of AAC solution, charging dimethyl formamide solution by 40-50ml / L, mixing uniformly, charging alkali-treated film in the mixed solution, steeping 10-20 minutes at room temperature, preparing solution of crosslinking agent 0.01-0.09mol / L and K2S2O3 0.1-0.3g, charging the readily made film into the solution, filling N2 and sealing, water-bathing, heating and washing with deionized water, the crosslinking agent is MBAA or diacrylic acid ethylene glycol ester.
Owner:TIANJIN POLYTECHNIC UNIV

Waterborne epoxy acrylate-grafted composite emulsion and preparation method thereof

The invention relates to the field of manufacture of epoxy acrylate composite resin materials, in particular to a waterborne epoxy acrylate-grafted composite emulsion and a preparation method thereof. The process mainly comprises the following steps of: firstly, by taking a polymerizing monomer as a dispersing medium, enabling epoxide resin and acrylic acid to react under the action of tetrabutylammonium bromide to generate an epoxy acrylate monomer; and secondly, pre-emulsifying the epoxy acrylate monomer and other monomers and then enabling the epoxy acrylate monomer and other monomers to generate a copolymerization reaction to prepare the waterborne epoxy acrylate-grafted composite emulsion by adopting a semi-continuous seeded emulsion polymerization method. According to the process, the copolymerization monomer is used as a solvent dispersing medium for the esterification reaction of the epoxide resin and the acrylic acid in the first step and is also a monomer of the copolymerization reaction in the second step; an organic solvent in the reaction of the first step is prevented from being removed by adopting reduced pressure distillation, so that the influence of residual solvent on the performance of the product is avoided; the waterborne epoxy acrylate-grafted composite emulsion has high grafting rate and can be used for improving the compatibility of the epoxide resin and acrylic acid resin and enhancing the performances of the water resistance, the adhesive force, the salt resistance and the like of a coating and can be widely applied to the fields of metal coatings, building coating materials and the like.
Owner:HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY

Macromolecular polymerizable photoinitiator and preparation thereof

The invention discloses a macromolecular polymerizable photoinitiator and a preparation thereof. The method comprises the following steps of: adding 4-hydroxybenzophenone and methanal to a three-necked flask, heating to 95 DEG C, reacting for 2 hours, heating to 150DEG C, leaching under at reduced pressure for 20 minutes, cooling to 105 DEG C, collecting products, pouring products into water, leaching to obtain a macromolecular photoinitiator, dissolving the macromolecular photoinitiator in an organic solvent, dissolving epoxy chloropropane in the solvent under catalysis of boron trifluoride,dropwise adding mixed liquid, reacting at a temperature of 0-5 DEG C, then stirring for 3 hours at a temperature of 70 DEG C, removing epoxy chloropropane and solvent, dissolving residues with a solvent, adding alkali and reacting for 0.5 hour at a temperature of 40 DEG C, removing salt and the solvent, re-dissolving residues with a solvent, washing with water and drying, adding crylic acid, p-hydroxyanisole and tetrabutylammonium bromide, heating for reacting for 6 hours, and then removing the solvent so as to obtain macromolecular polymerizable photoinitiator. The macromolecular polymerizable photoinitiator prepared by the method has the advantages of large molecular weight, weak mobility and good polymerizability.
Owner:HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH

Method for making temperature-sensitive polyvinylidene fluoride hollow fibre intelligent film and products thereby

Disclosed is a method for making temperature-sensitive PVDF hollow fibre intelligent film and products made by chemical grafting and copolymerization of NIPA on PVDF film surface, and the making process comprises the steps of, (1) steeping the film in pure water for 24 hours, (2) preparing 10-20% alkali solution, and charging 3-4gl / L of tetrabutylammonium bromide, charging immersed film in alkali solution, water-bathing, heating and washing for later use, the alkali solution is one of KOH, NaOH or LiOH, (3) preparing 1-2 mol / L of NIPA solution, charging dimethyl formamide solution by 40-50ml / L, mixing uniformly, charging alkali-treated film in the mixed solution, steeping at room temperature, preparing solution of crosslinking agent 0.01-0.09mol / L and K2S2O3 0.1-0.3g, charging the readily made film into the solution, filling N2 and sealing, water-bathing, heating and washing with deionized water, the crosslinking agent is MBAA or diacrylic acid ethylene glycol ester.
Owner:TIANJIN POLYTECHNIC UNIV

Quaternary ammonium salt organic silicon gemini surfactant and preparation method thereof

The invention relates to a quaternary ammonium salt organic silicon gemini surfactant and a preparation method thereof. The preparation method is prepared by the following steps of mixing polyethylene glycol diglycidyl ether, alpha-hydrogen-omega-hydroxyl-polydimethylsiloxane and acetone, adding tetrabutylammonium bromide and sodium hydroxide solutions, stirring and refluxing at the temperature of 50 to 70 DEG C, so as to obtain epoxy polyether-modified siloxane; adding a hydrochloric acid solution, long-strand alkyl dimethye third amine and a solvent into a reactor, uniformly stirring, dripping the epoxy polyether-modified siloxane, and reacting until the amine value is not changed, so as to obtain a target product. The quaternary ammonium salt organic silicon gemini surfactant has the advantages that the product has excellent surface activity, the surface tension in the water solution is minimum to 28.24mN / m, and the critical micelle concentration is minimum to 1.5*10-6mol / L, and is far lower than the critical micelle concentration of the traditional hydrocarbon single-strand surfactant DTAB (dodecyl trimethyl ammonium bromide); by using the linking of covalent bonds, the hydrolysis resistance property or organic silicon is improved; the advantages of the quaternary ammonium salt organic silicon gemini surfactant and the organic silicon surfactant are simultaneously realized.
Owner:湖北天喜达生物科技有限公司

Self-emulsifying aqueous epoxide resin paint and method for producing the same

The invention relates to a self-emulsifiable water epoxide resin coating mainly consisting of water epoxide resin and a water curing agent; wherein, the water epoxide resin is the product obtained by the reaction of epoxide resin with Alpha-amino-Omega-alkyl polyether, or can be obtained by taking the product as epoxide resin emulsifier to carry out emulsification on the low molecular weight epoxide resin by adding water. The preparation method of the coating is as follows: preparing end alkoxy polyether at a chlorine end capping which is then put into well mixed mixture of hydroxyphenyl aliphatic amine, sodium hydroxide and tetrabutylammonium bromide; stirring, extracting, filtering and distilling the mixture to remove the solvent, thus getting the end alkane oxyl polyether; taking propylene glycol methyl ether as solvent, evenly mixing the epoxide resin and the end alkane oxyl polyether, and removing the solvent by being distilled after being stirred. The self-emulsifiable water epoxide resin coating has good storage stability, no toxity, and high packing ratio of filler, can be solidified under indoor temperature, has high adhesive force, high flexibility, good water resisting property and solvent resisting property.
Owner:WUHAN UNIV OF TECH

Alkylbenzene sulfonate Gemini surfactant and preparation method thereof

The invention relates to an alkylbenzene sulfonate Gemini surfactant and a preparation method thereof. The method comprises the following steps of: undergoing a substitution reaction: undergoing a substitutive etherification reaction at the temperature of 65-70 DEG C for 6 hours on phenol and dihalogenated alkane under the action of a phase transfer catalyst to generate bisether, wherein the molar ratio of the phenol to saturated dihalide is 1:3, the saturated dihalide is head-to-end dibromoalkane, the quantity of atoms C of the dibromoalkane is larger than 2, and the phase transfer catalyst is tetrabutylammonium bromide; performing Fourier alkylation: making the bis-ether react with an alkyl halide at the temperature of 80 DEG C and under the pressure of 0.3 MPa under the action of a Louis acid catalyst to generate dialkyl phenylate, wherein the molar ratio of the bis-ether to the alkyl halide is 1:2; undergoing a sulfonation reaction: undergoing a sulfonation reaction on the dialkyl phenylate and a chlorosulfonic acid in the molar ratio of 1:4 by taking dichloromethane as a solvent at the temperature of 0 DEG C; and undergoing a salt-forming reaction: adding an alkali to generate a target product. The alkylbenzene sulfonate Gemini surfactant has very high interfacial activity and a very low critical micelle concentration.
Owner:PETROCHINA CO LTD

Preparation method and application of functionalized polyvinyl alcohol microspheres

The invention discloses a preparation method and application of functionalized polyvinyl alcohol microspheres. The preparation method comprises the following steps: uniformly mixing polyvinyl alcohol microspheres, epoxy chloropropane and a hydrochloric acid solution, carrying out a stirring reaction for 1-5 hours in a water bath, and carrying out centrifuging, water cleaning and drying for later use after the reaction; uniformly mixing the obtained chloridized polyvinyl alcohol microspheres, tetrabutylammonium bromide, ethidene diamine and a sodium hydroxide solution, carrying out the stirring reaction for 4-10 hours in the water bath, and carrying out the centrifuging, ethanol cleaning and the drying for later use after the reaction; and uniformly mixing the obtained aminated polyvinyl alcohol microspheres with 2-(2-pyridine) azo-resorcinol, formaldehyde and distilled water, stirring for 6-18 hours in the presence of nitrogen, and carrying out the centrifuging, the ethanol cleaning and the drying after the reaction, so as to obtain an end product. The functionalized polyvinyl alcohol microspheres provided by the invention can be used for chelating heavy metal and detecting and processing divalent heavy metal ions in wastewater and have the characteristics of simple preparation condition, low cost, short detection response time and high adsorption capacity.
Owner:NANJING HEHAI TECH

Method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis

The invention relates to a method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis, particularly relates to a method for preparing high-purity tetrabutyl ammonium hydroxide by using tetrabutyl ammonium bromide as a raw material and adopting a three-compartment bipolar membrane electrodialysis device, and belongs to the field of organic chemistry. The method is characterized by comprising the following step: by adopting the three-compartment bipolar membrane electrodialysis device, continuously preparing 5-20% tetrabutyl ammonium hydroxide by using a 15-35% tetrabutyl ammonium bromide aqueous solution as a raw material under the condition that the reaction temperature is 30-60 DEG C, the current density is 200-600A / m<2> and the flow rate of the raw materials is 500-2000L / h, wherein the concentration of bromine ions in the prepared tetrabutyl ammonium hydroxide is less than 100ppm. According to the method provided by the invention, the materials in the compartments are relatively constant in concentration, the temperature is relatively constant, an ionic membrane is not easy to swell or shrink, the membrane cost is saved, the current efficiency and the product conversion ratio are improved and the energy consumption is reduced, and moreover, the product quality is further improved. The method is suitable for industrial safe production on a large scale, clean in production process and free of discharge of wastewater and solid wastes.
Owner:赵文洲

Synthetizing method of lacosamide

The invention provides a synthetizing method of lacosamide. The method comprises the steps of: based on D-serine as a raw material, performing an acylation reaction with acetic anhydride and then performing a condensation reaction with benzylamine; and finally, performing a methylation reaction with dimethyl sulfate, thereby obtaining lacosamide, wherein N,N' dicyclohexylcarbodiimide (DCC) or N,N' carbonyl diimidazole (CDI) is used as a catalyst in the condensation reaction; and a phase transfer catalyst including triethyl benzyl ammonium chloride (TEBA), tetrabutylammonium chloride (TBAC), tetrabutylammonium bromide (TBAB) or tetrabutylammonium hydrogen sulfate (TBAHS) is adopted in the methylation reaction. The method has the advantages of being simple in synthetizing process, moderate in reaction condition, simple in after-treatment, high in yield and high in product purity.
Owner:SUZHOU HONGRUI MEDICAL TECH

Electrochemical synthesis method for tetra-n-butylammonium tribromide

The present invention relates to an electrochemistry synthetic method of tetributyl tribromide of ammonium and belongs to the field of chemical formulation preparing technology. Sadi synthetic method in accordance with the present invention is as follow: dissolving tetrabutyl ammonium bromide in a aqueous solution of bromium salts such as ammonium bromide, potassium bromide or sodium bromide, magnetic-stirring it until reaching a entire solubilization, and then restirring it after adding organic solvent such as methylene dichloride or acetonitrile therein; putting the solution into an electrolytic tank of non-diaphragm type, selecting platinum meshwork as cathode and anode, inputting a constant electrical current for electroanalysis; electrolyzing for 3 hours under normal temperature and magnetic stirring to obtain tetributyl tribromide of ammonium in oil phase finally; washing the oil phase with distilled water, evaporating the organic solvent off and exposing it to air for a period of time, after the product solidifies, washing it with water, performing a recrystallization with methanol to obtain high-purity tetributyl tribromide of ammonium solid.
Owner:SHANGHAI UNIV

Synthesis method of Favipiravir

The invention belongs to the field of medicinal chemistry and particularly relates to a new synthesis method of Favipiravir. The method comprises the following steps: carrying out carboxyl protection on raw material shown in the formula (II) to generate a compound (III); carrying out diazotization hydrolysis reaction in the presence of concentrated sulfuric acid and sodium nitriteto generate a compound (IV); carrying out benzyl protection reaction to generate a compound (V), and then generating a compound (VI) in the presence of potassium fluoride and tetrabutylammonium bromide; removing a benzyl protection group to generate a compound (VII); and then adding an aminating agent to carry out amination to generate Favipiravir shown in the formula I. The method disclosed by the invention has the advantages that the reaction cycle is short, the operation is simple, the production cost is low, and the product is high in quality; therefore, the method is suitable for industrial production.
Owner:NANJING HUAWE MEDICINE TECH DEV

Method for preparing polymeric benzophenone derivative photoinitiator

The invention discloses a method for preparing a polymeric benzophenone derivative photoinitiator of which a formula is shown in the specification. According to the preparation method, epoxy group-contained benzophenone serving as a raw material and unsaturated carboxylic acid or unsaturated carboxylic ester are subjected to ring opening reaction in the presence of a polymerization inhibitor and tetrabutylammonium bromide to form the polymeric photoinitiator. Due to the existence of polymeric groups, the compatibility of the photoinitiator and a light polymerization system is improved, the surface mobility of the normal small molecular photoinitiator is greatly lowered in the photo-curing process, and the polymeric group can also be used as a monomer for synthesizing the macromolecular photoinitiator. Therefore, the preparation method has a wide application prospect.
Owner:HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH

High biomass content epoxy resin composition, and curing method and applications thereof

The invention discloses a high biomass content epoxy resin composition. The high biomass content epoxy resin composition comprises, by mass, 100 parts of epoxidized plant oil, 1 to 100 parts of unsaturated bio-based dicarboxylic acid, 1 to 10 parts of a curing accelerator 1, and 1 to 10 parts of a radical initiator; wherein the curing accelerator 1 is tetrabutylammonium bromide, triphenylphosphine, 2-methylimidazole, 2,4,6-tris(dimethylaminomethyl)phenol, or boron trifluoride, and the radical initiator is a peroxy curing agent or an azo curing agent. The invention also discloses a curing method and applications of the high biomass content epoxy resin composition. The high biomass content epoxy resin composition is capable of improving material mechanical properties greatly; the main raw materials come from biomass renewable resources, are both green and nontoxic, and possesses certain positive functions in alleviating oil crisis and reducing carbon dioxide release; damage on human body is reduced, environmental pollution is reduced, and it is beneficial for industrialized application and especially application in the field of paint.
Owner:NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI

Anticorrosive paint

The invention discloses anticorrosive paint which comprises, by mass, the following materials of 2-5 parts of allyl heptanoate, 1-4 parts of 4-methyl guaiacol, 1-2 parts of acetylacetone selenium, 4-9 parts of polyamide resin, 2-4 parts of 3-chlorine-2-carboxyl propyl trimethyl ammonium chloride, 1-3 parts of chromic chloride, 3-7 parts of vinylidene chloride, 2-5 parts of tetrabutylammonium bromide, 0.2-0.5 part of yttrium oxide, and 3-6 parts of decabromodiphenyl ether. The anticorrosive paint is not only convenient to use, easy to produce and manufacture, good in painting performance, and good in wettability for object surfaces, but also rapid in paint film drying, good in mechanical capacity, and good in acid-base resistance property, water resisting property, and resistance to organic solvent.
Owner:NANTONG HAISHUN CHEM

Preparation method of molybdenum dioxide nanorod

The invention discloses a preparation method of a molybdenum dioxide nanorod. The preparation method comprises the following steps of: by taking sodium molybdate as a molybdenum source, acetic oxide as an additive, dimethylformamide as a solvent, concentrated hydrochloric acid as an acidifier, and tetrabutylammonium bromide as a settling agent, through a simple experiment device and reaction steps, controlling concentration of molybdate suspension, an additive amount of the additive, a pH value of the solution and the amount of the settling agent, recrystalizing and purifying to obtain precursor tetrabutyl ammonium hexamolybdate; and thermally treating the precursor tetrabutyl ammonium hexamolybdate in a quartz tube under an inert atmosphere to have decomposition to obtain a monoclinic phase molybdenum dioxide nanorod. The method, prepared by the invention, has the advantages of low cost and high reaction yield, and capability of overcoming the vices of expensive instrument device, rigorous reaction conditions and reduction at high temperature with H2 with safety hidden trouble of the conventional preparation method.
Owner:XI'AN POLYTECHNIC UNIVERSITY

Preparation method of moisture-absorbing polyester fabric

InactiveCN107641966AGood hygroscopicityOvercoming the characteristics of poor hygroscopicityFibre typesFiberPolyester
The invention discloses a preparation method of a moisture-absorbing polyester fabric. The preparation method comprises the following steps of (1) preparing an alkaline treatment solution, impregnating polyester fibers into a solution, washing and drying; (2) preparing a sucrose fatty acid ester solution, impregnating the polyester fibers into the sucrose fatty acid ester solution, washing, and drying; (3) selecting a certain mass of raw silk, and preparing into 2 2 to 5% sericin solution; (4) preparing the following solutions comprising 8 to 12wt% of epichlorohydrin solution, 1 to 5wt% of tetrabutylammonium bromide solution, 1 to 3wt% of coupling agent solution, 30 to 50wt% of JCH solution with concentration of 0.3%, and 40 to 50wt% of sericin solution; (5) impregnating the polyester fibers into the solutions in step (4), washing, and drying; (6) performing secondary impregnating on the treated polyester fibers in step (5), washing, and drying; (7) preparing the polyester fibers intothe fabric. The preparation method has the advantage that the outer surface of the polyester fiber is coated with one layer of sericin, and the sericin has good moisture absorbing property, so that the defect of poor moisture absorbing property in the polyester fiber is overcome.
Owner:JIANGSU MEIHENG TEXTILE IND

Method for preparing cyclic carbonate

The invention discloses a method for preparing cyclic carbonate. The method specifically comprises the following step: with a quadri-aryloxy bridged rare earth metal compound as a catalyst, catalyzing carbon dioxide and alkylene oxide to react in the present of quaternary ammonium salt, wherein the general formula of the quadriaryloxy bridged rare earth metal compound is LLn(THF), wherein L refers to ethanediamine group bridged quadri-aryloxy, Ln refers to rare earth metal ions, and the quaternary ammonium salt is one of tetrabutylammonium iodide, tetrabutylammonium bromide, tetrabutylammonium chloride, tetraoctyl ammonium bromide, bis(triphenylphosphine) ammonium chloride and benzyl butyl ammonium bromide. The rare earth catalyst in the catalysis system is clear in structure, easy to synthesize, high in catalysis activity, less in using amount, mild in reaction conditions and wide in universality to alkylene oxide. According to the preparation method disclosed by the invention, raw materials are easily available, the reaction conditions are wild, a reaction substrate is wide in universality, the reaction time is short, the yield of the target product, namely the cyclic carbonate is high, and the reaction operation and the posttreatment process are simple.
Owner:SUZHOU UNIV

Favipiravir synthesis process

The invention relates to a favipiravir synthesis process, which comprises: 1) dissolving a pyrazine compound in an organic reagent I, adding an oxidizing agent M, and carrying out a nitrogen oxidation reaction to obtain a white solid; 2) adding the obtained white solid to an organic reagent II, and carrying out a chlorination reaction to obtain a pale yellow solid; 3) uniformly mixing the obtained pale yellow solid, a dried aprotic polar solvent, a dried fluorine ion donor reagent and tetrabutylammonium bromide, and carrying out a stirring reaction to obtain a pale yellow solid; 4) adding the obtained pale yellow solid to water, and carrying out a reaction with 1,4-dioxane and sodium acetate to obtain a yellow oily matter; and 5) uniformly mixing the obtained yellow oily matter and concentrated sulfuric acid to obtain the target product favipiravir. According to the present invention, the method has advantages of simple and easily available raw materials, simple synthesis process and mild conditions, nitrogen oxidation, chlorination, fluorization and hydrolysis are performed to finally prepare the 6-fluoro-3-hydroxypyrazine-2-formamide, and the good industrial value is provided.
Owner:WUHAN INSTITUTE OF TECHNOLOGY +1

Method for synthesizing quinolone medicaments

InactiveCN101781313ASolve the environmental odor problemRealize cleaner productionOrganic chemistryCarbonyldiimidazoleCarboxylate
The invention discloses a method for preparing quinolone medicaments. The conventional methods using organic solvents with a high boiling pint and a large polarity, adopting other solid alkali materials except reaction materials or using other liquid alkali materials except the reaction materials have obvious defects. The method of the invention adopts a technical scheme that: quinolone compounds are prepared by a piperazidine reduction of quinolone carboxylate nuclear parent and piperazidine derivates in water; the piperazidine reduction is completed in the presence of a catalyst which may be one or a mixture of more than two of cerous chloride heptahydrate, N,N-carbonyldiimidazole, 4-dimethylamino pyridine, tetrabutylammonium bromide, benzyl triethylammonium chloride and tetrabutyl ammonium hydroxide. The method for preparing the quinolone medicaments radically solves the problems of terrible smell, realizes clean production, avoids using the other alkali substances except the reaction materials as an acid-binding agent and overcomes the defects of the prior art.
Owner:ZHEJIANG JINGXIN PHARMA +1

Preparation method of ethylene carbonate

The invention belongs to the field of lithium battery electrolyte additive preparation, and particularly relates to a preparation process of ethylene carbonate. The method comprises: making monochloroethylene carbonate react with organic amine in an organic solvent in the presence of a catalyst; wherein the catalyst is a mixture of potassium bromide, sodium bromide, sodium iodide, potassium iodide, or any combination thereof and 18-crown ethers-6, tetrabutylammonium bromide or a combination thereof. The preparation method of the ethylene carbonate can improve a yield, the reaction condition ismild and environment-friendly.
Owner:ZHANGJIAGANG HUASHENG CHEM CO LTD

Method for grafting graphene oxide on biphenyl thermotropic liquid crystal compound

The invention discloses a method for grafting graphene oxide on a biphenyl thermotropic liquid crystal compound. The method comprises the following steps of: dissolving sodium hydroxide in absolute ethanol, adding 4,4'-p-hydroxyl biphenyl diphenol for reacting, adding ethanol, and continuing to react to obtain 4,4'-bis(beta-hydroxyethoxy)biphenyl(BP2); dissolving the sodium hydroxide in deionized water, dissolving the BP2 in N,N-dimethylformamide (DMF), reacting at the temperature of between 70 and 120 DEG C for 1 to 5 hours, and adding epichlorohydrin and tetrabutylammonium bromide, continuously reacting to obtain a biphenyl liquid crystal compound; and dripping SOCl2 in a graphene oxide mixed solution formed by ultrasonic wave dispersion for reacting, dissolving the biphenyl liquid crystal compound in the DMF, and mixing and continuously reacting to obtain a graphene oxide-grafted biphenyl liquid crystal compound. The preparation method is simple, pollution-free and low in cost, raw materials are wide in sources, and large-scale industrial production is facilitated.
Owner:福州乐道知识产权运营有限公司

Preparation method of high-purity fumaric acid tenofovir disoproxil fumarate

The invention discloses a preparation method of high-purity fumaric acid tenofovir disoproxil fumarate. The method comprises the following steps: (1) preparing tenofovir; (2) preparing tenofovir disoproxil fumarate, carrying out condensation reaction between tenofovir and chloromethyl isopropyl carbonate in an organic solvent under the action of a catalyst, purifying the product to obtain the tenofovir disoproxil fumarate, wherein the catalyst is a mixture of triethylamine and tetrabutylammonium bromide which are in the molar ratio of (22-30) to (1.5-3.0); the ratio of the triethylamine to the organic solvent is (22-30mol) to (150L-200L); and (3) preparing fumaric acid tenofovir disoproxil fumarate, salifying tenofovir disoproxil fumarate and fumaric acid which are obtained in the step (2), carrying out suction filtration, and drying to obtain the fumaric acid tenofovir disoproxil fumarate. According to the preparation method, dual catalysts are adopted in the process of preparing the tenofovir disoproxil fumarate, so that the yield and the efficiency of the tenofovir disoproxil fumarate are effectively increased, and the reaction process of the whole reaction is greatly shortened.
Owner:TAICANG YUNTONG BIOCHEM ENG

Improved systhesizing process for dicyclohexyl-18-crown-6

This is the modified synthesizing craft of dicyclohexyl-18-crown-6 (DCH18C6) belonging to the preparation field of crown ether compound. To solve the problems that the synthesizing production rate of the present DCH18C6 is low and the content of the cis three-dimensional isomereffective of the component DCH18C6 is low. The invention discloses the modified synthesizing craft and simple purifying method of cis three-dimensional isomereffective. In the systemization of DCH18C6, add tetrabutylammonium bromide to increase production rate and reduce reaction time, meantime it brings forward the purifying method of adopting toluene to have recrystallization. In the hydrogenation reaction, use acidic picher-ruthenium catalyst, increase temperature to 130 -140 Deg. C, the production rate can be increased to 90%, and promote the preparation of cis three-dimensional isomereffective; purify DCH18C6 cis three-dimensional isomereffective by the method of crystallizing in n-heptane. The synthesizing craft has strong practicability, low cost and high feasibility.
Owner:TSINGHUA UNIV

Method of synthesizing axungia alkyl dimethyl group amine oxide

A synthetic method of the fatty alkyl dimethyl amine oxide is provided, which belongs to the synthesis technology field of the amphoteric surface reactive agent in the organic chemical. The fatty alkyl dimethyl amine and the hydrogen peroxide are utilized as raw materials and perform oxidation reaction in the polar dielectric under the condition that the hydrogen peroxide stabilizer and the phase transfer catalyst exist; the sodium bisulfite is added to remove the residual hydrogen peroxide after reaction to produce the fatty alkyl dimethyl amine oxide; the phase transfer catalyst is the tetrabutylammonium bromide or the hexadecyl trimethyl ammonium bromide and the addition of the phase transfer catalyst is 1 per cent to 10 per cent of the weight of the fatty alkyl dimethyl amine; the mol ratio between the fatty alkyl dimethyl amine and the hydrogen peroxide is 1 : 1.0 to 1.5. The invention reasonably utilizes the phase transfer catalyst and greatly shortens the reaction time and increases the product yield through reasonably adjusting the addition and mixture ratio of the fatty alkyl dimethyl amine and the hydrogen peroxide and optimally selecting the reaction temperature and time.
Owner:王伟松

Dimer acid modified epoxy resin and preparation method therefor

The invention discloses dimer acid modified epoxy resin. The epoxy resin has a structural formula represented by a formula shown in the description. The invention also discloses a method for preparing the dimer acid modified epoxy resin. The method comprises the following steps: weighing epoxy resin, putting the weighed epoxy resin in a three-mouthed flask, adding dimer acid into the three-mouthed flask, introducing dry nitrogen gas into the three-mouthed flask, heating the three-mouthed flask to the temperature of 100-110 DEG C, and adding 2wt% of 1,4-dioxane into the three-mouthed flask; and after the temperature is maintained stable, adding a catalyst tetrabutylammonium bromide into the three-mouthed flask, stopping nitrogen gas introducing, adding a polymerization inhibitor into a system when the acid number of the system is lower than 30mgKOH / g during reaction, adding acrylic acid or methylacrylic acid into the three-mouthed flask, stopping the reaction when the acid number of the system is lower than 10mgKOH / g during the reaction, thereby obtaining the product. The dimer acid modified epoxy resin and the preparation method therefor have the advantages that the toughening effect is good, the functionality of modified resin is not changed, the curing rate is higher, and the hardness is not lowered obviously.
Owner:ANQING HONGTAI NEW MATERIAL

Preparation of high-catalytic activity Ti-based electrodes, Ti/nanoTiO2-RE2O3 and Ti/nanoTiO2-ZrO2

The invention relates to a convenient and fast method for preparation of high-catalytic activity Ti-based electrodes, Ti / nanoTiO2-RE2O3 and Ti / nanoTiO2-ZrO2, and a related key problem in the method is preparation of a modification material having high catalytic activity and stability. According to the invention, the process of sacrificial anodes is adopted, an inert electrode is used as a cathode, metallic Ti is used as a sacrificial anode, and a small amount of tetrabutylammonium bromide (Bu4NBr) is added into anhydrous ethanol as a conductive salt; ethyl titanate (Ti(OEt)4), a precursor of TiO2, is prepared through electrolysis; salt compounds of rare earth metals and zirconium metal are respectively added into ethyl titanate, and ethyl titanate is directly subjected to hydrolysis so as to respectively obtain rare earth metal doped composite nanometer TiO2 sol and zirconium metal doped composite nanometer TiO2 sol; pure titanium metal is used, the rare earth metal doped composite nanometer TiO2 sol and the zirconium metal doped composite nanometer TiO2 sol are respectively coated on Ti substrates having clean surfaces by using the Czochralski method, and electrodes modified by films doped with different metal oxides, i.e., Ti / nanoTiO2-RE2O3 and Ti / nanoTiO2-ZrO2 electrodes, are prepared after calcination.
Owner:HUAINAN NORMAL UNIV

Preparation method of cefditore

ActiveCN105175432AIngenious designAvoid the shortcomings of unsuitable storage and poor stabilityOrganic chemistryOrganic solventMethylene Dichloride
The invention belongs to the field of medicine synthesis, and particularly relates to a preparation method of cefditore. The method comprises the following steps that (1) under the photophobic condition, 7-ATCA and AE-active ester are added into methylene dichloride; catalysts are added; the temperature is lowered to 0 to 5 DEG C; triethylamine is added to obtain cefdiporen acid; a water solution of organic amine is added into organic solvents containing dissolved cefdiporen acid; crystal separation is carried out to obtain organic amine salts of the cefdiporen acid; (2) the organic amine salts of the cefdiporen acid take a reaction with iodomethyl pivalate under the existence of tetrabutylammonium bromide and sodium carbonate in N,N-dimethyl formamide to obtain the cefditore. The preparation method has the advantages that the organic amine salts of the cefdiporen acid are used; the defects of difficult storage and poor stability of the sodium salts of the cefdiporen acid are effectively avoided; E-shaped isomers are effectively removed; meanwhile, the esterification condition is optimized, so that the purity of final products is higher.
Owner:SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD

Method of preparing sodium azide

The invention discloses a making method of sodium azide, which comprises the following steps: dripping sulfuric acid in the solution with alcohol, sodium nitrite and water; aerating ethyl nitrite gas into solution with hydrazine hydrate, sodium hydroxide, tetrabutylammonium bromide and alcohol; generating sodium azide; evaporating solvent; crystallizing; separating solid from liquid to obtain the product.
Owner:ANHUI LANGXI LIANKE IND +1
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