87 results about "2,2,2-Trifluoroethanol" patented technology

The invention relates to a tissue engineering material and a preparation method thereof, in particular to a nano fiber tissue engineering blood vessel and a preparation method thereof. The invention consists of a three-dimensional reticular non-woven film formed by an inner layer of nano fiber and an outer layer of nano fiber; the inner layer of the blood vessel is natural polymer, wherein, calculated by weight, 40 percent to 80 percent is fibroin, 20 percent to 50 percent is gelatine, 0 percent to 20 percent is extracellular matrix protein; while the outer layer of the blood vessel is synthetic polymer. The preparation method is that the natural polymer is dissolved in trifluroroethyl and other solution, while the synthetic polymer is dissolved in hexafluoroisopropanol and other solution, which are respectively prepared into spinning solution; the static electricity spinning technique is adopted to subsequently form the inner and the outer layers on a gather roller; cross-linked treatment is conducted after the inner and the outer layers are taken down, to prepare the nano fiber tissue engineering vessel. The inner layer can simulate the structure of the extracellular matrix, provide good environment for endothelial cells to grow, support adhesion, proliferation and differentiation of the cells, and is good for endothelization of the blood vessel; and the outer layer has good mechanical performance.

A process for preparing hydrofluoroether features the reaction between one of trifluoroethene, tetrafluoroethene, hexafluoro propene, etc and one of trifluoroethanol, trifluoropropanol, metanol, etc in organic solvent (DMF or DMSO). Its advantages are high output rate and easy purifying and separating.

The invention relates to a paclitaxel-loaded sustained release nano-fibre material which comprises the components of bio-degradable polymer material and pure paclitaxel, the mol ratio of which is 1.33 to 10. The diameter of the nano-fibre is 90nm to 1.44micrometer, and the drug-loading rate can be regulated within the range of 0 percent to 100 percent. The preparation of the nano-fibre comprises the steps as follows: (1) the bio-degradable polymer material is solved in organic solvent and stirred to be solved completely to obtain lamella spinning solution A; (2) the white pure paclitaxel powder is solved in trifluoroethanol and stirred to be solved completely to obtain core spinning solution B; (3) clear transparent solutions A and B are respectively added into two injectors; the speed of a microinjection pump, the voltage of a static generator and the receiving distance between a grounded aluminum foil and a spinning needle are adjusted, and unordered drug-loaded nano-fibre is obtained by a coaxial electrostatic spinning technology. A nanometer control release system composed by the drug-loaded nano-fibre effectively controls the sustained release of the drug and is applied to the preparation of the drug for remedying malignant tumor.

A liquid/liquid extraction method is used for separating a perfluorinated polyether (PFPE) into two molecular-weight distributions using an alcohol or cyclic ether as one solvent and a fluorinated solvent as the other solvent. The more polar alcohol or cyclic ether solvent extracts the lower molecular weight PFPE and the less polar fluorinated solvent extracts the higher molecular weight PFPE. In addition, when the PFPE is a mixture of PFPEs with different end groups, such as a mixture of predominantly Z-Tetraol but with other PFPEs with Z-Dol end groups, there is an enrichment of the Z-Tetraol in the more polar solvent. The preferred PFPE is a mixture of PFPEs in as-purchased Z-Tetraol and the preferred solvents are methanol or trifluoroethanol as one solvent and a perfluorinated hydrocarbon, such as perfluorohexane, as the other solvent.

The invention discloses a method for synthesizing chiral benzosultam via palladium-catalytic asymmetric hydrogenation, comprising the following reaction conditions that: the temperature is 25-70DEG C; a solvent is 2,2,2-trifluoroethanol; the pressure is 28-40atm; the proportion of a substrate to a catalyst is 50/1; the catalyst is a complex of palladium trifluoroacetate and diphosphine ligand; the benzo six-membered ring shaped sulfonyl enamine of the benzo is hydrogenated to obtain the corresponding chiral benzo six-membered sultam with an enantiomeric excess up to 98%; and the benzo five-membered ring shaped sulfonyl enamine is hydrogenated to obtain the corresponding chiral benzo five-membered sultam with an enantiomeric excess up to 94%. The method disclosed by the invention is simple, convenient and practical for operation, high in enantioselectivity, good in yield and environmentally friendly, and has green atom economy for the reaction.

The invention discloses a preparation method and application of a water-soluble SnO2 inorganic semiconductor nanomaterial. The preparation method comprises the following steps: dissolving SnCl4.5H2O into a mixed solvent of water and ethanol, and adding a 8-10% tetramethylammonium hydroxide water solution; then, carrying out a hydro-thermal synthesis reaction; and carrying out acetone precipitationto obtain the water-soluble SnO2 inorganic semiconductor nanomaterial. The water-soluble SnO2 inorganic semiconductor nanomaterial disclosed by the invention not only has excellent dispersibility inwater, but also has relatively good dispersibility in trifluoroethanol, so that the water-soluble SnO2 inorganic semiconductor nanomaterial can be used for coating an ITO or perovskite film by using aspin-coating method to obtain an SnO2 film; and the preparation method is safe, simple, low in cost and environment-friendly.

The invention discloses diisocyanate having fluorine-containing branched chain, a preparation method and application of diisocyanate having fluorine-containing branched chain in waterborn fluorine-containing polyurethane. The diisocyanate is prepared from (by weight parts) 6-10 parts of trimethylolpropane, 100-120 parts of isophorone diisocyanate, 5-20 parts of 2,2,2-trifluoroethanol and 0.06-1.8 parts of catalyst by stirring trimethylolpropane at 100-120 DEG C under vacuum for dehydration, adding isophorone diisocyanate and 0.03-0.9 parts of catalyst under the protection of nitrogen, reacting at 80-85 DEG C for 2-3 h, adding 2,2,2-trifluoroethanol and the rest of catalyst, and further reacting at 80-85 DEG C for 2-3 h. The diisocyanate is used for preparing waterborn fluorine-containing polyurethane, and the obtained waterborn fluorine-containing polyurethane has flexibility, elasticity, and good tensile strength, elongation at break, and contact angle with water.

The invention provides a preparation method of naphthonone and analogues thereof, which is simple in reaction condition, simple in after-treatment, high in yield and low in production cost. According to the preparation method, in the presence of alkali, a compound shown by a general formula (I) reacts with a compound shown by a general formula (II) or (III) at room temperature by taking multi-fluorine alcohol as a solvent to prepare a compound shown by a general formula (IV) or (V), and the chemical equations are shown in the specification, wherein R is H, C1-C4 alkyl, chlorine or bromine, R' is H or C1-C4 alkyl, X is chlorine or bromine, the multi-fluorine alcohol is trifluoro-ethanol or hexafluoro-isopropanol, and the alkali is sodium carbonate, potassium carbonate, trifluoro-ethanol sodium or triethylamine.

The invention relates to a trifluoromethyl substituted azide polymer and a preparation method thereof. The structural formula of the trifluoromethyl substituted azide polymer is as shown in the description, wherein x is an integer ranging from 3 to 5, m is an integer ranging from 1 to 30, and n is an integer ranging from 1 to 30. The preparation method comprises the steps that trifluoroethanol and epichlorohydrin which serve as the raw materials are subjected to a debydrochlorination reaction, and trifluoroethanol methyl ether ethylene oxide is obtained; trifluoroethanol methyl ether ethylene oxide and epichlorohydrin are both monomers, and the trifluoromethyl substituted azide polymer is obtained through the steps of cation ring opening polymerization, azidation and the like. A trifluoromethyl substituted azide polymer synthetic route is economical and practical, and a wide application value in the aspect of energetic binders is achieved.

The invention relates to a method for preparing exenatide, and solves the problems that cost is high, yield is low, impurity (des-Glu<15>, Glu<16>-exenatide) content is relatively large and large-scale production cannot be realized in the prior art. The concrete steps comprise: A) taking amino resin as initial resin, employing an Fmoc solid-phase synthesis method, according to the peptide sequence of the exenatide main chain to successively couple with amino acids with Fmoc protection at N terminal and with protected side chains, wherein in the amino acid coupling reactions of the peptide sequence 15-17, a solution DMF is added with 2,2,2-trifluoroethyl alcohol accounting for 20% by volume of the solution and 1.5 mol/L of urea; and B) after peptide resin is subjected to cracking, employing a reverse-phase filling material for first purification, and employing anion resin for second purification, desalinating to enable the content of impurities des-Glu<15>, Glu<16>-exenatide to be reduced to 0.1% or less, and performing freeze drying, so as to obtain exenatide. The method is a low-cost preparation technology suitable for large-scale production of exenatide with high purity, and the technology is capable of effectively controlling the content of des-Glu<15>, Glu<16>-exenatide and does not influence the yield of exenatide.

The invention provides a method for synthesizing 1,4-diketone compound by using 2-halogenated cyclopentanone as a raw material. In the presence of alkali, 2-halogenated cyclopentanone reacts with silyl enol ether in perfluoroalkyl alcohol used as a solvent to obtain a 1,4-diketone compound, wherein perfluoroalkyl alcohol is trifluoroethanol or hexafluoroisopropanol, and the alkali is selected from sodium carbonate, potassium carbonate, sodium trifluoroethanol, triethylamine and pyrrolidine . The synthesis method provided by the invention has advantages as follows: raw materials are easily available; costs are low; reaction conditions are mild; operation is simple and easy to control; there exists less side reaction; post-treatment is simple; product yield is high; and the solvent can be recovered and recycled so as to greatly save production cost. The method has good environmental protection benefit and economic benefit and is suitable for industrial production.

The invention discloses a preparation method of a polycarboxylate superplasticizer with high viscosity reduction performance. The preparation method comprises the following steps: reacting trifluoroethanol with a double bond-containing enoic acid acyl chloride compound to generate a viscosity-reducing functional monomer I, reacting maleic anhydride with a straight-chain diol compound to generate aviscosity-reducing functional monomer II, finally preparing a special solution A, a special solution B and a special solution C, and dropwise adding the solutions A, B and C into a water phase systemto react to obtain the finished product. Compared with common PCE, the polycarboxylate superplasticizer has a good viscosity reduction effect, and the flowing time and T500 are obviously shortened; an emulsion polymerization method is adopted, the reaction polymerization efficiency is high, the molecular weight distribution of the prepared product is more uniform, and the molecular structure andperformance of the product are more stable; and the phenomena of high viscosity, bottom scrabbling and the like caused by low water-binder ratio in the mixing process of the high-strength concrete canbe effectively solved.

The invention relates to a preparation method of an insoluble drug sustained-release film. The preparation method comprises the following steps of dissolving GelMA in trifluoroethanol to obtain a clear transparent solution, adding an insoluble drug, and uniformly mixing to obtain a spinning solution; then pouring the obtained spinning solution in a liquid feeding device, and performing electrostatic spinning to obtain a GelMA nanofiber loaded with the drug; soaking the whole nanofiber film loaded with the drug in a polymer solution containing an optical crosslinking agent; and finally, taking out the nanofiber film, triggering a crosslinking reaction under UV-irradiation, and performing crosslinking curing on the nanofiber, thereby obtaining the drug sustained-release film. The process is simple and low in cost; and the preparation method can be widely applied to sustained release of various insoluble drugs, and has a good application prospect.

The invention relates to a high-purity fluorine-containing organophosphorus flame retardant and a preparation method thereof. The preparation method comprises the following steps: (1) preparation of trifluoroethyl phosphate, namely adopting phosphorus oxychloride and trifluoroethanol of which the total molar weight ratio is (1:3)-(1:6), adding a catalyst which accounts for 2%-10% of total weight of reactants, carrying out catalytic reaction at the temperature of 10-90 DEG C for 2-16 hours, carrying out reduced pressure distillation for 1-5 hours to remove insufficiently reacted phosphorus oxychloride and trifluoroethanol after the catalytic reaction is completed, and then carrying out suction filtration to obtain the catalyst capable of being recycled and a crude trifluoroethyl phosphate product; (2) purification and refining of the trifluoroethyl phosphate, namely refining phosphate by adopting a continuous rectification process, adding a drying agent to the crude trifluoroethyl phosphate product so as to remove moisture contained in a to-be-purified substance, rectifying by introducing into a low-boiling removing rectifying column, condensing high-purity trifluoroethyl phosphate rectified through multi-times column chromatography into liquid, namely the high-purity trifluoroethyl phosphate flame retardant contained in the electrolyte of a lithium ion secondary battery, by virtue of a condenser, wherein the purity is more than or equal to 99.9%, and the yield is more than or equal to 92%.

The invention discloses a preparation method of vinyl alkylphosphonate, the vinyl alkylphosphonate and application of the vinyl alkylphosphonate. The preparation method of the vinyl alkylphosphonatecomprises the following steps: A, performing a mixing reaction: mixing phosphorus oxychloride and hexamethyldisiloxane to react for 1 hour; B, adding a catalyst: adding a catalyst into a reacted solution in step A, wherein the catalyst is gamma-aluminum oxide nanofibers; C, carrying out a dropwise adding reaction: dropwise adding a mixed solution of ethylene glycol and trifluoroethanol or a mixed solution of ethylene glycol and allyl alcohol into the reacted solution obtained in step B, controlling the temperature to be 80-90 DEG C in the dropwise adding process, and carrying out heat preservation reaction for 5 hours after dropwise adding is finished; and D, carrying out reduced pressure distillation: collecting 100-120 DEG C/(10-15) mmHg fractions to obtain the vinyl trifluoroethyl phosphate or vinyl allyl phosphate. The method has the beneficial effects of simple process, easiness in operation, low energy consumption, simple feeding mode, few byproducts, high product yield and high product purity.

The invention relates to a method for synthesizing chiral 3-trifluoromethyl-3, 4-dihydroquinoxalinone by palladium-catalyzed asymmetric hydrogenation. A catalytic system is a chiral diphosphorus complex of palladium, and the reaction conditions are as follows: the temperature is 0-80 DEG C, the solvent is 2, 2, 2-trifluoroethanol or hexafluoroisopropanol, the pressure ranges from 100 psi to 1000 psi, the ratio of the substrate to the catalyst is 33/1, the used metal precursor is palladium trifluoroacetate, and the used chiral ligand is a chiral diphosphorus ligand. The preparation method of the catalyst comprises the following steps: stirring a metal precursor of palladium and a chiral diphosphine ligand in acetone at room temperature, and then carrying out vacuum concentration to obtain the catalyst. Corresponding chiral dihydroquinoxalinone containing trifluoromethyl can be obtained by hydrogenating quinoxalinone containing trifluoromethyl, and the enantiomeric excess of the dihydroquinoxalinone containing trifluoromethyl can reach 99%. The method is simple, convenient and practical to operate, high in enantioselectivity and high in yield, and the reaction has green atom economyand is environmentally friendly.

The method of catalyzing hydrogenation of ketone enantioselectively with homogeneous Pt catalyst system has chiral diphosphorus complex of Pt as catalyst system, reaction temperature of 25-75deg.c, solvent of 2, 2, 2-trifluoroethanol, reaction pressure of 3-70 atm and chiral diphosphorus ligand used. The homogeneous Pt catalyst system is prepared through mixing metal precursor of Pt and chiral diphosphorus ligand at room temperature and the subsequent vacuum concentrating. The catalyst can result in asymmetrical inducing as high as 92 % on alpha-one-benzamide substituted ketone. The present invention has simple operation, facile material, high reaction selectivity, high yield and environment friendship.

The invention discloses a preparation technology of a UV-resistant hydrophobic material. Perfluorooctyl acrylate, acrylic acid and hydroxyethyl acrylate serve as raw materials, azodiisobutyronitrile serves as an initiator, and a perfluorooctyl acrylate homopolymer is prepared through reasonable reaction temperature setting and a dripping technology; the perfluorooctyl acrylate homopolymer, isocyanate, a silane coupling agent and trifluoroethanol are mixed in proportion to prepare a UV-resistant hydrophobic film liquid. The UV-resistant hydrophobic film liquid is used for being sprayed on the surface of a glass base material or a ceramic base material and has the characteristic of normal-temperature curing or low-temperature curing, and a formed film layer has good UV resistance and ageingresistance and has good adhesive force on the glass base material and the ceramic base material.

The invention relates to a trifluoroethanol/difluoroethanol reagent and a preparation method and an application thereof, the chemical structural formula of the trifluoroethanol reagent is shown in thespecification, in the formula, R1, R2 and R3 represent substituent groups on silicon atoms, and R1, R2 and R3 are independently selected from aryl, heteroaryl and alkyl respectively. The trifluoroethylation reagent and the difluoroethylation reagent provided by the invention can be used as synthesis intermediates of a plurality of organic compounds, some of the compounds have pharmaceutical activity, the preparation steps of the compounds are simplified, and the synthesis method is mild in condition and wide in substrate applicability.

The invention discloses a preparation method and application of a gold nanoparticle based nano-enzyme. According to the preparation method, a polypeptide is modified to the surface of a gold nanoparticle through an Au-S bond and is induced to represent an alpha-helical structure on the gold nanoparticle with trifluoroethanol, so that a triplet is catalyzed to be positioned in a corresponding spatial position to form a charge relay network, and advanced simulation of a natural hydrolase from the molecular level. The nano-enzyme has excellent performance of difficult degeneration due to the stability of the Au-S bond; after the trifluoroethanol is removed, the nano-enzyme still as a stable secondary structure and excellent catalytic activity. The nano-enzyme has a simple synthesizing methodand high catalyzing efficiency. The method selects the gold nanoparticle as a rigid frame and can greatly improve the stability of the nano-enzyme, and the surface of the nano-enzyme is formed by conformation adjustable polypeptides and has a flexible dynamic secondary structure. The conformation adjustment of the nano-enzyme enables a group without a function to have a function and is an advancedsimulation of natural enzyme.

The invention relates to the field of organic chemicals, aims to solve the problems that a solvent is used and the reaction yield is low in the synthesis process of vinyl tri(2,2,2-trifluoroethoxy) silane, and discloses a method for preparing the vinyl tri(2,2,2-trifluoroethoxy) silane. The method comprises the following steps: adding dropwise trifluoroethanol into vinyl trichlorosilane which is maintained to a certain temperature in advance, keeping the temperature to implement a reaction, increasing the temperature till refluxing, and maintaining the refluxing process; cooling the reaction material to the room temperature so as to obtain a crude synthesis produce, neutralizing the system by using an alkali neutralizer, performing filtering, and collecting filtrate; and transferring the collected filtrate into a rectification tower, and performing treatment, so as to obtain the vinyl tri(2,2,2-trifluoroethoxy) silane. The method is simple in operation condition, simple in step, free of extra solvent except raw materials for reactions, high in target product yield, easy in separation and purification, and very applicable to large-scale production.

The invention relates to a method for selectively preparing an alpha-acyloxylation or beta-acyloxylation product of an enamine ketone compound. When the alpha-acyloxylation product of the enamine ketone compound is selectively prepared, the enamine ketone compound and PIDA are added into trifluoroethanol according to the proportion of 1.0:1.3 and stirred for 0.5-3 hours at room temperature to obtain the alpha-acyloxylation product. When the beta-acyloxylation product of the enamine ketone compound is selectively prepared, the enamine ketone compound and PIDA are added into a reaction vessel according to the proportion of (1:1)-(1:2), water and solvents are added, and the materials are stirred for 3-6 hours at the room temperature to obtain the beta-acyloxylation product. The process is simple, reaction conditions are mild, the alpha-acyloxylation product of the enamine ketone compound can be effectively prepared in a high-yield manner, and the beta-acyloxylation product of the enamineketone compound can be selectively rearranged to obtain a beta-acyloxylation alpha, beta-unsaturated amide compound.

The invention discloses a synthesis method of trifluoroethoxy vinyl phosphate, and relates to the technical field of battery electrolyte additives. The synthesis method comprises the following steps: taking phosphorus oxychloride and hexamethyldisiloxane for pre-reaction, dropwise adding ethylene glycol and trifluoroethanol, and carrying out esterification reaction to obtain the trifluoroethoxy vinyl phosphate. According to the invention, the phosphorus oxychloride, the ethylene glycol and the trifluoroethanol are taken as raw materials and are directly subjected to cyclization reaction, and dichloromethane is added as a solvent to disperse a reaction system, so that severe side reaction can be reduced, and the reaction is promoted to proceed towards a required reaction direction. According to the method, the reaction process is simple, raw materials used in the reaction are easy to obtain, the reaction process is milder and safer compared with the prior art, and the yield of the product is further improved by reasonably controlling the dosage of the reaction raw materials and the reaction process, so that the yield reaches 32.61% or above, and the purity reaches 99.5% or above.