74 results about "Fluoroacetic acid" patented technology

A method for producing an aromatic heterocycle-substituted difluoroacetic acid derivative having a partial structure represented by the formula (III), by reacting an N-oxido aromatic heterocyclic compound having a partial structure represented by the formula (I) with tetrafluoroethylene in the presence of a compound represented by the formula (II): R—YH, in a solvent selected from an aromatic hydrocarbon solvent, an ester solvent and an ether solvent:

The application relates to the technical field of metal organic thin layer material preparation, in particular to a kilogram-level preparation method of metal organic thin layer material. The preparation method comprises the following steps: S1, adding zirconium tetrachloride and H2BPYDC into a polytetrafluoroethylene reaction kettle, dissolving the zirconium tetrachloride and the H2BPYDC, and then adding a composite; S2, sequentially adding a DMF solution of palladium fluoroacetate, a catalyst and concentrated hydrochloric acid into the reaction kettle; S3, transferring the reaction kettle into an oven, centrifuging to obtain a cyan suspension after 18-20 hours, dispersing the cyan suspension in a DMF solution in batches at 60 DEG C, placing for 5-6 hours, removing unreacted substrates, and obtaining a solid; S4, cleaning the solid obtained in S3 by using DMF and tetrahydrofuran respectively, and vacuum drying for 12 hours to obtain the metal organic thin layer material. The kilogram-level preparation method of metal organic thin layer material is provided, so as to solve the problems of low preparation yield, slow rate and difficulty in kilogram-level preparation of metal organic thin layer material in the related art.

The invention discloses a preparation method and application of a silicon-based functionalized fluorenyl polysubstituted acetylene copolymer and a gas separation membrane thereof. Belongs to the technical field of polymer material and gas separation. The invention provides a new thought for preparation of a high-permeability gas separation membrane material. The preparation method comprises the following steps: carrying out copolymerization on 1-phenyl-2-(7-trimethylsilyl-9, 9-bis (trimethylsilyl-fluorene-2-yl) acetylene and 1-phenyl-2-(7-trimethylsilyl-9, 9-dimethyl-fluorene-2-yl) acetylene under the catalysis of TaCl5-n-Bu4Sn, so as to prepare a copolymer with high molecular weight; the preparation method comprises the following steps of: carrying out film casting on a solution of the nano-silver oxide, and then carrying out desiliconization treatment by using normal hexane / trifluoroacetic acid to obtain a gas separation membrane with the thickness of 100-220 microns, the specific surface area of 298-492 m / g and the total pore volume of 0.134-0.299 cm / g. The prepared separation membrane has the advantages that the COpermeability is up to 36,900 Barrer, the Opermeability is 19,800 Barrer, the thermal decomposition temperature exceeds 420 DEG C, the separation membrane can be used for separating gases such as COO, ON and the like, the preparation process is simple and convenient, and the industrial potential is realized.

FIELD: pharmacology.SUBSTANCE invention can be used to determine the concentration of an anti-tuberculosis drug in blood serum. The method for determining the concentration of bedaquiline in the blood serum in patients with tuberculosis or mycobacteriosis is that whole blood samples are centrifuged at 3000 rpm for 20 minutes, then the blood plasma is collected in sterile 1.5 mL Eppendorf tubes, then 900 mcL of acetonitrile are added to 300 mcL of plasma and centrifuged at 13500g for 15 minutes, then 1 mL of the supernatant is transferred to a chromatographic vial and make the assay by UHPLC MS / MS using an Athena UHPLC C18, 1.8 mcM, 120A, 2.1×100 mm chromatography column, when using an aqueous solution containing 5 g / L of ammonium acetate, 25 ml / L of concentrated acetic acid, 2 ml / L trifluoroacetic acid as mobile phase A and 100% acetonitrile as mobile phase B, the concentration of bedaquiline is determined using a pre-plotted calibration curve.EFFECT: determination of bedaquiline in human blood plasma in a time not exceeding 6 minutes.1 cl, 9 dwg, 6 tbl

The invention provides a method for preparing 2, 6-diamino-3, 5-dinitropyridine, which comprises the following steps: (1) reacting 2, 6-diaminopyridine with an amino protection reagent to obtain an intermediate A; (2) in the presence of a dehydrating agent, carrying out double nitration reaction on the intermediate A and a nitration reagent to generate an intermediate B; (3) 2, 6-diamino-3, 5-dinitropyridine is obtained after the intermediate B is subjected to deprotection, and an amino protection reagent is selected from one or more of acetic anhydride, trifluoroacetic anhydride, di-tert-butyl dicarbonate, benzyl chloroformate and concentrated sulfuric acid; wherein the molar ratio of the amino protection reagent to the 2, 6-diaminopyridine is (2: 1)-(30: 1) by mole; and preferably, the ratio is 2: 1-12: 1.

The embodiment of the invention provides a bromo-ethyl difluoroacetate-mediated novel amide dehydration cyaniding method, which comprises the following steps of: heating and reacting 0.2 mmol and 1.0 equivalent weight of amide compound and 0.6 mmol and 3.0 equivalent weight of bromo-ethyl difluoroacetate for 24 hours under an oil bath condition of 90 DEG C to generate an experimental reactant; concentrating the experimental reactant under reduced pressure to obtain a residue; and purifying the residue by silica gel rapid column chromatography to obtain the target product nitrile compound. According to the scheme, the process reaction conditions are mild, a strict anhydrous and anaerobic environment is not needed, the harsh requirements on equipment and operation are greatly reduced, and the production safety and practicability are improved. Acetone is used as a solvent, so that high-efficiency reaction can be realized, the solvent after reaction is convenient to recycle and recycle, the production cost and the environmental burden are remarkably reduced, and the remarkable green chemical engineering characteristic is embodied.

The invention belongs to the technical field of electrolysis, and discloses a method for preparing p-hydroxyanisole through electrolytic oxidation of anisole. The method comprises the following steps: S1, adding anisole, an acylation reagent, an organic alkali proton trapping agent and an alkaline amine group-containing solvent into a single-chamber electrolytic bath together, starting electrification, carrying out electrolysis, and obtaining a product liquid containing p-methoxytrifluoroacetic acid phenyl ester in the single-chamber electrolytic bath after electrolysis is finished; the organic base proton trapping agent is at least one of N, N-diisopropylethylamine, tributylamine and tripropylamine; and S2, adding a saturated sodium bicarbonate aqueous solution into the product liquid containing p-methoxytrifluoroacetic acid phenyl ester in the step S1 to hydrolyze p-methoxytrifluoroacetic acid phenyl ester, and extracting to obtain p-hydroxyanisole. The selectivity of para-position and ortho-position products of methoxyl on anisole is regulated and controlled, so that the selectivity of p-hydroxyanisole prepared by the method is higher.

This invention belongs to the field of responsive material production technology, specifically relating to a high-viscosity fluoropolymer solution and its applications. The preparation method of the high-viscosity fluoropolymer solution is as follows: (meth)acrylate naphthyl ester, fluorinated methacrylate, and vinylcarbazole are dissolved in a solvent and stirred to obtain a clear and transparent solution. Then, an initiator is added, and the mixture is heated to 60-90℃ under magnetic stirring for 16-24 hours to polymerize. After the reaction is completed, a transparent high-viscosity polymer solution with a viscosity range of 800-8000 Pa·s is obtained. After the high-viscosity fluoropolymer solution forms a film on the substrate, it forms an anti-counterfeiting coating that can be stimulated by ultraviolet light and trifluoroacetic acid, exhibiting excellent multi-stimulus responsiveness. The preparation method of this anti-counterfeiting coating is simple, has good film-forming properties, long service life, and low cost. It can be industrially produced and provides dual anti-counterfeiting capabilities, showing great application prospects in anti-counterfeiting, information encryption, and other fields.

The application relates to the field of biological medicine, and discloses an active oxygen response thione aldehyde linker as well as a preparation method and application thereof. The thione aldehyde linker structure is a thione aldehyde structure with a p-hydroxyphenyl as a center. The thione aldehyde carbon atom is connected with two -CH2CH2COOH groups through a sulfur atom. The preparation method of the active oxygen response thione aldehyde linker comprises the following steps: dissolving 3-mercapto propionic acid and p-hydroxybenzaldehyde in ethyl acetate, adding trifluoroacetic acid as a catalyst, stirring and reacting at room temperature, and after the reaction is completed, the thione aldehyde linker is obtained through separation and purification. The thione aldehyde linker can respond to the increased ROS level in a tumor microenvironment, is broken under a high ROS condition, and thus realizes the release of a drug molecule connected therewith, which is beneficial to realizing the specific release of the drug at a tumor site.

The invention relates to the field of macromolecules, and discloses a method for refining polyetherketoneketone and a polyetherketoneketone refined product. The method comprises the following steps: (1) treating a polyetherketoneketone complex by adopting a pretreatment agent; (2) the polyether ketone ketone crude product and a mixed chain supporting solution are mixed and washed, a first product is obtained, the mixed chain supporting solution comprises a main chain supporting agent and a cosolvent, the main chain supporting agent comprises one or more selected from parachlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid, the cosolvent comprises one or more selected from N, N-dimethylformamide and dimethyl sulfoxide, and the main chain supporting agent comprises one or more selected from dichlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid. The solvent is one or more of water, N-methyl pyrrolidone and N-methyl formamide; (3) adding a mixed aqueous solution into the first product to remove at least part of metal ions to obtain a second product; and (4) washing the second product for multiple times by using an organic solvent, and washing and drying to obtain the refined polyether ketone ketone. The content of aluminum ions in the polyetherketoneketone prepared by the method is low.

The application relates to the field of liquid chromatography analysis, and provides a method for high-performance liquid chromatography analysis of DNA dyes, which comprises the following steps: performing high-performance liquid chromatography analysis on a DNA dye-containing sample to be measured; wherein the DNA dye comprises at least one of PicoGreen and SYBR Green I; the high-performance liquid chromatography analysis adopts gradient elution, and mobile phase A, mobile phase B and mobile phase C are mixed in different proportions as mobile phases; the mobile phase A comprises at least one of acetonitrile and methanol; the mobile phase B comprises at least one of phosphoric acid aqueous solution, formic acid aqueous solution and trifluoroacetic acid aqueous solution; and the mobile phase C comprises ammonium acetate aqueous solution. The method can be used for detecting the purity of Picogreen, SYBR Green I and the DNA dyes, and realizes effective separation of target peaks and impurity peaks.

This invention belongs to the field of biochemistry technology, and relates to a near-infrared chemiluminescent probe responsive to tau protein, its preparation method, and its application. The preparation method of the near-infrared chemiluminescent probe includes the following steps: adding compound (I), compound (II), a catalyst, and an alkaline additive to a first solvent for reaction to obtain compound (III); adding compound (III), compound (IV), and piperidine to a second solvent for reaction to obtain compound (V); adding compound (V) and trifluoroacetic acid to a third solvent for reaction to obtain compound (VI); and adding compound (VI), compound (VII), and an acid compound to a fourth solvent for reaction to obtain the near-infrared chemiluminescent probe. The chemiluminescent probe of this invention exhibits high selectivity and efficient chemiluminescence capability, providing a promising tool for the diagnosis of Alzheimer's disease (AD). Its structural formula is: [Insert structural formula here].

The application relates to the technical field of compound synthesis, and discloses an aromatic dipeptide functionalized mercapto compound, 3,5-di(triphenylmethylthio)benzoic acid is obtained by adding 3,5-di(methylmercapto)benzoic acid and pyridine into a solution of chloromethyl triphenylphosphonium, purifying after sufficient reaction; then the 3,5-di(triphenylmethylthio)benzoic acid is mixed with N-hydroxysuccinimide and dissolved in an organic solvent, EDC.HCl is added, purifying after sufficient reaction; then 2,5-dioxopyrrolidin-1-yl 3,5-bis(triphenylmethylthiomethyl)benzoate is obtained; then phenylalanine-tryptophan and triethylamine are added, purifying after sufficient reaction; then (3,5-bis(triphenylmethylthiomethyl)benzoyl)tryptophylphenylalanine is obtained; then trifluoroacetic acid and triethylsilane are added, purifying after sufficient reaction; and finally the aromatic dipeptide functionalized mercapto compound is obtained. The aromatic dipeptide functionalized mercapto compound can quickly and effectively identify sodium and potassium ions, and has relatively low detection limit and relatively loose detection condition.

The invention discloses an HPLC (High Performance Liquid Chromatography) detection method for ipragmine hydrochloride enantiomers, and belongs to the technical field of pharmaceutical analysis. The HPLC detection method provided by the invention comprises the following steps: dissolving ipragmine hydrochloride to be detected in a diluent to prepare a test solution; detecting the test solution by adopting normal-phase high performance liquid chromatography; the stationary phase of the normal-phase high performance liquid chromatography is silica gel of which the surface is covalently bonded with cellulose-tri (3-chloro-4-methyl phenyl carbamate); a mobile phase of the normal-phase high performance liquid chromatography is a mixed solution of normal hexane, isopropanol, trifluoroacetic acid and diethylamine. According to the detection method established by the invention, the ipragmine hydrochloride main peak and the S-configuration enantiomer impurity peak can be subjected to baseline separation, the separation degree can reach 4.5 or above, the method is high in specificity and sensitivity, and various methodology verification parameters all meet the drug quality control requirements.

The invention belongs to the technical field of biochemistry, and relates to a ratio type probe compound, a preparation method thereof, a Cu (I) response photoacoustic probe composition and application. The preparation method of the ratiometric probe compound comprises the following steps: (1) reacting a compound (I), a compound (II), acetic acid and piperidine to obtain a compound (III); (2) reacting the compound (III) with trifluoroacetic acid to obtain a compound (IV); (3) carrying out a reaction on the compound (IV), the compound (V), 2-(7-azabenzotriazole)-N, N, N ', N'-tetramethylurea hexafluorophosphate and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, so as to obtain a compound (VI); and (4) reacting the compound (VI), the compound (VII), acetic acid and piperidine to obtain the compound. The photoacoustic probe provided by the invention has excellent selectivity and high sensitivity.

This invention discloses an acylhydrazone-linked covalent organic framework material, its preparation method, and its application, belonging to the field of covalent organic framework material synthesis technology. The preparation method of the acylhydrazone-linked covalent organic framework material is as follows: benzo[1,2-b:3,4-b':5,6-b”]trithiophene-2,5,8-tricarboxaldehyde, benzodiazepine, o-dichlorobenzene, and n-butanol are mixed to obtain suspension A; trifluoroacetic acid is added to suspension A and mixed to obtain mixture A; mixture A is sequentially subjected to freeze degassing and heating treatment, followed by extraction to obtain the final product. This invention uses benzo[1,2-b:3,4-b':5,6-b”]trithiophene-2,5,8-tricarboxaldehyde and benzodiazepine with a specific structure as main raw materials, and by adjusting the concentration, type, and amount of catalyst, an acylhydrazone-linked covalent organic framework material with higher crystallinity and stability is prepared.

The invention discloses a fluorine-containing medical intermediate ethyl difluoroacetate and a preparation method thereof, and belongs to the technical field of synthesis of organic fluorine compounds. The method comprises the following steps: firstly, taking tetrafluoroethylene and ethanol as raw materials, and reacting under the action of a basic catalyst to prepare an intermediate 1, 1, 2, 2-tetrafluoroethyl ether with stable properties; and then gasifying the intermediate, and performing catalytic cracking through a modified gamma-aluminum oxide catalyst bed layer subjected to specific high-temperature pre-fluorination treatment under the mild condition of 160-190 DEG C to generate high-activity difluoroacetyl fluoride in situ, and finally, directly introducing the cracking gas containing difluoroacetyl fluoride into a low-temperature reaction solution containing ethanol and an acid-binding agent without separation, and carrying out esterification reaction. According to the method, a brand-new synthesis route and a special catalyst are adopted, reaction conditions are mild, the cracking step selectivity is high, the production efficiency and the total yield are remarkably improved through integrated process design, and the technological process is simple, safe and reliable.

The application belongs to the technical field of biochemistry, and relates to a ratio type probe compound, a preparation method thereof, a Cu(I) response photoacoustic probe composition and application. The preparation method of the ratio type probe compound comprises the following steps: (1) reacting compound (I), compound (II), acetic acid and piperidine to obtain compound (III); (2) reacting compound (III) and trifluoroacetic acid to obtain compound (IV); (3) reacting compound (IV), compound (V), 2-(7-azabenzotriazole)-N,N,N',N'-tetramethyluronium hexafluorophosphate and 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride to obtain compound (VI); and (4) reacting compound (VI), compound (VII), acetic acid and piperidine to obtain the compound. The photoacoustic probe provided by the application has excellent selectivity and high sensitivity.

The invention relates to the technical field of batteries, in particular to a wide-temperature-range high-rate lithium battery ester-based electrolyte and application. The electrolyte comprises soluble lithium salt and a liquid component, the liquid component is a solvent; the solvent comprises at least three of propylene carbonate, fluoroethylene carbonate, isopropyl trifluoroacetate, ethyl trifluoroacetate, ethyl acetate, methyl acetate and methyl trifluoroacetate; the lithium salt lithium battery comprises at least two of common lithium salts. The electrolyte developed by the invention is used in the lithium battery and can stably work at 40-60 DEG C, the specific discharge capacity of the battery is still 62.83% of the specific discharge capacity of the battery at room temperature even at 30 DEG C and 4C multiplying power, and the electrolyte has excellent wide-temperature fast charge performance. In addition, the electrolyte effectively inhibits the growth of lithium dendrites and the side reaction of an electrode-electrolyte interface at low temperature, and promotes the formation of a solid interface film which is rich in inorganic matters and low in interface impedance. The invention has the advantages of reasonable component design and excellent product performance, and is convenient for industrial application.

The utility model relates to the technical field of trifluoroacetic acid processing, and discloses a solvent separation system for trifluoroacetic acid production. The first-stage extraction tanks and the second-stage extraction tanks are arranged, and one second-stage extraction tank corresponds to a plurality of first-stage extraction tanks, so that in the extraction layering process of the plurality of first-stage extraction tanks, liquid at a part of boundary lines can be fed into the second-stage extraction tanks to be extracted again, on one hand, continuous operation of the whole equipment is guaranteed, and on the other hand, the extraction efficiency is improved; on the other hand, the purity of the extracted finished product is improved. The liquid outlet pipe is respectively connected with the first discharge pipe, the second discharge pipe and the first pipeline to respectively correspond to the lower-layer liquid, the liquid at the middle interface and the upper-layer liquid of the first extraction tank, and the liquid is respectively drained into the first liquid collecting tank, the second liquid collecting tank and the material collecting tank.

The invention discloses an alpha-amino amide derivative and a synthesis method thereof. According to the synthesis method of the alpha-amino amide derivative, halogenated difluoroacetate, aromatic aldehyde or alkyl aldehyde and alkylamine or aromatic amine are used as raw materials, under the catalysis of metal copper salt, Bronsted acid is used as an additive, an organic reagent is used as a solvent, and the alpha-amino substituted amide derivative is obtained through a one-step reaction. The raw materials are cheap, easy to obtain, safe and non-toxic, the reaction conditions of the synthesis method are mild, the operation is simple and safe, and the synthesized alpha-amino substituted amide derivative can be widely applied to the fields of organic synthesis and drug research and development.

This invention provides a method for constructing HPLC characteristic chromatograms of processed medicinal slices, standard decoctions, and formulated granules of *Sophora flavescens*, comprising: A) dissolving and extracting the test sample raw material using a solvent to obtain a test solution; B) determining the test solution using high-performance liquid chromatography (HPLC) to obtain HPLC characteristic chromatograms of processed medicinal slices, standard decoctions, and formulated granules of *Sophora flavescens*; the HPLC chromatographic conditions are as follows: a C18 column; mobile phase A is acetonitrile solution, mobile phase B is 0.05% trifluoroacetic acid aqueous solution, and gradient elution is performed; specifically, the gradient elution is as follows: 0–15 min, phase A: 5%–11%, phase B: 95%–89%; 15–40 min, phase A: 11%–18%, phase B: 89%–82%; 40–60 min, phase A: 18%–21%, phase B: 82%–79%. This invention employs high-performance liquid chromatography (HPLC) with acetonitrile-0.05% trifluoroacetic acid solution as the mobile phase for gradient elution. Using magnoflorine, isocoryne, styraxine, and styraxine as references, a method for establishing characteristic HPLC chromatograms of processed slices, standard decoctions, and formulated granules of *Sophora flavescens* was developed. This provides more scientific technical means for controlling the medicinal quality of processed slices, standard decoctions, and formulated granules of *Sophora flavescens*.

The invention provides a preparation method of an upatinib intermediate, and relates to the technical field of organic synthesis. The preparation method comprises the following steps: mixing a compound as shown in a formula V, trifluoroacetic anhydride, a first alkaline compound and an organic solvent, and carrying out amidation reaction to obtain a compound as shown in a formula M; mixing the compound as shown in the formula M with a copper catalyst, a ligand, a second alkaline compound, a silicon acetylene reagent and an organic solvent, and carrying out a coupling-cyclization reaction to obtain a compound as shown in a formula N; and carrying out silicon group removal reaction on the compound as shown in the formula N under an acidic condition to obtain the upatinib intermediate (as shown in a formula II). According to the method, the cheap copper catalyst is used, and an unrecyclable expensive homogeneous palladium catalyst is abandoned, so that the cost can be greatly reduced, and industrial production is more facilitated; and the preparation method disclosed by the invention is high in yield.

The invention belongs to the technical field of medical imaging, and discloses a gallium-based radioactive contrast agent with glycosylation-modified maltotriose covalently linked with a chelating group as well as a preparation method and application of the gallium-based radioactive contrast agent. The preparation method comprises the following steps: firstly, modifying a cyclic polydentate ligand, carrying out nucleophilic substitution, then connecting an upper half flexible chain or loop chain, and then carrying out glycosylation on acetyl protected maltotriose to connect a sugar part half flexible chain or loop chain; the preparation method comprises the following steps: preparing a polydentate ligand, carrying out reductive amination or urea condensation connection on aldehyde groups or aldehyde groups on half-chain end groups on two sides to form a whole, adding methanol and a sodium methoxide solution, removing acetyl of sugar, adding trifluoroacetic acid to remove protective groups on the polydentate ligand, and finally adding 68Ga for chelation to obtain a final product. And maltotriose is adopted as a guiding group, so that higher bacterial specificity and permeability are achieved, and the distinguishing degree in diagnosis of bacterial infection is higher.

The invention discloses a method for preparing triphenyl sulfonium salt containing a ketal structure and purifying an isomer of the triphenyl sulfonium salt, which comprises the following steps: S1, carrying out condensation reaction on sodium difluoroacetate sulfonate and keto-containing alcohol to obtain keto-containing sodium difluorosulfonate acetate; s2, enabling the keto-containing sodium difluorosulfonate acetate to react with triphenyl sulfur chloride, so as to obtain keto-containing triphenyl sulfonium salt; s3, the keto-containing triphenyl sulfonium salt and D-ketonic acid lactone are subjected to a reaction, and a mixed product containing a ketal structure triphenyl sulfonium salt isomer is obtained; s4, dissolving the mixed product in C1-C4 fatty alcohol, cooling, crystallizing, filtering and drying to obtain a purified product; the content of the cis-triphenylsulfonium salt containing the ketal structure in the purified product is 95% or above. The obtained triphenyl sulfonium salt containing the ketal structure is stable in structure and good in solubility, the purity of the product is improved through C1-C4 fatty alcohol and a cooling crystallization method, and the problem of insufficient purity caused by poor batch stability in a synthesis process is effectively solved.

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of 2-bromo-5-trifluoromethylpyrimidine. According to the method, isoamyl nitrite is used as a nitroso donor, benzyltrimethylammonium bromide is used as a bromine source, and 5-trifluoromethyl-2-aminopyrimidine is used as a raw material to synthesize the target product 2-bromo-5-trifluoromethylpyrimidine. The method is simple in reaction condition and high in yield, and the yield can reach 65%. In addition, the invention further provides a preparation method capable of remarkably improving the reaction yield by adding trifluoroacetic acid, and the yield is 94% or above.

The invention provides a photocatalyst Zr-MOF and a preparation method and application thereof.The preparation method comprises the following steps that ZrOCl2 or ZrCl4, 3, 9-perylene diacid and biphenyldicarboxylic acid are mixed in an N, N-dimethylformamide solution according to a certain proportion, trifluoroacetic acid is added under the ultrasonic condition, a reactor is sealed and then placed in a drying oven to be heated, a reaction is conducted for 1-3 days at a certain temperature, and the photocatalyst Zr-MOF is obtained. Carrying out solid-liquid separation to obtain an HTU-1-x% crystal; or ZrOCl2 or ZrCl4 and 3, 9-perylene diacid are mixed in a N, N-dimethylformamide solution according to a certain proportion, trifluoroacetic acid is added under the ultrasonic condition, a reactor is sealed and then placed in a drying oven to be heated, a reaction is conducted for 1-3 days at a certain temperature, and HTU-1 crystals are obtained after solid-liquid separation. According to the scheme, the HTU-1 material is used for carrying out photoATRP reaction under green light catalysis, the use amount of Cu salt is effectively reduced, environmental pollution is reduced, the reaction conversion rate is high, controllability is good, and the excellent controllable polymerization effect under green light is achieved.

The invention belongs to the field of chemical synthesis, and particularly relates to a method for clean production of 5-methyl-3-(trifluoromethyl)-1H-pyrazole. Methyl trifluoroacetate is used as a raw material and reacts with acetone under the conditions of a solvent and a catalyst, a reaction solution is subjected to acidification and negative pressure distillation to obtain a trifluoroacetylacetone methanol solution, the trifluoroacetylacetone methanol solution directly reacts with hydrazine hydrate, and 5-methyl-3-trifluoromethyl-lH-pyrazole is obtained. The content of the 5-methyl-3-(trifluoromethyl)-1H-pyrazole obtained through the method reaches 99% or above, the two-step synthesis yield reaches 70%, and the method has the advantages of being high in product content, few in impurities, simple in technological process, convenient in solvent recovery and the like, and meets the requirement of clean production.

The application discloses a local high-concentration lithium metal battery electrolyte and a preparation method and application thereof. The electrolyte comprises a lithium salt, an organic solvent, an additive and a diluent; the organic solvent comprises at least one of methyl formate, methyl acetate, methyl propionate, methyl butyrate, ethyl propionate, ethyl acetate, ethyl butyrate, methyl trifluoroacetate and ethyl trifluoroacetate; the additive comprises at least one of fluoroethylene carbonate, lithium difluorobisoxalate phosphate and lithium difluorophosphate; and the diluent is a fluorine-containing ether compound. The local high-concentration electrolyte has the advantages of high-voltage resistance of high-concentration electrolyte and inhibition of corrosion of sulfonimide-based electrolyte on aluminum foil, meanwhile, the problems of high viscosity, low conductivity and poor impregnation with a separator of high-concentration electrolyte are overcome, the cycle performance and low-temperature performance of the lithium metal battery are significantly improved, and the local high-concentration electrolyte is particularly suitable for application in a low-temperature high-voltage lithium battery. The preparation method is simple, the cost is low, and the method is suitable for industrial production.

The invention provides a latent amine curing agent as well as a preparation method and application thereof. The curing agent is a mixture containing a compound with a structure I and a compound with a structure II, the structure of the compound with the structure I is shown in the specification, and the structure of the compound with the structure II is shown in the specification. The preparation method comprises the following steps: S1, carrying out primary amine substitution reaction on diamine and Boc anhydride (di-tert-butyl dicarbonate) to generate a secondary amine compound intermediate; and S2, carrying out secondary amine reactive hydrogen substitution reaction on the secondary amine compound intermediate and anhydride containing a fluoroacetic acid structure to obtain a mixture containing a structure I compound and a structure II compound. The latent amine curing agent not only has an excellent storage period and can be stably stored for more than three months after being matched with epoxy resin at room temperature, but also endows a cured product with excellent toughness and solvent resistance due to introduction of a carbamate structure, and has a good application value in the fields of epoxy SMC (Sheet Molding Compound), prepreg and the like.