42 results about "Caesium carbonate" patented technology

The invention provides a beta '-sulfo-alpha, beta-unsaturated gamma-lactam derivative as well as a preparation method and application thereof, and belongs to the technical field of organic chemical synthesis. The beta '-thio-alpha, beta-unsaturated gamma-lactam derivative has a structure as shown in a formula I. According to the method disclosed by the invention, cesium carbonate is taken as alkali, and a molecular skeleton of the beta'-thio-alpha, beta-unsaturated gamma-lactam derivative is constructed through free radical coupling and olefin isomerization processes under the condition of blue light irradiation. Bioactivity evaluation shows that the beta '-sulfo-alpha, beta-unsaturated gamma-lactam derivative prepared by the method disclosed by the invention has an inhibition effect on MDA-MB-231 human breast cancer cells.

The invention discloses a preparation method and application of a multimode luminescent cesium yttrium chloride lead-free perovskite luminescent material. In the specific synthesis process, firstly, precursor materials-cesium carbonate, yttrium carbonate and cerium acetate are dissolved in a mixed solution of glacial acetic acid and hydrochloric acid, and a precursor solution is obtained; then dissolving a certain amount of antimony acetate with acetonitrile to form an anti-solvent solution; and finally, adding the precursor solution into the anti-solvent solution to obtain the Sb / Ce double-doped cesium yttrium chloride lead-free perovskite luminescent material. During application, the Cs3YCl6 Sb and the Cs3YCl6 Sb / Ce luminescent materials are combined for use to form a pattern, and protected information can be decrypted through a specific excitation wavelength. According to the invention, the cesium yttrium chloride lead-free perovskite luminescent material capable of realizing multimode luminescence can be prepared in a short time.

The invention relates to a double-coordination passivated red-light perovskite quantum dot and a preparation method and application thereof. The preparation method comprises the following steps: preparing a monovalent cation precursor from cesium carbonate, 1-octadecene and oleic acid; preparing a lead source precursor from lead halide, zinc halide, 1-octadecene, diisooctyl hypophosphorous acid and oleylamine; thermally injecting the monovalent cation precursor into the lead source precursor, and cooling to prepare a perovskite quantum dot solution; performing anti-solvent purification on the perovskite quantum dot solution to obtain red light perovskite quantum dots; a process of preparing a double-coordination passivated red light perovskite quantum dot from the red light perovskite quantum dot and taurosulfonamide hydrochloride; the invention also discloses an application of the double-coordination passivated red light perovskite quantum dot prepared by the preparation method in preparation of an electroluminescent diode. The post-treatment passivation operation method is simple and convenient, and the quantum dot treated by the double-coordination ligand achieves the purpose of preparing the halide perovskite quantum dot with excellent optical performance and excellent performance of the prepared electroluminescent diode.

The invention discloses a catalyst for synthesizing 1, 3-dioxane-2-ketone as well as a preparation method and application of the catalyst. The catalyst is prepared from the following components in percentage by mass: 60wt%-90wt% of a component A, 5wt%-20wt% of a component B and 5wt%-30wt% of a component C, wherein the component A is one or more of N, N-dimethyl formamide, N, N-dimethylacetamide, N, N-diethyl formamide and urea, and the component B is one or more of N, N-dimethyl formamide, N, N-dimethylacetamide, N, N-diethyl formamide and urea; the component B is one or more of lithium carbonate, sodium carbonate, potassium carbonate, cesium carbonate, calcium carbonate and magnesium carbonate; and the component C is 1-butyl-3-methylimidazolium tetrafluoroborate and / or 1-butyl-3-methylimidazolium hexafluorophosphate, and the component C is 1-butyl-3-methylimidazolium hexafluorophosphate. According to the present invention, the components of the catalyst have the mutual synergistic promotion effect, the reaction substrate can be adsorbed and activated, the reaction condition is mild, the product yield is high, the catalyst can be recovered and regenerated, and the environmental pollution is low.

The invention discloses an alpha-dideuterium methylated sulfone compound as well as a synthesis method and application thereof, and belongs to the field of organic chemistry. In an air atmosphere, benzyl methyl sulfone and 2-((3, 5-dimethyl-4-methoxypyridine-2-yl) methylsulfonyl)-5-methoxy-1H-benzo [d] imidazole are used as substrates, in the presence of a catalyst [Cp * IrCl2] 2 and cesium carbonate, deuterated paraformaldehyde is used as a carbon source, sodium formate is used as an additive, and the alpha-dideuterium methylated sulfone compound is obtained through a reaction in an acetonitrile solvent at 120 DEG C. The reaction does not need to use a ligand and hydrogen, the reaction is simple and efficient, the potential value of the compound in medicinal chemistry is shown, and the compound has a certain inhibition effect on H3N2 subtype influenza viruses and has remarkable application potential.

This invention discloses an organic liquid energy storage carrier and its application, relating to the field of liquid organic hydrogen carrier technology. The organic liquid energy storage carrier of this invention is any one of p-fluorotoluene, m-fluorotoluene, o-fluorotoluene, and fluoromethylbenzene. The application method of this organic liquid energy storage carrier is as follows: 4Å molecular sieve, Rh catalyst, cesium carbonate, and the organic liquid energy storage carrier are sequentially added to a high-pressure reactor, and the reactor is sealed before hydrogen gas is introduced. Following this, microwave plasma pretreatment is performed, and then hydrogen gas is introduced until the pressure inside the reactor reaches 50 bar, followed by a hydrogenation reaction. After cooling, post-processing is performed to obtain the energy storage carrier. The organic liquid energy storage carrier of this invention not only possesses excellent safety and extremely low toxicity, but its application method also reduces reaction energy consumption and increases yield. Therefore, this invention has broader application prospects.

The application provides a kind of spectral analysis device and medical cesium carbonate preparation method, it is related to spectral detection technical field, including analyzer, analysis mechanism and bearing mechanism;The top of the analyzer is rotatably connected with the cover plate, the inside of the analyzer is fixedly provided with the mounting plate, and the outer wall of the mounting plate and inside the analyzer is fixedly provided with the side plate;The analysis mechanism includes the mounting sleeve fixedly arranged in the inside of the side plate, the top of the mounting sleeve is provided with the sealing plate, the inside of the mounting sleeve is slidably connected with the spring rod, and the inside of the mounting sleeve and the bottom end of the spring rod are fixedly provided with the lifting frame.The scheme can automatically explore the infrared generator during the process of turning over and closing the cover plate, and the two turning plates are synchronously turned to form an avoidance during the exploring process, so that the emission end of the infrared generator can be protected from being covered by external factors based on protection, which can effectively improve the spectral detection accuracy, and the infrared generator can be well protected to further improve the spectral detection accuracy.

The invention provides a high-purity spherical cesium iodide preparation method, which comprises: S1, dissolving cesium carbonate in pure water to obtain a cesium carbonate solution, carrying out a reaction on the cesium carbonate solution, hydrazine hydrate and an iodine simple substance, and carrying out solid-liquid separation to obtain a cesium iodide solution; s2, evaporating and concentrating the cesium iodide solution to a saturated state, cooling to room temperature by program temperature control, separating out cesium iodide, and then carrying out solid-liquid separation to obtain a cesium iodide wet material; s3, drying the cesium iodide wet material to obtain a first batch of cesium iodide; s4, washing the first batch of cesium iodide, and then carrying out solid-liquid separation to obtain a second batch of cesium iodide; s5, the second batch of cesium iodide is redissolved, an organic dispersing agent is added into the solution, evaporative crystallization is conducted under the stirring condition, then solid-liquid separation is conducted, and finally the high-purity spherical cesium iodide product is obtained.The technology is simple, operability is high, energy consumption is low, and large-scale production can be achieved.

The present disclosure broadly relates to a high temperature chemical process for the synthesis of cesium tungstate in the solid state and the preparation of aqueous solutions or deuterated solutions of cesium tungstate. More specifically, but not exclusively, the present disclosure relates to a high temperature chemical process in which tungsten oxide compounds such as tungsten oxides, or natural or synthetic concentrates such as wolframite or scheelite, tungsten industrial by-products or there mixture thereof, are mixed with cesium compounds such as cesium carbonate, or cesium sulfate, or cesium hydroxide or their mixtures thereof and the mixture is roasted in air or oxygen at high temperature inside a kiln. After cooling, the solid sintered mass containing cesium tungstate is leached or dissolved with water or heavy water for producing dense aqueous solutions or deuterated solutions of cesium tungstate.

The application provides a preparation method of a diaryl ether compound with higher yield, and belongs to the field of organic synthesis. The preparation method of the diaryl ether compound provided by the application has the following reaction formula: the method comprises the following steps: mixing and reacting a compound 1 or a salt thereof, a compound 2, a solvent and a base reagent, and then the diaryl ether compound is obtained. In the application, at least one of sodium carbonate, cesium carbonate or potassium carbonate is used as the base reagent, so that the target compound can be prepared with higher yield. In the application, the cesium salt is used as a reaction catalyst, so that the reaction time can be effectively shortened, and the reaction yield is further improved.

The application provides a method for defluorocyclization reaction of perfluoroalkyl tetrahydronaphthalenone and amidine compound and cobalt-1,3-dicarbonyl complex under the promotion condition of cesium carbonate, and a series of fluorine alkyl substituted furan quinazoline compounds are synthesized. The strategy is free from the dependence on multi-step pre-functionalization and transition metal catalysis in the traditional synthesis path. In the reaction process, six carbon-fluorine bonds at three perfluoroalkyl carbon sites of the polyfluoroalkyl ketone are continuously broken, five carbon-carbon / carbon-nitrogen / carbon-oxygen bonds and two heterocycles are constructed through one-pot method, the accurate synthesis of the fluorine alkyl substituted furan quinazoline compound is realized, and the method has the characteristics of mild condition, good functional group tolerance, simple post-treatment, green step, low pollution and high economic benefit; and the obtained compound shows certain inhibition activity on human malignant melanoma (A-375) cells.

The invention relates to the technical field of organic synthesis, in particular to a sulfentrazone synthesis method which comprises the following steps: mixing a substrate II, a polar aprotic solvent and cesium carbonate, heating while stirring, and introducing chlorodichloromethane gas for reaction to obtain an intermediate product III; mixing the intermediate product III, concentrated nitric acid and silver nitrate, and heating for reaction to obtain an intermediate product IV; mixing the intermediate product IV, a solvent and water; then adding palladium-carbon, carrying out nitrogen displacement, introducing hydrogen, starting stirring and heating for reaction to obtain an intermediate product V; heating the intermediate product V, dichloroethane and phosphide under a stirring condition; dropwise adding methanesulfonic acid; and after the methanesulfonic acid is dropwise added, heating and reacting to obtain a product I, namely sulfentrazone. According to the method, the unique steps 1, 2, 3 and 4 are combined, so that the total yield of sulfentrazone is increased by 20% or above, and the production process is green and environment-friendly.

The invention discloses a method for synthesizing a pyrazole methylene phenol derivative, which comprises the following steps: by taking p-methylphenol and a derivative thereof as well as pyrazole and a derivative thereof as raw materials, reacting under mild conditions without a metal catalyst and a stoichiometric amount of redox reagent; the corresponding para-substituted phenol derivative is prepared through a one-step electrosynthesis reaction by stirring an easily available electrode under the conditions of room temperature, anhydrous cesium carbonate, an acetonitrile solvent and constant current. The method provided by the invention has the advantages of low price, reaction at room temperature and mild reaction conditions, provides a convenient way for oxidation of p-methylphenol, the obtained p-substituted phenol is a key structure motif of many natural products and drug intermediates, and the method is simple and convenient in synthesis operation, environment-friendly, free of special protection and wide in industrial production prospect.

The invention discloses a three-dimensional network imino covalent organic framework material as well as a preparation method and application thereof, and belongs to the field of materials. A specific number of multi-aldehyde benzene series and multi-amino benzene series are subjected to a Schiff base reaction, in the preparation process, a mode of combining ultrasonic dispersion and mechanical oscillation is adopted to ensure that reactants are uniformly mixed, and efficient polymerization can be realized at room temperature in cooperation with the synergistic catalysis of acetic acid or cesium carbonate and aniline or benzaldehyde; reaction conditions are mild and easy to control, damage of high temperature and high pressure to a material structure is avoided, meanwhile, directional assembly of a covalent organic framework is promoted through a solvent in a specific proportion and solvent types, formed imine bonds are stably combined, functional groups in a molecular structure endow the material with good chemical activity, and the covalent organic framework material is prepared. The accurate reaction of the multi-aldehyde benzene series and the multi-amino benzene series successfully constructs a three-dimensional network spherical structure.

The application provides a beta'-thio-alpha, beta-unsaturated gamma-lactam derivative and a preparation method and application thereof, and belongs to the technical field of organic chemical synthesis. The beta'-thio-alpha, beta-unsaturated gamma-lactam derivative has a structure shown in formula I. The method constructs a beta'-thio-alpha, beta-unsaturated gamma-lactam derivative molecular skeleton through a free radical coupling and olefin isomerization process under the condition of blue light irradiation with cesium carbonate as an alkali. Through biological activity evaluation, it is found that the beta'-thio-alpha, beta-unsaturated gamma-lactam derivative prepared by the method has an inhibitory effect on MDA-MB-231 human breast cancer cells.

The invention discloses a method for synthesizing lead-free Cu: CsBr perovskite (Cu: CsBr NCs) stable in an aqueous solution by using a one-pot method, which comprises the following steps of: selecting cesium carbonate, copper bromide and citric acid as reactants, and oleic acid and oleylamine as surface ligands, adding a proper amount of octadecene or mineral oil, performing ultrasonic treatment to obtain a Cu: CsBr-coated CC solution, and centrifuging, purifying and drying the solution to obtain the lead-free Cu: CsBr-coated CC perovskite (Cu: CsBr NCs) stable in the aqueous solution. Cu: CsBr (at) CC powder is obtained. The method disclosed by the invention is simple to operate, short in time and good in repeatability, can be synthesized by only one step, and the prepared compound is good in solubility in an aqueous solution, excellent in dispersity, stable in fluorescence and easy to store.

The invention provides a method and a device for separating alum compounds from lepidolite pickle liquor at low temperature and preparing high-purity rubidium carbonate and cesium carbonate. The method for separating the alum compounds from the lepidolite pickle liquor at low temperature and preparing the high-purity rubidium carbonate and cesium carbonate comprises the following steps that S1, lepidolite raw materials which are crushed and pass through a 200-mesh standard sieve are placed in a reaction device, water vapor is introduced for roasting to obtain lepidolite clinker, then sulfuric acid is added for an acid leaching reaction, continuous stirring is conducted, and lepidolite powder is obtained; and after the reaction is finished, filtering to obtain an acid leaching solution. According to the method for separating the alum compound from the lepidolite pickle liquor at low temperature and preparing the high-purity rubidium carbonate and cesium carbonate, the alum compound is converted into the soluble salt through high-temperature roasting, and the subsequent rubidium and cesium leaching rate is greatly increased, so that the recovery rate of metal resources is increased, and the raw material cost is saved; and a pure solution containing rubidium and cesium is obtained through multi-step adjustment of the pH of the leachate, and meanwhile, the purity of a metal product needing to be recycled is improved.

This invention discloses a method for synthesizing α-hydroxycarboxylic acid compounds. The method includes the following steps: adding a reaction substrate, a photosensitizer, and a base to a dry reaction tube; then adding a solvent and additives under a CO2 atmosphere; and reacting under visible light irradiation. After the reaction is complete, the reaction system is acidified and quenched, and then purified to obtain the product, the α-hydroxycarboxylic acid compound. The photosensitizer includes Ir(ppy)2(dtbbpy)PF6 and 3DPA2FBN; the base is potassium tert-butoxide, cesium carbonate, or potassium tert-valerate; the additives are N,N-diisopropylethylamine and chlorosilane; and the reaction substrate is an aldehyde or ketone compound. This invention provides a highly efficient and selective synthesis of α-hydroxycarboxylic acid compounds under visible light induction and a CO2 atmosphere. The reaction conditions of this invention are mild, the reactant range is broad, the selectivity is good, and it can be scaled up to the gram scale.

The application relates to the technical field of pharmaceutical intermediates, and provides a preparation method of a Resmetirom key intermediate III. The application uses a compound with a structure shown in formula V and a compound with a structure shown in formula E to prepare the Resmetirom key intermediate III, the preparation steps are simple and easy to operate, expensive silver nitrate, cesium carbonate, isopropenyl magnesium bromide and lithium chloride do not need to be used, the product yield is high, the intermediate products are all solid, purification is convenient, moreover, the method provided by the application has small solid waste and waste liquid, is good in environmental protection, finally, the compound with the structure shown in formula G used by the application is stable in property and is not easy to be oxidized. In summary, the method provided by the application can significantly reduce the production difficulty and production cost of the Resmetirom key intermediate III, and is more beneficial to industrialized production.

The application provides an infrared absorption substance, a preparation method thereof and an ink. The preparation method of the infrared absorption substance comprises the following steps: preparing a first solution, a second solution and a third solution, mixing the first solution, the second solution and the third solution to obtain a mixed solution, and standing the mixed solution for a preset standing time; the first solution contains a copper phosphate salt, the second solution contains sodium tungstate dihydrate, and the third solution contains cesium carbonate and citric acid; the mixed solution is synthesized by using a hydrothermal synthesis method to obtain a solid-liquid mixture; and the solid-liquid mixture is washed with water, washed with alcohol, centrifuged and dried to obtain the infrared absorption substance. The infrared absorption substance has an infrared absorption rate of 85% or more in the infrared wave band of 850 nm-1250 nm.

A synthesis method of the nano material comprises the following steps: by taking a mixed solution of hydrochloric acid and ethanol as a solvent, adding oleic acid and octylamine, and stirring; continuously adding a hydrochloric acid solution containing cesium carbonate, and magnetically stirring; and washing the product with isopropanol, centrifuging, and drying to obtain the nano material. According to the method, the surface of the nano material is coated with the precursor through two organic ligands including oleic acid and octylamine, so that the nano material is good in dispersity and uniform in size, the method is easy and convenient to operate, the preparation time is short, high temperature is not needed, energy loss is effectively reduced, and an experimental basis is provided for controllable preparation and surface engineering of the nano material; the application in the fields of light-emitting devices, light detection and the like is promoted. And meanwhile, the prepared nano material can be directly applied to the scintillator, and an additional grinding step is not needed, so that the production efficiency is remarkably improved.

The application relates to a preparation method of an NHC-PdCl2-3-chloropyridine complex, which comprises the following steps: reacting 2,6-diisopropylaniline, glyoxal and acetic acid in an ethanol solvent for 2-4 days to obtain glyoxal-bis-(2,6-diisopropylphenyl) imine; stirring and reacting a mixed solution of the glyoxal-bis-(2,6-diisopropylphenyl) imine, chloromethyl ether, tetrahydrofuran and water at 30-50 DEG C for 10-20 hours to obtain 1,3-bis(2,6-diisopropylphenyl) imidazolium chloride, and the molar ratio of the glyoxal-bis-(2,6-diisopropylphenyl) imine to water is 1:2%-10%; reacting 1,3-bis(2,6-diisopropylphenyl) imidazolium chloride, palladium chloride, cesium carbonate and 3-chloropyridine at 60-100 DEG C for 10-20 hours to obtain [1,3-bis(2,6-diisopropylphenyl) imidazol-2-ylidene](3-chloropyridyl) palladium (II) dichloride, the method has the advantages of easy raw material acquisition, simple operation, mild and easy-to-control reaction conditions and convenience in industrial large-scale production.

The invention relates to a synthesis method of oseltamivir phosphate, which comprises the following steps: by taking (1R, 5R, 6R)-trans-5-(1-ethyl propoxy)-7-oxobicyclo [4.1. 0] hept-3-ene-3-carboxylic acid ethyl ester as a starting raw material, reacting with acetonitrile under the catalysis of indium chloride to synthesize (3aR, 4R, 7aR)-2-methyl-4-(pent-3-alcohol oxy)-3a, 4, 7, 7a-tetrahydrocyclohexene [2, 1-d] [1, 3] oxazole-6-ethyl formate; the preparation method comprises the following steps: synthesizing (3R, 4R, 5S)-4-(acetamido)-5-[(diphenylmethylene) amino]-3-(pent-3-oxyl) cyclohexene-1-ethyl formate by using ethyl acetate as a raw material, performing ring-opening reaction with benzophenonimine under the catalysis of cuprous iodide and cesium carbonate to synthesize (3R, 4R, 5S)-4-(acetamido)-5-[(diphenylmethylene) amino]-3-(pent-3-oxyl) cyclohexene-1-ethyl formate, hydrolyzing benzophenone to synthesize oseltamivir, and reacting with phosphoric acid to synthesize oseltamivir phosphate. The method has the advantages of short synthetic route, low cost, easily available initial raw materials, simple operation, few and controllable reaction impurities, and suitableness for industrial production.

The application provides a kind of CsPbBr3 perovskite quantum dot material and preparation method thereof, and relates to perovskite nanocrystal preparation technical field.The method comprises the following steps: (1) cesium carbonate, lead acetate, octadecene and dodecyl benzene sulfonic acid are mixed, heated under inert gas protection, to obtain the precursor solution of cesium source and lead source;(2) oleylamine and hydrogen bromide are mixed under inert gas protection to obtain the oil hydrobromide precursor solution;(3) the precursor solution of (1) is heated and injected into the precursor solution of (2), mixed and then cooled to obtain a quantum dot colloid crude solution;(4) the solution of (3) is centrifuged, and the supernatant is added with a detergent and then centrifuged again, and the precipitate is collected and dried to obtain the CsPbBr3 perovskite quantum dot material.The surface ligand of the cesium lead bromide quantum dot prepared by the application has strong binding force with the quantum dot, and is not easy to fall off, thereby showing higher colloidal structure stability.

The invention discloses a preparation method of large-particle-size nickel hydroxide in the field of inorganic functional materials. According to the method, particle size control is achieved through a strategy of combining step-by-step parallel flow feeding and guiding agent regulation and control. The method comprises the following steps: firstly, synchronously dropwise adding a nickel salt with relatively high concentration and alkali liquor into a reaction base solution containing ammonia water and the guiding agent, generating a uniform crystal nucleus under a weakly alkaline condition, and ageing; next, nickel salt with relatively low concentration and alkali liquor are dropwise added synchronously, and crystal nucleus epitaxially grows under a slightly strong alkaline condition; and finally, aging, washing and drying to obtain the product. Vanadium pentoxide is activated by hydrogen peroxide and then reacts with cesium carbonate, layered cesium vanadate is prepared through hydrothermal crystallization, and then the layered cesium vanadate is subjected to surface modification by a silane coupling agent to obtain the guiding agent. The heterogeneous nucleation and growth guiding effects of the guiding agent are utilized, and a two-step feeding process is cooperated, so that homogeneous nucleation is effectively inhibited, controllable synthesis of nickel hydroxide with the particle size within a target range is realized, the process is stable, and the repeatability is good.

The invention provides tail liquid cesium ion trace detection equipment and a high-purity cesium carbonate preparation process, and relates to the technical field of cesium ion trace detection, the tail liquid cesium ion trace detection equipment comprises a detection table, a reaction tank, a pushing mechanism, a sample liquid extrusion mechanism and a detection mechanism; a mounting seat is mounted in the detection table, an electric turntable is mounted in the mounting seat, a positioning plate is fixedly arranged at the top of the electric turntable, the reaction tank is positioned above the positioning plate, a side frame is mounted on the side wall of the mounting seat and positioned on one side of the reaction tank, and the detection table adopts an ECL mode for detection. According to the scheme, the detection sample liquid is pushed into the reaction tank in a pushing extrusion mode, the volume, the flow velocity and the mixing state of the sample liquid can be accurately controlled through the design, which is crucial to the accuracy and the stability of trace cesium ion detection, and the pushing extrusion mode can ensure that the volume of the sample liquid injected into the reaction tank each time is consistent; and a reliable basis is provided for subsequent generation of light-emitting signal detection concentration quantitative matching.

The invention discloses a near-infrared two-region fluorescent molecule as well as a preparation method and application thereof, and the preparation method comprises the following steps: (1) reacting a compound 3 with a compound 7 under the action of cesium carbonate and PdCl2 (dppf). CH2Cl2 to synthesize a compound 8; (2) reacting the compound 8 under the action of zinc powder to synthesize a compound 9; and (3) reacting the compound 9 with a sulfur trioxide pyridine complex SO3. Py to synthesize the target compound LJW-4S. The fluorescent molecule has excellent water solubility, and the in-vivo metabolism efficiency of the fluorescent molecule can be remarkably improved; meanwhile, the sulfonic acid group introduced into the structure can effectively enhance the fluorescence quantum yield after being combined with in-vivo plasma protein, so that high-sensitivity imaging is realized on the premise of ensuring the biological safety.

The application discloses a preparation method of a photoetching coating, which comprises the following steps: S1, mixing titanium white powder and cesium carbonate, calcining to obtain a solid; S2, acid dipping the solid, solid-liquid separation, adding the obtained solid phase into a tetramethylammonium hydroxide solution to stir, and peeling to obtain a titanium dioxide dispersion liquid; S3, adding a coupling agent into the titanium dioxide dispersion liquid to modify, solid-liquid separation, and ball milling to obtain modified titanium dioxide; S4, dissolving a hydroxyl-terminated hyperbranched polyester in a solvent, adding the modified titanium dioxide, ultrasonic dispersion, adding a vinyl-terminated compound to mix to obtain a mixed liquid; and S5, coating the mixed liquid on a substrate, and heating and curing to obtain the photoetching coating. The prepared photoetching coating has a high refractive index, is easy to remove through developing, and can be used for preparing a photomask plate.

The invention relates to a synthesis method of 4H-benzo [d] [1, 3] dioxane-4-ketone and a derivative thereof, salicylic acid and the derivative thereof can easily realize various functional reactions, because the salicylic acid and the derivative thereof widely exist, have abundant reaction sites and are low in price, the synthesis method is undoubtedly a simple organic synthesis strategy. Salicylic acid and derivatives thereof not only can be subjected to simple coupling reaction with R-NH2 and R-X, but also can be subjected to reaction with CH2X2 to synthesize 4H-benzo [d] [1, 3] dioxane-4-ketone, and in the air atmosphere, the reaction temperature is reduced, and the reaction time is shortened. Bis (triphenylphosphine) nickel chloride (20mol%) is used as a catalyst, triphenylphosphine (0.5 equivalent) is used as a ligand, cesium carbonate (1.5 equivalent) is used as alkali, ethyl acrylate (4.0 equivalent) is used as an additive, and a target product is formed through reaction at 90 DEG C for 16 hours. According to the scheme reported by the invention, the conditions are simple, the raw materials are cheap and easy to obtain, the reaction can be directly carried out in the air atmosphere without external gas, the method has step and atom economy, and various 4H-benzo [d] [1, 3] dioxane-4-ketone and derivatives thereof can be effectively obtained.

The invention discloses a synthesis method of propargyl alcohol, calcium carbide, formaldehyde and / or polyformaldehyde and water react in an organic solvent in the presence of a catalyst and basic carbonate to obtain propargyl alcohol, the catalyst comprises a quaternary ammonium salt catalyst and / or a cesium carbonate catalyst, and the organic solvent comprises dimethyl sulfoxide. Compared with a traditional synthesis method, the propargyl alcohol synthesis method has the advantages that the catalyst is easier to obtain and lower in price, the requirement on equipment is lower, the operation is simpler and more convenient, and propargyl alcohol can be prepared with lower cost and higher efficiency. In addition, the propargyl alcohol synthesis method is safe in reaction and free of escape of a large amount of gas, and a closed reaction container does not need to be specially used. The propargyl alcohol synthesis method is more suitable for industrial production of propargyl alcohol and has higher economic benefits.