234 results about "Acetic oxide" patented technology

The invention relates to a method for synthesizing 6-methyl-17alpha-acetoxyl-19-norpregnane-4,6-diene-3,20-diketone. The method comprises the following steps: 1) reacting acetylene with estrone-3-methyl ether so as to obtain 17alpha-acetenyl estrone-3-methyl ether; 2) carrying out Birich reaction at a low temperature; 3) carrying out alkene etherification on the product obtained in the step 2); 4) carrying out a Vilsmeier reaction on the product obtained in the steps 3); 5) reacting the product obtained in the step 4) with benzene sulfenyl chloride; 6) reacting the product obtained in the step 5) with sodium methoxide and trimethyl phosphate; 7) reducing the formoxyl at the 6-position of the product obtained in the step 6); and 8) reacting the product obtained in the step 7) with Pd-C/cyclohexene, then reacting with acetic oxide so as to obtain the target product 6-methyl-17alpha-acetoxyl-19-norpregnane-4,6-diene-3,20-diketone. By using the method, the operation is simplified, and theproduction cost is reduced; and the reactions involved in the invention are simple to operate, and the yield is high.

The invention discloses a method for preparing ultra-high heat resistant polyimide polymer. The method includes the following steps: dissolving aromatic-diamine containing carborane component and traditional aromatic dianhydride or aromatic dianhydride containing the carborane component and traditional aromatic-diamine into DMF or DMAc, carrying out ring opening polymerization to obtain polyamic acid; adding proper amounts of acetic oxide and pyridine into the obtained polyamic acid solution, stirring at room temperature for appropriate time, adding a proper amount of methyl alcohol to precipitate solid, and drying the solid to obtain polyimide containing the carborane component. According to the method provided by the invention, the 5% weight loss temperature of the prepared polyimide in nitrogen is greater than 600 DEG C, and that in the air is greater than 1000 DEG C, which are higher than those of the currently developed polyimide materials.

The related catalyst system comprises Rh compound as catalyst, all of alkyl iodide, heteropoly salt and alkali iodide together as promoter. This invention is fit to prepare acetyl oxide by carbonylating methyl acetate or acetic acid by methanol.

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.

The invention relates to a chemical synthetic method, and concretely relates to a synthetic method of a perfume o-tert-butylcyclohexyl acetate. The synthetic method comprises the following steps: reacting a raw material phenol with isobutene under the catalysis of anhydrous aluminum trichloride to obtain o-tert-butyl phenol, carrying out catalytic hydrogenation of o-tert-butyl phenol under the catalysis of Raney nickel to obtain o-tert-butyl cyclohexanol, and carrying out an esterification reaction of o-tert-butyl cyclohexanol and acetic anhydride under the catalysis of anhydrous sodium acetate to obtain o-tert-butylcyclohexyl acetate. The method has the advantages of mild reaction conditions, safe and convenient operation, high reaction yield, fine and strong fragrance of the obtained product, raw material source enlargement and raw material cost saving because of the adoption of industrially cheap phenol and isobutene as initial raw materials, total synthetic reaction yield improvement, suitableness for the industrial adoption, and good economic benefit.

The invention discloses a process and a device for synthesizing peroxyacetic acid. The process includes: enabling acetic anhydride and hydrogen peroxide to be respectively and intensively mixed in a micro-mixer, entering a micro-channel reactor with the length of 1-10m and the inner diameter of 0.5-2.0mm, enabling the reaction temperature to be 10-70 DEG C and the retention time to be 2-10min, and synthesizing to obtain the 5-30wt% peroxyacetic acid. The synthesis device comprises a constant flow pump, the micro-mixer, the micro-channel reactor and a water bath, wherein the constant flow pump is connected with the micro-mixer which is connected with the micro-channel reactor, and the micro-channel reactor is disposed in the water bath.

The invention discloses a preparation method of a banana cellulose crystallite/polylactic acid aerogel. The preparation method comprises the following steps: step one, taking banana cellulose crystallite and ionic liquid and blending the banana cellulose crystallite and the ionic liquid, then performing reflux condensation for 3 hours under the protection of nitrogen at the constant temperature of 100 DEG C, then adding acetic oxide for modification, and then continuously stirring for 3 hours at the temperature of 90 DEG C under the protection of nitrogen to obtain a banana cellulose crystallite hydrosol; and step two, firstly taking polylactic acid and dichloromethane in the mass-to-volume ratio of 1.8: 10, dissolving the polylactic acid in the dichloromethane, then putting the banana cellulose crystallite hydrosol obtained in the step one into the dichloromethane dissolved with the polylactic acid, and then blending to obtain a crude banana cellulose crystallite/polylactic acid aerogel product. The invention also discloses the banana cellulose crystallite/polylactic acid aerogel. The invention also discloses use of the banana cellulose crystallite/polylactic acid aerogel for oil absorption.

The invention relates to a preparation method and application of an efficient corn straw adsorbent. The preparation method of the efficient corn straw adsorbent particularly comprises the following steps: cleaning corn straw, drying, crushing, sieving and dewaxing; then adding nitrilotriacetic acid into a mixed organic solution containing acetic anhydride and an activator, stirring at 60-70 DEG C, adding the corn straw after reaction, stirring at 70-80 DEG C, and separating, washing and drying after reaction so as to obtain the efficient modified corn straw adsorbent. The adsorbent can be used for removing heavy metal ions such as Cd<2+> and Pb<2+> in wastewater, has the absorbing capacity reaching up to 100mg/g and 160mg/g respectively for heavy metal ions of Cd<2+> and Pb<2+>, has the characteristics of simple preparation method, high absorbing capacity, reusability, adsorption stability and no secondary pollution, and also achieves resource utilization of biomass resources.

The invention relates to a method for synthesizing 5-bromoindole. The method comprises the following steps of: (1) dissolving indole into alcoholic organic solvents, adding an aqueous solution of sodium hydrogensulfite or potassium hydrogensulfite, reacting for 15 to 20h, filtering a reaction solution, washing, and drying to obtain an intermediate I; (2) mixing the intermediate I and acetic anhydride, raising the temperature to 68 to 75 DEG C, reacting for 2 to 3h, adding ester or benzene organic solvents, reacting for 0.5 to 1h, cooling to room temperature after the reaction is finished, filtering, washing, and drying to obtain an intermediate II; and (3) dissolving the intermediate II into water, adding bromine at the temperature of between 0 and 5 DEG C, keeping the reaction for 1 to 3h, raising to room temperature, continuing to react for 1 to 2h, adding the aqueous solution of sodium hydrogensulfite or potassium hydrogensulfite, reacting for 10 to 30min, adding an aqueous solution of sodium hydroxide or potassium hydroxide, refluxing for 12 to 18h, cooling a reaction solution, precipitating crystals, filtering, washing, and drying to obtain a product, namely the 5-bromoindole. The method is low in cost consumption and is simple, and the quality of the product is high.

The invention discloses a high selectivity method for synthesizing moxifloxacin. The method comprises the following steps of: reacting boric anhydride with trifluoro acetic anhydride to obtain a chelant; reacting 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid ethyl ester with the chelant, cooling to room temperature, adding ice water, performing suction filtration, and washing a filter cake with water until neutrality to obtain a 1-ethyl-7-chloro-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methyl ester trifluoroacetic anhydride boronized chelate; and reacting the 1-ethyl-7-chloro-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methyl ester trifluoroacetic anhydride boronized chelate with (S,S)-2,8-diazabicyclo[4,3,0]nonane to obtain a 1-cyclopropyl-6-fluoro-7-([S,S]-2,8-diazabicyclo[4,3,0]nonane-8-methoxy-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid ethyl ester trifluoroacetic anhydride boronized chelate, recycling a solvent under reduced pressure, adding alkali, refluxing, discoloring, filtering, freezing, performing suction filtration, and drying a filter cake. The method is simple, mild in conditions, and high in selectivity, avoids difficultly separated impurities, is high in reaction yield and product purity, and is suitable for industrial production.

The invention belongs to the field of synthesis of acetic acid and acetic anhydride through carbonylation, and relates to a lithium pyridine carboxylate-rhodium acetate complex catalyst for synthesizing acetic acid and acetic anhydride through carbonylation of methanol, and a preparation method and application of the catalyst. When the catalyst is used for catalyzing carbonylation reaction of the methanol to prepare the acetic acid and catalyzing carbonylation reaction of methyl acetate to prepare the acetic anhydride, the catalyst has good catalytic activity and reaction stability. Under the relative mild conditions, the catalyst can catalyze the carbonylation of the methanol to prepare the acetic acid and catalyze the carbonylation of the methyl acetate to prepare the acetic anhydride at high speed and high selectivity. The catalyst has an active ingredient of rhodium; and a coordination structure formed by the rhodium active ingredient and the lithium pyridine carboxylate is shown as the specifications.

The invention provides a method for preparing a BiFe1-xCrxO3 ferroelectric film by using a sol-gel method. The method comprises the following steps of: dissolving bismuth nitrate, ferric nitrate and chromic nitrate according to a molar ratio of 1.05: (1-x): x into a mixed solution containing ethylene glycol monomethyl ether, acetic oxide and cholamine, and magnetically stirring to obtain a stable BiFe1-xCrxO3 precursor with the metal ion concentration of 0.003-0.3mol/L, wherein x is equal to 0.00-0.03, and the volume ratio of the ethylene glycol monomethyl ether to the acetic oxide to the cholamine is 14: 5: 1. A film is prepared by spin-coating the BiFe1-xCrxO3 precursor on an FTO (Fluorine-doped Tin Oxide)/glass substrate by using a spin-coating method, and a crystalline BiFe1-xCrxO3 film is obtained by adopting a layer-by-layer annealing process. The method disclosed by the invention has simple requirements on equipment, and experimental conditions are easy to achieve; the prepared film is better in uniformity, and the doping amount is easy to control; and the ferroelectric property of the BiFeO3 film is improved through B-bit Cr doping.

The invention provides a preparation method of a low-leakage current Bi0.92Tb0.08Fe(1-x)CrxO3 film. The method comprises the following steps of: dissolving bismuth nitrate, ferric nitrate, terbium nitrate and chromic nitrate at a molar ratio of 0.97:(1-x):0.08:x into the mixed solution of ethylene glycol monomethyl ether and acetic anhydride to form a mixed solution; adding ethanolamine into the mixed solution to adjust the viscosity and the complexing degree to obtain a stable BiFeO3 precursor liquid; and preparing a Tb and Cr co-doped crystalline BiFeO3 film by a spin-coating method and layer-by-layer annealing technology. The film is a crystalline Bi0.92Tb0.08Fe0.99Cr0.01O3 film, wherein the leakage current density is still kept below 10<-4>A/cm<2> in a 150kv/cm test electric field. According to the method provided by the invention, the requirements on equipment are simple, the experimental conditions are easy to realize, the prepared film has good uniformity, and the leakage current of the film is reduced through the co-doping of Tb and Cr.

The invention discloses a synthesis method of medroxyprogesterone acetate. The method comprises the following steps of: 1) enabling 17 alpha-hydroxyprogesterone and ethylene glycol to perform ketalation under the catalysis of para-toluenesulfonic acid to obtain a ketal; 2) enabling the ketal to perform epoxidation reaction under the action of a peroxyacetic acid solution of anhydrous sodium acetate to obtain an epoxide; 3) enabling the epoxide and methylmagnesium bromide to perform Grignard reaction, and then performing hydrolysis reaction by dilute sulphuric acid to obtain a Grignard matter; 4) performing hydrolysis on the Grignard matter by glacial acetic acid to perform deprotection so as to obtain 5 alpha, 17 alpha-dihydroxy-6 beta-methyl progesterone; 5) performing hydrogenation translocation reaction under the action of hydrogen chloride to obtain 6 alpha-methyl-17 alpha-hydroxyprogesterone; and 6) enabling the 6 alpha-methyl-17 alpha-hydroxyprogesterone to perform acetylation reaction with acetic acid and acetic anhydride so as to obtain the medroxyprogesterone acetate. During the reaction process of the method disclosed by the invention, the use of a precious metal catalyst, namely palladium on carbon is avoided, the cost of auxiliary materials and the recovery cost are greatly reduced, the reaction conditions in each step are mild, the violent heat release and deflation phenomena are avoided, and the safety in production is good.

The invention discloses a preparation method of a modified starch biodegradable film and belongs to the technical field of environmental science. The preparation method includes: using sweet potato starch as a raw material, crosslinking with epoxy polypropylene as a crosslinking agent to obtain crosslinked starch, esterifying the crosslinked starch with acetic anhydride to obtain crosslinked esterified starch, adding deionized water, an enhancer polyvinyl alcohol, a water repellent urea, a crosslinking agent glyoxal and a plasticizer glycerol into the crosslinked esterified starch, and subjecting the crosslinked esterified starch to swelling, pasting and crosslinking reaction to obtain a substance of certain viscosity, spreading the substance to polyester flakes, drying, and taking down a film to obtain the modified starch biodegradable film. The film prepared herein has good biodegradability, is free of environmental pollution, good in water resistance and high in stability, and is good in water tolerance and high in mechanical strength.

The present invention relates to preparation process of biodegradable cellulose acetate film. Ramie cellulose is swelled first with water and then with glacial acetic acid, and reacted with acetic anhydride under catalysis of sulfuric acid to obtain yellow cellulose acetate gel. The obtained cellulose acetate gel is dissolved in acetone, and the solution is filtered and added with different kinds of plasticizer to compound film casting liquid. The film casting liquid is cast in mold to form cellulose acetate film of certain thickness, and after volatilizing the solvent, the cellulose acetate film is separated from the mold in a water bath. The biodegradable cellulose acetate film may be used in preserving soil moisture and may be biodegraded without destroying soil structure and polluting environment.