63 results about "Butyric anhydride" patented technology

The invention discloses cellulose acetate butyrate mixed ester with high butyryl content, and a preparation method thereof. The cellulose ester is prepared from the following components in parts by weight: 600 parts of wood pulp, 800-1200 parts of butyric acid, 2500-3500 parts of butyric anhydride, 20-40 parts of acetic anhydride, and concentrated sulfuric acid catalyst accounting for 5-10% of total weight parts of wood pulp. The preparation method comprises the following steps: activating, performing esterification reaction, mixing, adding magnesium acetate solution, hydrolyzing, performing chromatography, and then sequentially conventionally filtering, washing and drying to obtain a finished product. According to cellulose acetate butyrate mixed ester with high butyryl content, cellulose acetate butyrate with the butyryl content of 48-53% and acetyl content of less than or equal to 4% can be obtained after the combination according to specific formula and proportion, and the product is stable in performances. The preparation method is simple in steps, the preparation period is short, the preparation conditions are not strict and easily achieved, and especially, the activated solid is fed into a cooling liquid within 2-5min, so that the quality of products can be guaranteed while the fast follow-up reaction is guaranteed.

The invention discloses a preparation method for a biomass-based carbon nanofiber. The method particularly includes the following steps: first, mixing lignin with butyric anhydride and 1-methylimidazole, stirring under a nitrogen atmosphere for reaction, washing with n-hexane, then placing in deionized water, stirring, performing extraction filtration, and drying to obtain esterification modifiedlignin; dissolving polyacrylonitrile and the esterification modified lignin in a N, N-dimethylformamide solution to obtain a spinning solution; performing electrostatic spinning on the spinning solution to prepare a carbon nanofiber precursor, performing pre-oxidation on the carbon nanofiber precursor in a muffle furnace, and then performing carbonization treatment to obtain the biomass-based carbon nanofiber.The biomass-based carbon nanofiber prepared by the method of the invention is used as an electrode material of a super-capacitor, is excellent in electrochemical performance, and can meetapplication requirements in the fields of electric automobiles, high-load industries, new energy power storage, and the like.

The invention provides a preparation method for cellulose acetate-butyrate. The preparation method comprises the following concrete steps: (1) stirring butyric acid, acetic acid and refined cotton linter in a mixer and carrying out activation at a temperature of 80 to 95 DEG C for 2 to 4 h; (2) adding butyric anhydride into the activated refined cotton linter and carrying out esterification at a temperature of 80 to 95 DEG C for 4 to 6 h under stirring, with sulfuric acid used as a catalyst; (3) after esterification, adding an aqueous solution of butyric acid into esterification liquid and carrying out hydrolysis at a temperature of 80 to 95 DEG C for 4 to 6 h under stirring; and (4) after hydrolysis, maintaining stirring, adding sodium butyrate to neutralize sulfuric acid, adding the aqueous solution of butyric acid for dilution, dumping an obtained diluted solution into water under stirring for precipitation and rinsing and drying an obtained product. The method provided by the invention has the advantages of a simple process, conservation of raw materials, optimized steps and low cost.

The invention relates to a method for preparing a cellulose acetate butyrate microsphere adsorption material by an ionic liquid as a solvent. The method comprises that cellulose is dissolved in an ionic liquid, the cellulose solution reacts respectively with butyric anhydride and acetic anhydride to produce cellulose acetate butyrate products having different substitution degrees, the cellulose acetate butyrate solution is condensed to form liquid drops by reversed phase suspension and programmed cooling, a curing agent is added into the cellulose acetate butyrate liquid drops to cure the liquid drops so that microspheres are formed, and the ionic liquid is removed by distilled water washing so that cellulose acetate butyrate microspheres are obtained. The method has simple processes, realizes recycle of the solvent, utilizes the cellulose raw material having a wide source and a low cost, and realizes high-value utilization of natural plant cellulose. The cellulose acetate butyrate microspheres prepared by the method have acetyl content of 3-20% and butyryl group content of 5-43%, have controllable acyl content and have regular spherical shapes. 95% of the cellulose acetate butyrate microspheres have grain diameters of 50-200 microns. The cellulose acetate butyrate microspheres have good mechanical properties, good thermostability and acid and alkali resistance and are good carriers and adsorption materials.

The invention relates to the technical field of drug synthesis, in particular to a method for preparing calcium dibutyryladenosine cyclophosphate. The preparation method comprises the following steps: taking adenosine cyclophosphate as a raw material, and preparing adenosine cyclophosphate triethylamine salt with triethylamine under an aprotic solvent; taking butyric anhydride as an acylating agent, and synthesizing the calcium dibutyryladenosine cyclophosphate in an organic aprotic solvent. Compared with the traditional process, the method has the advantages that the production period is shortened from the original 9-10 days to 3-4 days, the yield of crude products is increased to 78-82 percent, the purification yield is increased to 90-94 percent, and the total reaction yield is increased to 70-75 percent. The method disclosed by the invention adopts a continuous washing method and performs reversed phase extraction, and the liquid chromatogram purity of the obtained dibutyryladenosine cyclophosphate is 98-98.5 percent.

The present invention relates to a preparation method of a cellulose nanometer crystal with functionalized alkynyl on the surface. The preparation method comprises: 1) preparing 4-oxo-4-(prop-2-yn-1-oxy)butyric anhydride; 2) carrying out ultrasonic and uniform mixing reaction according to a mass ratio of the cellulose nanometer crystal to the 4-oxo-4-(prop-2-yn-1-oxy)butyric anhydride of 1:5-1:20, wherein the mass of a catalyst is 0.1-20% of the mass of the 4-oxo-4-(prop-2-yn-1-oxy)butyric anhydride, the reaction temperature of 60-100 DEG C, and the reaction time is 2-8 h; and 3) after completing the reaction, cooling to a room temperature to obtain a primary product, washing a plurality of times, and drying to obtain the cellulose nanometer crystal with the functionalized alkynyl on the surface, wherein the surface hydroxyl substitution degree is 4.5-13.8%. The preparation method of the present invention has advantages of low-cost, environmental-protection and completely-biodegradable raw materials, simpleness, rapidness, and high efficiency.

The invention discloses a butyrate starch preparing method and belongs to the technical fields of preparation and application of modified starch and deep processing of agricultural products. Accordingto the butyrate starch preparing method, starch serve as the principal raw material for esterification with butyric anhydride to achieve stabilization of butyric acid and small releasing of the butyric acid in gastric juice; resistant starch prepared through esterification of the butyric acid and the starch can well avoid being absorbed in small intestines, resist digestion by enzymes secreted bybrush borders, selectively release micromolecular effective load in large intestines; fermented by enteric microorganisms, the resistant starch can produce more short-chain fatty acids and probiotics, thereby improving the bioavailability of the butyric acid and expanding the application range of the starch. Compared with other butyric acid products, the butyrate starch is odorless and can be esterified into the resistant starch to convey the butyric acid to the rear end of the intestines; the butyrate starch can be fermented by the enteric microorganisms and decomposed by bacterial esteraseinto butyric acid and other short-chain fatty acids and increase the content of the probiotics, thereby belonging to probiotic products.

The invention discloses a calcium dibutyryladenosine cyclophosphate preparation method, which is characterized by comprising: (1) adding adenosine cyclophosphate and calcium hydroxide to water according to a molar ratio of 1:1-1.2, carrying out a reaction for 30-40 min, filtering to remove insoluble matters, adding ethanol having the volume 2-3 times the volume of the filtrate to the filtrate, filtering after a calcium adenosine cyclophosphate salt is precipitated, and carrying out vacuum drying at a temperature of 60-80 DEG C to obtain calcium adenosine cyclophosphate; (2) adding the calcium adenosine cyclophosphate obtained in the step (1) and butyric anhydride to a reaction kettle according to a ratio of 1 g:7-12 ml, protecting with nitrogen, and carrying out a stirring reaction for 1-3 h; and (3) adding 0-4 DEG C water having the volume 3-4 times the volume of the reaction liquid obtained in the step (2) to the reaction liquid, stirring for 30-40 min, carrying out nano-filtration on the reaction liquid, concentrating the trapping liquid, and carrying out freeze drying or spray drying to obtain the calcium dibutyryladenosine cyclophosphate. According to the present invention, the selectivity of the obtained calcium dibutyryladenosine cyclophosphate is more than 90%, the reaction time is short, the reaction process is simple and environmental friendly, and the method is suitable for industrial application.

The invention discloses a method of preparing cellulose acetate butyrate by means of a dichloromethane solvent method. The method comprises the following steps: (1) spraying acetic acid to wood pulp and performing activation at constant temperature; in addition, uniformly mixing acetic anhydride, butyric anhydride, butyric acid and a sulfuric acid catalyst; (2) inputting the material in an esterification kettle with a dichloromethane solvent for esterification reaction, after reaction, adding magnesium acetate into the reaction system, uniformly stirring the mixture, adding acetic acid into the mixture to dilute, and discharging the diluted solution into a hydrolysis kettle; (3) adding acetic acid into the hydrolysis kettle to promote hydrolysis, wherein the temperature of the system is 60-85 DEG C, and the time is controlled within 3-7h; and after hydrolysis, adding magnesium acetate into the system; and (4) performing filter pressing, performing flash evaporation on the filtrate, adding water for chromatography, and performing washing and drying. By this way, the cellulose acetate butyrate, the dynamic viscosity of which is 5000cps-7000cps, is obtained. The method is simple in operating step, high in controllability, good in atom economy, safe in operating environment and small in wastewater quantity.

The invention belongs to the field of organic photochemistry and medicinal chemistry, and particularly relates to a beta receptor blocker Acebutolol intermediate synthesized by photochemical Fries rearrangement. An efficient continuous acetylation synthesis method is adopted, raw materials including p-aminophenol and n-butyric anhydride are mixed and subjected to a water diversion reaction with a water-carrying agent, then the water-carrying agent is removed through distillation, reactants are cooled, water is added as a dispersing agent, then liquid caustic soda is added for a reaction, phenate is generated, acetic anhydride is dropwise added, the mixture is stirred for a reaction, ester is generated, recrystallizing is carried out to generate a first-step product N-(4-acetoxyphenyl) butyrylamide; and in the step 2 photochemical Fries liquid phase rearrangement reaction is adopted, the product in the first step is dissolved in an organic solvent, then Fries rearrangement is carried out by irradiation of ultraviolet-visible light with a specific wavelength, the solvent is heated and evaporated after the reaction is completed, and the important intermediate 2-acetyl-4-n-butyryl aminophenol of Acebutolol is obtained after recrystallization. The method is simple and easy to implement, and low-toxicity, efficient and cheap green chemical reagents are used in the synthesis process.

The invention discloses an apparatus for preparing butyric anhydride through reactive distillation of acetic anhydride and butyric acid, and a process thereof. The apparatus comprises a reactor, a reactive distillation tower, a butyric anhydride refining tower, a condenser, a condenser, a reboiler, a refluxing tank, a kettle tank, a pump and pipelines. The process using the combination of the reactive distillation tower, the rector and the butyric anhydride refining tower comprises the following steps: adding acetic anhydride and butyric acid to the reactor, reacting, and carrying out reaction and rectification on acetic anhydride and butyric acid flowing into the reactive distillation tower on each layer of trays of a reaction section; carrying out stripping section rectification on a material flowing down in the reaction section; carrying out rectifying section rectification on a material rising in the reactions section, and extracting from the tower top to obtain 80-100% acetic acid; pressurizing a material from the bottom of the reactive distillation tower to enter the butyric anhydride refining tower for rectification; and obtaining some of acetic acid, acetic anhydride, butyric acid, acetic butyric anhydride and butyric anhydride at the top of the butyric anhydride refining tower and butyric anhydride with the purity of 80-100% at the bottom of the refining tower. The apparatus and the process solve the problems of unstable quality, low yield and low production efficiency of products intermittently produced by using butyric anhydride.

The invention discloses a method for synthesizing 2-chlorobutyric acid, which comprises the following steps that: n-butyric acid and liquid chlorine are reacted in the presence of butyric anhydride serving as a catalyst at 50 to 150 DEG C for 5 to 15 hours, namely chloride ions substitute hydrogen ions at position-2 of the molecules of butyric anhydride to form 2-chlorobutyric anhydride and then the 2-chlorobutyric anhydride reacts with n-butyric acid to form butyric anhydride and 2-chlorobutyric acid; and after reaction, the 2-chlorobutyric acid with a purity of over 99 percent can be obtained by rectification. In the invention, butyric anhydride is used as a catalyst, and by controlling the reaction temperature and chlorine content, the conversion rate can be kept between 85 and 95 percent, the by-products generated can be reduced, and excessive chlorination can be prevented; and after being hydrolyzed, the catalyst can be recycled, and unreacted n-butyric acid can be reclaimed by rectification and can be reused in subsequent production. In the invention, the used amount of chlorine is small, fewer byproducts are produced, the utilization rate of n-butyric acid is high, and the environment-protection effect is improved considerably.

The invention discloses a preparation method of sodium salt of N-(all trans-retinol)-L-cystathionine methyl ester shown as formula I-Na. The preparation method comprises the following steps: step 1, in a dipolar aprotic solvent, performing acylation reaction on all-trans retinoic acid butyric anhydride shown in formula III and L-cystathionine methyl ester shown in formula II in the presence of organic base to obtain N-(all-trans-retinol)-L-cystathionine methyl ester shown in formula I; and step 2, prepare the n-(all trans-retinol)-l-cystathionine methyl ester shown in formula I obtained in thestep 1 into the sodium salt of n-(all trans-retinol)-l-cystathionine methyl ester shown in the formula I-Na. The preparation method disclosed by the invention has mild reaction conditions, simple operation, high yield and high purity of the obtained product. The production cost is low, the equipment requirement is low, and the method is suitable for industrial production.