552 results about "Water methanol" patented technology

The invention relates to a process for the production of acetic acid by carbonylation of methanol, and reactive derivatives thereof, in a reaction mixture using a rhodium-based catalyst in low water conditions. The process is used to achieve reaction rates of at least 15 g mol/l/hr. The high rate reactions proceed at water concentrations of less than 2.0 wt. %. Under certain conditions, the water concentration in the reaction mixture of the process is maintained at a desired concentration by at least one process step including adding a compound such as methyl acetate, dimethyl ether, acetic anhydride, or mixtures of these compounds to the reaction system. The process step of adding the components to the reaction mixture may be combined with other process steps for controlling water concentrations in reaction mixtures for the carbonylation of methanol.

The invention provides a preparation method of triazine structure containing benzoxazine intermediate, which sequentially includes: (1) performing synthetic reaction of aldehyde compound and amine compound at a molar ratio of at least 1:1 which includes adding aldehyde compound and solvent of at least one of clean water, methanol, ethanol, isopropanol, and ethyl acetate into a reactor at the room temperature under the normal pressure to obtain mixed solution with aldehyde mass concentration of no greater than 95%, adding amine compound while stirring, and reacting at 0-100 DEG C under the normal pressure for at least 15 minutes to obtain the reactant liquor; (2) pouring into the cleaning solution, stirring and cleaning, and filtering to collect solid substance, or directly filtering the reactant liquor to collect the solid substance; and (3) drying the solid substance obtained in step (2) at 30-100 DEG C.

A process for the preparation of an organosilicon condensate which comprises reacting together a silicon containing compound having at least one silanol group and a silicon containing compound having at least one —OR group or at least one silanol group (or a compound having both groups) in the presence of strontium oxide, barium oxide, strontium hydroxide or barium hydroxide and optionally a solvent such as water, methanol, ethanol, 1-propanol, 2-propanol, 1-butanol and 2-butanol, acetone or toluene.

The invention discloses a reproducible supported desulfurizer and a preparation method. Following procedures are included: 1) a solution is obtained by adding ionic liquid, polymerizable ionic liquid and initiator, or polymerizable ionic liquid, initiator, and crosslinked monomer into water, methanol, or ethanol solvent; a dosage of the initiator is 0.05-2wt% of that of the polymerizable ionic liquid; a dosage of the crosslinked monomer is 0.5-3wt% of that of the polymerizable ionic liquid; 2) polyporous solid load material is immersed into the solution obtained in procedure 1), and is stirred, with the mass ratio of the ionic liquid to the polyporous solid load material is 0.2:1-2:1, and then the material is volatilized at the room temperature for 0.5 to 1 hour, processed at the temperature of 40 to 60 DEG C for 0.5 to 4 hours, then processed at the temperature of 60 to 100 DEG C for 6 to 12 hours. The desulfurizer has the advantages that the absorbing speed is high; the selectivity is good; the absorbing capacity is high; the regeneration is easy, and can be repeatedly used in circulation; the mechanical intensity is high, and the mechanical intensity and absorption property can not be influenced after certain amount of water vapor is absorbed; the tolerance temperature for desorption is high; the preparation technique is simple; scale production is suitable.

A clarifying agent composition comprises a diacetal powder and an organosilane treated fume silica having a pH value of 5.5 to 8, measured in a 4% w/w dispersion in 1:1 mixture of water-methanol. The diacetal has the general structure formula (I), (II), (III), (IV) or (V),

This invention also intents to provide a new manufacturing method for preparing superfine powdery diacetal composition with high dispersion characteristic the use of said compositions for preparing polyolefin plastic article without the visible white spots on the surface of the corresponding article.

The invention relates to a method for preparing a drug carrier based on a magnetic carbon quantum dot/chitosan composite microsphere. The method specifically comprises the following steps of: (1) carrying out a coprecipitation reaction on bivalent and trivalent iron salts in an alkaline aqueous solution so as to prepare nano magnetic ferroferric oxide; (2) carrying out microwave radiation reaction on a glucose and polyethylene glycol mixed solution to prepare carbon quantum dots, and forming magnetic carbon quantum dot composite particles through electrostatic adsorption; (3) reacting the chitosan which is dissolved in a mixed solution of sodium methoxide/absolute methanol with nitric oxide in a high-pressure kettle, and forming a chitosan-nitric oxide addition product; and (4) dropwise adding the magnetic carbon quantum dots into the addition product, and forming the magnetic carbon quantum dot/chitosan composite microsphere through electrostatic adsorption. Compared with the prior art, the method is simple, rapid, low in cost, and the prepared product can be developed into the drug carrier which integrates magnetic targeting, fluorescence imaging or tracing, nitric oxide in-situ release and fluorescence detection.

The invention discloses a Pd nano-particle loaded ferronickel double hydroxide nanosheet array structure material, a preparation method and application thereof. The preparation method comprises the following steps: adding nickel salt, ferric salt, urea and quaternary ammonium salt into absolute methanol, ultrasonically dissolving the components, adding a palladium source solution, uniformly mixingthe components, transferring the mixed solution into a reaction kettle, obliquely placing foamed nickel into the mixed solution, carrying out solvothermal reaction, naturally cooling the reaction product to room temperature, and washing and drying the reaction product to obtain the Pd nanoparticle loaded NiFe LDH nanosheet array structure material. The material has the advantages of high activity, good durability, simple preparation process and low cost in alkaline electrolyte, shows excellent activity and stability for oxygen evolution reaction, hydrogen evolution reaction and total hydrolysis reaction, and has very high value in practical application of electro-catalytic water decomposition materials.

The invention provides a method for preparing a Salen-metal complex. The method comprises the following steps of: under the argon atmosphere, adding ligands(II), sodium methoxide, absolute methanol soluble ligands(II) and sodium methoxide into a reactor in sequence; stirring the mixture for 2 minutes, and adding 1mol/L cobalt acetate anhydrous/ methanol solution dropwise, wherein the molar ratio of the ligands(II) to sodium methoxide to cobalt acetate is 1:1:1; and making the mixture reacted at the room temperature for 24 hours, adding anionic salt which has the same molar weight as the cobalt acetate, stirring the mixture for three days in the air, stopping the reaction, concentrating the mixture, performing dissolution and filtration by adding methylene chloride, drying the filtrate by anhydrous sodium sulfate overnight, filtering the mixture, concentrating under reduced pressure, and drying the mixture under the vacuum condition to obtain the Salen-metal complex. The Salen-metal complex prepared by the method has the advantages of simple method, low cost and high catalytic efficiency.

The invention relates to a preparation method of a porous scaffold material and discloses a preparation method of a nano-fibrous silk fibroin-based porous scaffold. The preparation method comprises the following steps: blending a silk fibroin solution and a collagen solution under the temperature of 0-20 DEG C, standing to ensure the complete reaction of collagen and silk fibroin and generate nano-fiber; freezing the mixed solution to obtain a freezing body; performing freeze drying treatment on the freezing body to obtain a nano-fibrous porous scaffold material; and placing the nano-fibrous porous scaffold material in a vacuum drier with water and methanol, or an ethanol aqueous solution at the bottom, vacuumizing, and then standing to obtain the water-insoluble nano-fibrous porous scaffold. The obtained porous scaffold has 10-1000 microns of communicated pores. The pore walls consist of 10-100nm of nano-fibers; and the porous scaffold has similar nanoscale structures and micronscalestructures to extracellular matrix, is suitable for the adhesion and growth of cells and has good biocompatibility.

The invention belongs to a catalyst preparation technology field of reforming methane with carbon dioxide to produce synthesis gas, and particularly discloses a preparation method and application of MgO (111) load nickel-base catalyst. The catalyst is synthesized by a step of carrier synthesis and a step of Ni/MgO (111) preparation. The carrier is prepared by dissolving magnesium ribbon into a absolute methanol, adding anisyl alcohol and stirring, adding a water methanol solution dropwise under stirring, putting the hydrolyzed mixture into a high pressure reactor, leading argon into the reactor to replace the atmosphere, and then pressurizing to 1.0 MPa, reacting at the temperature of 265 DEG C, cooling and putting the obtained product into a tubular furnace, and calcinating the product; and the Ni/MgO (111) is prepared by immersing the carrier in an acetylacetone nickel solution uniformly, and calcinating for 5 h at the temperature of 650 DEG C after drying. The results of using the catalyst for catalyzing the reforming reaction of methane and carbon dioxide show that the catalyst has good activity and stability and enables the conversion rate of both CH4 and CO2 to be over 85%, and that the catalyst activity can stably maintain for 200 h without obvious inactivation.

The invention discloses a method for extracting rebaudioside D from stevioside crystalline mother liquor sugar, and belongs to the fields of bioengineering and novel sweetening agents. The method mainly comprises the following steps: dissolving primary crystal transformation mother liquid sugar after RA extraction into a mixed organic solvent of water and methanol with the ratio of 1:(7-10); keeping the stirring speed at 20-100rpm/min at 50-70 DEG C for 1-10 hours to crystallize; removing impurities in the mother liquor after washing a solid substance by solid-liquid separation; baking to obtain a high-purity rebaudioside D (RD) product. The ratio of the RD in the raw material sample can be improved to over 50% from 20-30% by primary crystallization, and the RD product with high purity can be obtained by repeating for a plurality of times on the basis, so that a foundation is established for production of the high-purity RD product. The method is simple in technology, low in energy consumption, and easy to produce, and is used for stirring and controlling temperature in production. The mother liquor can be recycled after being concentrated, and the solvent can be recycled after being distilled. Thus, good economic benefits and low environmental pollution are achieved.

The invention discloses a preparation method of 1-N-ethyl gentamicin C1a sulfate. The method comprises the following steps of: carrying out a complexation reaction on gentamicin C1a and zinc acetate in a methanol solvent; then, dropping a mixed solution of acetic anhydride, triethylamine and tetrahydrofuran to carry out an acylation reaction and obtaining 3,2',6'-3-N-acetyl-gentamicin C1a by post-treatment; then, carrying out a silylation reaction with hexamethyl disilazane in a chloroform solvent; carrying out an N-alkylation reaction with acetaldehyde in a carrene solvent; then, carrying out a reduction reaction with potassium borohydride; hydrolyzing with an NaOH solution; obtaining 1-N-ethyl gentamicin C1a by post-treatment; adding the 1-N-ethyl gentamicin C1a to anhydrous ethanol or anhydrous methanol for stirring or dissolving; then, dropping concentrated sulfuric acid; and obtaining 1-N-ethyl gentamicin C1a sulfate by post-treatment. The method of the invention has higher yield.

The invention discloses a preparation method for a chitosan-based biomimetic membrane material with an asymmetric structure, and the preparation method comprises the following steps of dispersing chitosan into acetic acid aqueous solution, adding absolute methanol and acetic anhydride for reacting after the chitosan is completely dissolved, and then, centrifugally removing sediment; dropping in alkaline solidification liquid under stirring condition, and filtering to obtain chitosan microgel; adding the chitosan microgel in glycerin solution, injecting the solution in a mold, and standing and draining water, freeze-drying one part to obtain a chitosan-based porous sponge material, and drying the other part to obtain a chitosan-based dense membrane material; bonding the chitosan-based porous sponge material and the chitosan-based dense membrane material to obtain the chitosan-based biomimetic membrane material with asymmetric structure. The preparation method provided by the invention has the advantages that the preparation technology is simple, the prepared chitosan-based biomimetic membrane material has a porous sponge structure and a dense membrane material structure, the chitosan-based biomimetic membrane material is not curly when encountering water, guiding bone regeneration performance is good, and the chitosan-based biomimetic membrane material is degradable and controllable and can be widely used as a guided bone tissue regeneration membrane material in treatment of the fields such as dental implant, osteoarthritis, bone defect, and the like.

The invention discloses a preparation method of an eucommia extract product, comprising the following steps of: (1) extraction of a solvent, wherein the solvent is selected from water, methanol, ethanol, isopropanol, 1-butanol, glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,3-butylene glycol, acetone, ethyl acetate or their combination; (2) separation of an extract and residue so as to obtain the extract; (3) recovery of the optional solvent; and (4) optional dissolution or dilution. The eucommia extract product obtained by the method has antioxidation and UVA and UVB irradiation resistant effects, and can be used for ageing resistance of skin, especially light ageing resistance. The eucommia extract product can be used as a cosmetic additive or medicinal active component. The invention also discloses an application of the eucommia extract product in preparation of cosmetics or medicines for skin ageing resistance, especially for light ageing resistance.

The invention provides a tobacco active ingredient, an extraction method and an application thereof, and belongs to the technical field of tobacco product processing and extraction. Through pretreating tobacco raw materials, and sequentially carrying out normal temperature extraction on the pretreated tobacco raw materials, High temperature extraction, methanol extraction three times, and purifiedwater using high polar solvent, methanol as the extraction solvent, through the use of different extraction solvents and different extraction conditions, can ensure that the tobacco active ingredients in tobacco raw materials can be fully extracted, improve the extraction content of tobacco active ingredients. It is found that the target component has antibacterial and anti-tumor functions and isa low toxicity product. Therefore, it has the development potential of antibacterial and anticancer drugs, and provides a theoretical basis for new drug research and development.

A synthetic method for aliphatic alpha-calcium picrolonate comprises the following steps: 1. adding carbonyl group reactant in glycolylurea in the presence of catalytic accessory and water and heating, wherein the mol ration of the glycolylurea and the carbonyl group reactant is 1:1.2-1.4; the carbonyl group reactant is aldehyde compound or ketone compound; when aldehyde compound is adopted the catalytic accessory is potassium bicarbonate, and when ketone compound is adopted the catalytic accessory is ethanolamine; 2. cooling to the room temperature, regulating the pH valve to 7 and separating out the intermediate product; 3. filtering and washing the intermediate product; 4. stirring and refluxing the intermediate product and sodium hydroxide solution, wherein the mol ratio of the intermediate product and sodium hydroxide is 1:3-5; 5. regulating the pH value to 4-5, antiregulating the pH value to 7 with the sodium hydroxide solution, and evaporating to remove the moisture; 6. adding absolute methyl alcohol to extract for several times and filtering; 7. distilling to remove the methyl alcohol; and 8. adding de-ionized water and aqueous calcium chloride solution of equivalent amount and separating out alpha-calcium picrolonate. As massive subsidiary products are removed in the method, the calcium content in the prepared product can achieve the standard.

The invention provides a preparation method of a biodegradable plastic poly(butylene succinate). The traditional polyolefin plastic is undegradable, so that the serious problem of environmental pollution is caused; as a molecular main chain of a degradable plastic contains an easily hydrolyzable ester bond, the degradable plastic is decomposed and metabolized easily in nature and is finally decomposed into carbon dioxide and water. The specific technical scheme is described as follows: performing a ring-opening reaction on tetrahydrofuran and a promoter hydrogen iodide, adding a product into a succinic acid device with functions of heating for temperature control, stirring and nitrogen protection and performing an esterification reaction for 1-3h under the action of a catalyst at the temperature of 95-200 DEG C; finally, performing a polycondensation reaction under a vacuum condition for 2-3h, so as to obtain a poly(butylene succinate) crude product, wherein the absolute pressure is 20-80Pa, and the reaction temperature is 135-235 DEG C; dissolving the crude product with purification-used trichloromethane, precipitating with absolute methanol, filtering and drying, so as to obtain poly(butylene succinate).

The invention discloses an oxidized graphene-rhamnolipid composite material which is black gray powder and is of a laminar multi-hole nano structure. The invention further discloses a preparation method of the composite material. The preparation method includes the following steps that oxidized graphene is added into a dispersing agent, and oxidized graphene mixed liquor is formed after ultrasonic dispersion; rhamnolipid, 1-ethyl-(3-dimethyl amino propyl) carbodiimide hydrochloride and 4-dimethylamino pyridine are added into the mixed liquor, then the ultrasonic reaction is performed, and a certain amount of absolute methanol is added and mixed for generating sediments; the sediments are washed and centrifuged, and finally the oxidized graphene-rhamnolipid composite material is prepared through vacuum freeze drying. The invention further relates to application, in aspect of cationic dye absorption, of the composite material prepared through the method. The prepared composite material is low in biological toxicity and not prone to agglomeration, the preparation method is simple and easy to carry out, and in the process of the cationic dye absorption, the prepared composite material has the advantages of being free of secondary pollution and enabling solids and liquids to be separated easily.

The invention relates to a method for preparing gastrodine, which has simple operation, light pollution and little equipment input. The method has the following process steps: taking coarse gastrodine powder; adding 60 to 90 percent ethanol into the coarse powder for percolation; collecting percolate of which the volume is 5 to 10 times the weight of a medical material; filtering, and reclaiming the ethanol at reduced pressure; condensing the percolate to dryness; adding methanol into residue for dissolution; injecting the solution into a high-efficient countercurrent extractor; using a lower phase of a water-methanol-acetic ether (1:1:8) solvent system as a stationary phase and an upper phase as a mobile phase, and collecting and condensing a gastrodine section; precipitating and separating crystal; and adding methanol-acetic ether (1:5-10) into the crystal for recrystallization. The gastrodine prepared by the method has high purity and is easy to realize industrialized amplification.

A solidifying agent for the self-hardening furan resin contains toluene (0-5 wt.%) or (0-20 wt%), xylene (2-10) or (5-25), sulfuric acid (35-65) or (10-40), water (0-20) or (20-60), methanol (10-45) or (6-30), alcohol (0-9) or (0-6), and regulating agent (0.05-0.9) or (0.1-0.7) for fast-hardening or slow-hardening furan resin used for casting.

The invention provides a method for on-line concentration and automatic analysis of endogenous polypeptides, and a special device. The method comprises the following steps: by utilizing the unique characteristic that a restricted access medium retains small molecular polypeptides and expels macromolecular proteins, the endogenous polypeptides are subjected to on-line concentration; a water solution, in which the volume concentration of formic acid or acetic acid is 0-5%, is used for leading a sample to pass through a pre-column of the restricted access medium for concentration; a buffer solution with the salt concentration being 10mM-2000mM and the pH value being 1-4 is used for eluting the sample concentrated in the pre-column to a reversed-phase column head; and the sample on the reversed-phase column head is subjected to separation and mass spectrometric detection with water/acetonitrile or water/methanol with the volume concentration ranging from 0% to 100%. By adopting the pre-column of the restricted access medium of a capillary and the stepwise gradient for elution, the invention achieves the effect of greatly simplifying the experimental facilities. The device can engage in on-line coupling with mass spectrum, and has the characteristics of simple operation, small sample consumption, the ability of carrying out multidimensional separation and the like.

The invention discloses a method for preparing furfurylideneacetone and di-furfurylideneacetone from furfural by catalyzing with a solid alkali catalyst and a separating process. In the process, furfurylideneacetone and di-furfurylideneacetone are prepared by undergoing an aldol condensation reaction on furfural and acetone serving as raw materials and taking 'water-alcohol' or 'water-methanol' as a solvent under the catalyzing action of solid alkali. Di-furfurylideneacetone can be directly separated by refrigerating a reaction liquid at low temperature and crystalizing; and furfurylideneacetone can be further separated out by rotationally evaporating a residual liquid in vacuum and crystalizing. The purities of the two products are over 98percent, and the total yield is up to 55.4 percent. The method has the advantages of mild reaction conditions, simple separation and extraction processes, high overall yield, capability of realizing comprehensive utilization of two kinds of products, environmentally-friendly production process and high economic benefit and environmental benefit.

The invention discloses a preparation method of a high-corrosion-resistance modified epoxy resin composite coating, which comprises the following steps: dissolving a metal salt and an imidazole ligandin absolute methanol, conducting stirring for 2-3 hours to obtain a white emulsion, carrying out centrifugal separation to obtain a white solid, alternately conducting washing with methanol and deionized water for 3-5 times, and carrying out vacuum drying at 60-80 DEG C to obtain a white powdery MOF nanometer material; mixing epoxy resin, the MOF nano material and a diluent, carrying out ball milling and stirring for 0.5-5 h, adding a curing agent, and conducting uniform mixing to obtain modified epoxy resin; coating the surface of a pretreated metal matrix with the modified epoxy resin, andconducting drying and curing to obtain the MOF modified epoxy resin composite coating on the surface of the metal matrix. According to the method, the epoxy resin is modified by the MOF nano material,so that the MOF nano material and the epoxy resin are chemically bonded, the problem of interfacial compatibility between the filler and the epoxy resin is solved, and the corrosion resistance and mechanical properties of the epoxy resin coating are improved.

The invention discloses a non-precious metal inactivated hydrogenation refining catalyst recovery method which consists of, processing the devitalized catalyst by carbon burning and with absolute methanol or ethanol or lightweight petroleum solvent, wherein the volume ratio of absolute ethyl alcohol and devitalized catalyst is 1-2 : 1, flushing, and reclaiming the absolute ethyl alcohol through filtration.

The present invention relates to a method of treating CD33+ acute and chronic myeloid leukemia in animals including humans, using fraction nos. 1 and 9 obtained from water:methanol fraction by column chromatography, with ratio of water and methanol ranging between 1:5 to 5:1, wherein said water:methanol fraction is obtained from the polar extract of piper betel by HPLC, with retention time of 3.6 and 24.0 minutes respectively, with said fractions used both individually, and in combination, and a composition comprising the said fraction nos. 1 and 9.

The invention relates to separation of natural medicines, in particular to a preparation method for separating an epigoitrin. After being ground, radix isatidis plants are decocted in 8 to 12 volumes of water to obtain the extract; then the extract group is obtained by concentration; ethanol is added to precipitate twice; the supernatant fluid above the alcohol precipitation is concentrated; the ethanol is recycled; the concentrated solution is filtered by a high speed centrifuge; the filtrate is separated by a membrane separator; the transmission fluid is chromatograph zed, separated and prepared through a macroporous resin column; the water ethanol is gradient eluted to obtain components and then to be separated and prepared by a highly efficient industrial chromatography column; the water methanol is gradient eluted to collect the eluent; and the epigoitrin is obtained by concentrating, freezing and drying the eluent. The products of the invention which is high in purity, large in preparation amount and reliable and stable in technique is especially suitable for separating and preparing a large amount of the epigoitrin compounds with the high purity from Chinese radix isatidis.