309results about How to "Save solvent" patented technology

The invention relates to a novel indoleamine-2,3-dioxygenase (IDO) inhibitor, as well as a preparation method and an application thereof. The inhibitor is compounds of a formula I or pharmaceutically-acceptable salt, solvate, polymorph, enantiomer or racemic mixture thereof, wherein R1 or R2 is independently selected from H, C1-C5 alkyl, halogen and a substituent of a formula II and either of R1 and R2 is the substituent of the formula II; R3 is an aryl group; and n is equal to 0, 1, 2 or 3. Compared with the know IDO inhibitors, the novel IDO inhibitor has significant inhibitory effect on IDO and can be used for treatment of diseases having IDO-mediated tryptophan metabolic pathway pathological features, such as tumors, cancers, Alzheimer's disease, autoimmune diseases, cataract, psychological disorders, depression and/or anxiety. The preparation method of the novel IDO inhibitor has the advantages of being convenient in operation, having mild reaction conditions and reducing solvent consumption and pollution, thereby facilitating industrial production.

The invention relates to a preparation method of a para-aramid nanometer fiber composite lithium ion battery separator, and belongs to the technical field of a high polymer material. The preparation method comprises the steps of preparing para-aramid polymer paste, coating the para-aramid polymer paste on a surface of a base membrane by a coating method, and solidifying the coating film in coagulation bath comprising N-methly-2-pyrrolidone and water to obtain the para-aramid nanometer fiber composite lithium ion battery separator; and washing and drying the para-aramid nanometer fiber composite lithium ion battery separator to obtain a finished product of the para-aramid nanometer fiber composite lithium ion battery separator. Compared with the prior art, the preparation method has the advantages that a solvent and an energy source are saved, energy consumption is also reduced, and unfavorable influence of impurity on battery performance is prevented; and moreover, the preparation process is simple, and the high-temperature resistant performance of the separator is improved, the prepared separator has favorable ion conductivity and can obtain relatively good performance when used as the lithium ion battery separator.

The invention relates to a Chinese magnoliavine fruit monomer composition separation preparation method; ethanol extracts from Chinese magnoliavine fruit are extracted by petroleum ether, chromatography is carried out to the petroleum ether extracts by a silicagel column, and then the petroleum ether is eluted by petroleum ether-ethylacetate, and HPLC is used for monitoring, and then crude extract A and crude extract B are fraction-collected, and eluted; the volume ratio of eluant petroleum ether and ethylacetate is 3-5:1, the crude extract A and crude extract B are respectively applied to a high-speed counter-current chromatography for separation, so as to obtain SCHisanhenol, deoxyschizandrin, schizandrin B, schisandrin C, schizandrol A, schizandrol B and schisantherrin B monomers, and the purity is higher than 98 percent.

The invention provides a preparation method of andrographolide. The preparation method includes steps of extracting ethanol of common andrographis herb crude medicine, filtering, decolorizing by the aid of activated carbon, filtering again, concentrating cooling of a concentrated liquor, removing supernatant fluid, collecting deposit, washing the deposit by ethanol to obtain macro-crystal, dissolving the macro-crystal by ethanol, decolorizing the macro-crystal by the aid of activated carbon, filtering the macro-crystal, concentrating filtrate, recrystallizing and drying so that andrographolide is obtained. The transfer rate of andrographolide of the method is high, remained organic solvent is less, and a product is safer and effective.

The invention relates to a process for producing polyphenyl thioether, comprising the following steps of:, mixing hydrogenous sodium sulfide, lithium chloride and N-methyl pyrrolidone in the weight ratio of (20-25): (2-6): (70-80), co-boiling the mixture and inert gases at 150-210 DEG C for distilling and dehydrating; separating solvent by refining; respectively adding santochlor, solvent and lithium chloride in anhydrous sodium sulfide, separating after complete reaction to obtain polyphenylene sulfide; compositely washing the polyphenylene sulfide to obtain pure polyphenylene sulfide; and reclaiming the lithium chloride by filtering, reclaiming the solvent and flashly evaporating dimethylbenzene solution in a two-period mode and cooling and crystallizing. The invention has the advantages of low cost, simple process, excellent performance of synthetic resin and high solvent recovering rate.

The invention discloses a crystal form G of ibrutinib. The crystal form G is characterized in that X-ray powder diffraction (X-RPD) which adopts Cu-Kalpha radiation and is represented with a 2theta angle has diffraction peaks in positions at angles of 5.0 degrees plus or minus 0.2 degrees, 7.3 degrees plus or minus 0.2 degrees, 10.1 degrees plus or minus 0.2 degrees, 12.0 degrees plus or minus 0.2 degrees, 13.2 degrees plus or minus 0.2 degrees, 17.1 degrees plus or minus 0.2 degrees, 19.5 degrees plus or minus 0.2 degrees, 20.8 degrees plus or minus 0.2 degrees, 22.3 degrees plus or minus 0.2 degrees, 24.3 degrees plus or minus 0.2 degrees, 27.4 degrees plus or minus 0.2 degrees and 31.2 degrees plus or minus 0.2 degrees. Related solvents in a preparation process of the crystal form G are cheap, the conditions are mild, the operation is simple, good controllability and reproducibility are realized, further, the prepared crystal form has great stability, the HPLC (high performance liquid chromatography) purity is higher than 99%, and the phenomenon of crystal transformation can be avoided; besides, the solubility is high, the dissolubility is good, and the bioavailability is high.

The invention discloses a method for qualitatively detecting polychlorinated biphenyl in soil and/or sediment. The method comprises the following steps of: (1) extracting the soil and/or sediment to be detected by adopting an accelerated solvent extraction method, thereby acquiring an extracting solution; (2) purifying the extracting solution through a gel permeation chromatograph, thereby acquiring an extract; (3) eluting the extract through a solid phase extraction column, and collecting the eluent; and (4) analyzing the eluent by a gas chromatograph-mass spectrometer so as to acquire full scan data, and then performing deconvolution analysis on the acquired full scan data according to a retention time locking database in the gas chromatograph-mass spectrometer, thereby qualitatively detecting the polychlorinated biphenyl in the soil and/or water body sediment to be detected.

The invention provides a preparation method of peony general glycoside, which comprises the following steps: soaking radix paeoniae alba or red paeonia in 2-10 times (weight) of hydrophilic solvent, wherein the hydrophilic solvent is water or a water solution containing less than 30% of methanol, ethanol, propanol and isopropanol; after soaking, percolating at low temperature of 5-40 DEG C; and concentrating the percolate, filtering to obtain the extracting solution, and passing the extracting solution through macroporous resin. The transfer rate of penoniflorin and peony Albiflorin is 85-90%, and the purity of the peony general glycoside extract is high.

The invention relates to a synthesizing method for a cephalosporin compound. The method comprises the following steps of: making 7-aminocephalosporanic acid serving as a raw material react with methyl mercapto tetrazole in a solvent under the catalyzing action of boron trifluoride to synthesize a 7-amino-3-[(1-methyl-1H-tetrazole-5-radical)]-3-cephem-4-carboxylic acid intermediate, and adding an acid binding agent into a reactant solution for neutralizing to acid state; and directly preparing the obtained intermediate solution into cefoperazone acid, cefpiramide acid and cefamandole sodium without the purifying or drying the intermediate. The method has the advantages of simple process, small environmental pollution, high product yield, low cost and suitability for industrial production.

The invention discloses an extraction process for lychee seed saponin. The process comprises the following steps: 1) lychee seeds are pulverized, a certain amount of lychee seed powder is weighted and is soaked with water, and combinative enzyme reagent, which accounts for 1 to 2 percent of the weight of the lychee seed powder, is added in for enzymolysis treatment; 2) ethanol solution is added in for ultrasonic extraction, so as to obtain ultrasonic extracting solution; 3) filtering treatment and vacuum concentration treatment are conducted to the ultrasonic extracting solution, so as to obtain lychee seed saponin coarse extractive; and 4) macroporous adsorption resin is adopted to sublimate the lychee seed saponin coarse extractive, so as to obtain the lychee seed saponin. In the process, cell walls are softened and degraded through enzymes; with the combination of ultrasonic cavitation, the cell walls are fully destroyed, and the dissolution of active ingredients is accelerated and increased; and through the nonpolar macroporous adsorption resin, saponin ingredients of the lychee seeds are concentrated and separated, so as to prepare the high-content lychee seed saponin. The process has the advantages of time and labor conservation, lower cost and the like.

The invention relates to a technique combination for extracting polysaccharide in glossy ganoderma mycelium cell. According to the mass ratio, the solid-liquid ratio is 1:10-1:60, the adding quantity of complex enzyme is 0.5-5.0% of the mass of raw materials, the range of ultrasonic wave power is within 100-500W, the range of enzymolysis time is 40-100min, the range of enzymolysis temperature is 30-60 DEG C, and the pH value range of enzymolysis is 4.0-8.0. The technique for extracting polysaccharide in glossy ganoderma mycelium cell and the method thereof comprise: high quality mycelium is selected for submerged fermentation to obtain mycelium dry powder; the solid-liquid ratio is determined; the adding quantity of the complex enzyme is determined; and the optimum extraction technique combination for extracting the mycelium dry powder polysaccharide by using an ultrasonic wave-composite enzymolysis method is determined.

The invention discloses a preparation method and an application of a ginkgo leaf extract, wherein the method comprises the following steps of: a) washing and then drying ginkgo leaves; b) crashing and sieving; c) soaking by ethanol; d) oscillating by a ultrasonic cell crasher; e) extracting and filtering; and f) condensing in vacuum and drying. The invention has the advantages of adopting an ultrasonic-assisted extraction method, utilizing the functions of strong vibration, extremely high acceleration, strong cultivation effect, even stirring and the like generated by ultrasonic waves, accelerating the entry of the medicament effective constituents into the solvent, simultaneously avoiding the effect of high temperature on extraction constituents and greatly improving the yield of the extract. In the extract, flavonoids accounts for 36 percent, ginkgo terpene lactones account for over 8 percent while the injurant phenolic acid is less than 3PPM, therefore, the product has high safety. The obtained Ginkgo leaf extract of 4 to 6g is added to each kilogram of feeding stuff, therefore, the animal immune anti-inflammatory action and the production property can be raised by more than 10 percent and 2 to 3 percent respectively.

The invention discloses an extraction method of monosialotetrahexosylganglioside. The extraction method mainly comprises the following steps: separating G1S in the total extract of a brain tissue total extract by adopting a macroporous resin for separating a hydrophilic and lipophilic natural product through an adsorptive process, wherein the hydrophilic and lipophilic natural product is sugar and the like; and separating out high-quality monosialotetrahexosylganglioside (GM1) dry power by common silicagel column chromatography. As different metal ionic impurities still exist in the product subject to the silicagel column chromatography, a cation exchange column is used for further ionic exchange. After improving the traditional method, a large amount of solvent and time are saved, the yield is improved, and the cost is lowered to a great extent.

The invention relates to a method for preparing lactuca indica and lactucin, which is a method for using two separation processes to obtain lactuca indica and lactucin from cichorium glandulosum by a high-speed countercurrent chromatography. The method has the advantages of large fractional dose, small sample loss, high recovery rate, mild separation environment and solvent saving. A great amountof lactuca indica and lactucin crude products can be placed in a countercurrent chromatograph, the separation result achieves the high purity and good separation effect. The method is not only suitable for preparing the product with high purity from plant crude extract, but also suitable for purifying lactuca indica and lactucin crude extracts obtained by various approaches.

A process for extracting huperzine A from clubmoss herb, cryptomeria, or masson fir includes such steps as breaking, immersing in acid solution, concentrating, decoloring by activated carbon, regulating pH value, extracting by chloroform, vacuum recovering, volatilizing, eluting out, vacuum recovering, crystallizing and drying.

The invention relates to an online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system. Two one-dimension low-pressure, middle-pressure and high-pressure preparation liquid chromatographic systems are organically combined through a six-way valve and software. Pressure used by a second dimension system is not lower than pressure used by a first dimension separation system. When the first dimension system and the second dimension system are low-pressure or middle-pressure preparation liquid chromatographic systems, through switching the six-way valve, target compound directly enters a second dimension chromatographic column for second dimension separation after first dimension separation; and when pressure used by a second dimension separation system is higher than pressure used by the first dimension separation system, a trapping column is connected on the six-way valve, the target compound is adsorbed on the head of the trapping column after the first dimension separation, and then the target compound enters the second dimension chromatographic column for second dimension separation. The invention has the advantages that the contradiction between sample injection volume and separation capacity is solved, the large sample injection volume is ensured and the separation capacity of the preparation chromatographic system is greatly improved; the system structure is simple and the establishment is easy; the operation is simple and convenient and the automation can be easily realized; and the application scope is wide.

The invention relates to a method for pre-treatment of wine, the wine is a sample which is waiting for being detected for content of pesticide residues, and the method comprises three steps of extraction, purification and concentration. The invention also relates to a pesticide residues detection method for the wine, and the pre-treatment method performs pre-treatment on the wine sample. The pre-treatment method can realize rapid pre-treatment on the wine sample for detecting the pesticide residues, and has the advantages of less step, short time consumption, no requirement of massive organic solvent, environmental protection and low cost.

The invention discloses an organic silicone modified phenolic resin encapsulating material and a preparation method and usage thereof. The encapsulating material comprises the following components in parts by weight: 15-19 parts of modified phenolic resin, 3-5 parts of titanium white, 1-2 parts of organic silicon, 50-64 parts of silicon micro powder, 5 parts of pigment, 3 parts of thixotropic agent, 5 parts of drying agent and 4-7 parts of curing agent. The preparation method of the encapsulating material comprises the following steps: spraying, extrusion, crushing and ball milling. The encapsulating material has the advantages of high pressure resistance, temperature difference resistance, good insulating property, good moisture proof performance, high mechanical strength, quick natural drying, stable electric property, good adhesion, no cracking before and after curing, no color variation and the like, the production efficiency is increased by 20%, the output rate is improved by 10%, the manufacturing cost is reduced, the encapsulated product has a bright and attractive surface, is green and environment-friendly, and can replace an imported encapsulating material. The organic silicone modified phenolic resin encapsulating material is mainly used for the dipping encapsulation of porcelain medium capacitors, ceramic filters, thermistors and other electronic components.

The invention belongs to the technical field of chemical drug synthesis, and particularly relates to a preparation method of an isoxazoline insectifuge. The preparation method is characterized in thatthe isoxazoline insectifuge is fluralaner; an intermediate I is sequentially subjected to an amidation condensation reaction, a substitution reaction and a ring closing reaction in the same reactioncontainer; and after the reactions are finished, a reaction product is poured into water, stirring and filtering are conducted to obtain a solid, and the obtained solid is recrystallized to obtain theisoxazoline insectifuge. The method has the beneficial effects that the method uses a solvent and one-pot method to synthesize fluralaner, technological operation of a synthesis process is reduced, treatment time and reaction time are shortened, product yield is improved, and the method is suitable for large-scale production.

The invention discloses a method for preparing Chinese medicinal granules for treating a cold, which belongs to the field of medicine and overcomes the defects of low extraction rate of the conventional preparation method and high effective ingredient loss of medicaments. The preparation method comprises the following steps of: crushing schizonepeta spike, mint and perilla leaf into coarse powderaccording to a formula of cold heat clearing granules (No.1-644, version 2005), and extracting the medicaments with volatile oil by adopting supercritical CO2 and ultrahigh pressure; crushing bupleurum, parsnip, kudzuvine root, platycodon root, bitter almond kernel, angelica dahurica, bunge's corydalis and reed rhizome into coarse powder, mixing the coarse powder and the rest medicament residue of the extracted medicaments, performing ultrahigh pressure extraction by adding water, filtering the extract, and concentrating the extract with reduced pressure to form clear paste; and adding auxiliary materials into the clear paste to prepare granules, and adding volatile oil into the granules to obtain the Chinese medicinal granules. The method has the advantages of preventing oxidation, dissipation and reaction of thermo-sensitive components, completely keeping the bioactivity of biomass and reducing loss of effective ingredients along with quicker medicament response and stronger function.

The invention discloses a needle-type solid-phase extraction filter. The needle-type solid-phase extraction filter comprises a shell, and the upper side and the lower side of the shell are provided with an injector nipple connector and a pintle connector which are communicated with an inner cavity of the shell respectively; an upper sieve plate, solid-phase extraction filler, a lower sieve plate and a filter membrane are sequentially arranged in the inner cavity of the shell from top to bottom, the upper sieve plate and the lower sieve plate are each provided with sieve holes of which the hole diameters range from 95 micrometers to 105 micrometers, and the particle size of the solid-phase extraction filler ranges from 110 micrometers to 130 micrometers. According to the needle-type solid-phase extraction filter, solid-phase extraction and membrane filtration are combined in one device for the first time, the operation steps are greatly simplified, the solvent and the filler are saved, and the operation cost is reduced; the needle-type solid-phase extraction filter can be suitable for different samples and solvents and is wide in application range and good in effect.