81results about How to "Reduce the difficulty of separation and purification" patented technology

The invention discloses a high-purity silymarin and a preparation method thereof. The content of the high-purity silymarin is 97-101%. The preparation method of the high-purity silymarin comprises the following steps of: taking a silymarin shell as a raw material; adding ethyl acetate for dissolving the silymarin shell; extracting total flavones; collecting flavones in vacuum; and dissolving, extracting, filtering and drying the total flavones to obtain the high-purity silymarin. The invention has the advantages that on the basis of a silymarin seed, shell and kernel separating technology, the silymarin shell is used as the raw material for preparing the silymarin, the total flavones are extracted and then separated and purified by using ethanol with different concentration, and a recrystallization technology is adopted to prepare the high-purity silymarin. Because 99% of silymarin oil exists in the silymarin kernel, the silymarin shell is used for extracting the total flavones, the grease is little, a traditional method in which gasoline, petroleum ether and other organic solvents are used for degreasing is not required, and impurity interference, separation and purification difficulty and environment pollution are reduced. The preparation method disclosed by the invention is relatively simple, and the product quality and yield of the high-purity silymarin are greatly improved.

The invention discloses a method of extracting squalene from bottom sediment with natural vitamin E extracted. The bottom sediment with the natural vitamin E extracted is used as the raw material to prepare high-content squalene through a saponification, rectification and silica gel column chromatography combined process. The method specifically comprises the steps that firstly, the bottom sediment is subjected to a saponification reaction, unsaponifiable matter obtained through extraction is subjected to separation in a secondary rectifying tower, distillate obtained through secondary rectification is used as the raw material and subjected to silica gel column chromatography separation, three organic solvents with different polarities are used for elution, and fractional collection is conducted to obtain a plant hydrocarbon component, a squalene component, a natural vitamin E component and a sterol component, wherein the squalene content of the squalene component is more than 95%. According to the method, the bottom sediment with the natural vitamin E extracted is used as the raw material for extraction of the squalene, the process is simple and convenient, separation efficiency is high, industrial production is easy, the obtained squalene content is high, crude natural vitamin E and sterol can also be obtained, and comprehensive utilization of effective ingredients in the bottom sediment is achieved.

The invention provides a construction method and use of Streptomyces roseosporus gene engineering bacteria. The construction method comprises: cloning upstream and downstream accessory key genes dptE, dptF, dptG, dptH, dptI and dptJ of a nonribosomal peptide synthetases (NRPS) gene in a daptomycin gene cluster; and constructing recombinant plasmids by using an Escherichia coli-Streptomyces shuttle expression vector. The recombinant plasmids are transferred into Escherichia coli ET12567 to culture the ET12567 and the Streptomyces roseosporus together, the Streptomyces roseosporus is transformed by a combined transfer method, a transformant is screened by brulamycin resistance and polymerase chain reaction (PCR) is performed for further confirmation. The Streptomyces roseosporus gene engineering bacteria constructed by the invention can be directly used in the industrial production of daptomycin and can improve yield and reduce cost.

The invention discloses a method for preparing the key intermediate of limaprost, particularly provides a chiral compound of formula I and a preparation method thereof. The method comprises the following steps: (1) reacting a compound of formula 3 with a compound of formula 4 to obtain a compound of formula 5; (2) reacting a compound of formula 6 with the compound of formula 5 to obtain a compound of formula 7; (3) mixing the compound of formula 7 with a compound of formula 8 to obtain the compound of formula 1; (4) reacting the compound of formula 1 with a reducing agent to obtain a raw product, separating and purifying the raw product by column chromatography to obtain a compound of formula 2; (5) reacting the compound of formula 2 with a protector reduction agent to obtain a compound of formula 9, wherein each structural formula and substituent are defined as the specification. According to the invention, the method has mild reaction conditions, and the high-purity chiral compound can be conveniently and efficiently prepared.

The invention discloses a synthesis method of vitamin A palmitate. The method is characterized in that vitamin A palmitate is prepared by vitamin A acetate and palmitic acid through an enzyme method reaction. The method comprises the following steps: vitamin A acetate and palmitic acid are dissolved in an organic solvent to prepare a reaction material, the reaction material is pre-heated and is sent to a reaction column for consecutive reaction according to a certain flow; the reaction column is filled with immobilization lipase and ion exchange resin, the reaction material is proportional lipase and ion exchange resin; and after the reaction is completed, a reaction solution is post-treated to obtain the vitamin A palmitate. The vitamin A palmitate has the advantages of high yield and good quality. The appearance of the vitamin A palmitate is a light yellow grease substrate. By analyzing with United States Pharmacopeia USP28, the content is greater than 95%.

The invention discloses a phosgenation reactor and a method for preparing an isocyanate monomer by using the phosgenation reactor. The phosgenation reactor comprises an inner material inlet pipe, an outer material inlet pipe, a mechanical stirring rotation shaft, a rotation area and a kettle body, wherein the rotation area comprises a support structure, a rotation area filler block, an upper material outlet device and a lower material outlet device, the inner material inlet pipe and the outer material inlet pipe are coaxially arranged from inside to outside, the upper material outlet device and the lower material outlet device are arranged in parallel, are connected through the support structure, and are respectively communicated to the outer material inlet pipe and the inner material inlet pipe, the rotation area filler block is filled between the upper material outlet device and the lower material outlet device, the upper material outlet device is connected to the mechanical stirringrotation shaft, and the kettle body is provided with a gas phase material outlet, a liquid phase material outlet, a gas phase material inlet and a liquid phase material inlet. According to the present invention, by pre-treating the hydrochloride solution in the reactor, the salt forming concentration and the quality of the hydrochloride solution are improved while the rapid removal of hydrogen chloride gas during the phosgenation is achieved, such that the generation of chlorination by-products is effectively reduced, and the product separation difficulty is reduced.

The invention discloses a method for extracting taxane type active ingredients from Chinese yew efficiently. The method comprises the following steps of: firstly extracting with water, further extracting with alcohol, and further purifying by a traditional purification method to get paclitaxel, 10-deacetyl baccatin III, taxol-7-xyloside, cephalomanine and other non-water-soluble taxane type substance monomers. According to the method disclosed by the invention, macroporous resin is applied to the extraction process, the extraction yield of the active ingredients is far higher than that of a traditional extraction method, the using quantity of an organic solvent is further significantly reduced, and the method is suitable for large-scale production of the paclitaxel and comprehensive extraction of other taxane active ingredient substances.

The invention discloses a method for leaching valuable metal from cobalt-copper white alloy. The method includes the following steps that (1) the cobalt-copper white alloy is melted into an alloy melt, wherein the cobalt-copper white alloy contains silicon and almost contains no manganese; (2) a Mn-containing material is added into the alloy melt, and meanwhile gas is led in for blowing and slagging; (3) obtained slag is separated from the melt; (4) the melt with the slag separated out is atomized into alloy powder, wherein the mass friction of Mn in the alloy powder is 0.5%-20%; and (5) the alloy powder is subjected to acid leaching, and the valuable metal is recovered. Due to the fact that the Mn-containing material is added and reacts with the silicon in the cobalt-copper white alloy to generate the MnO-SiO2 slag, the silicon removal effect is achieved, and the method has the beneficial effects of being good in silicon removal effect and small in valuable metal loss. Besides, the melting temperature is much lower than the melting point of CaO-(MgO)-SiO2 binary system or ternary system slag in the prior art.

The invention relates to an effective part of ginseng stems and leaves, as well as a preparation method and an application thereof, belongs to the technical field of natural medicinal materials, and aims to provide an effective part of ginseng stems and leaves having simple composition for treating or preventing diabetes mellitus and related complications. The active ingredient of the effective part comprises ginsenoside Re and ginsenoside Rg1 in a mass ratio of 1:(0.667-5). The effective part of ginseng stems and leaves has the characteristics of exact active ingredient, simple composition, strong quality controllability, good product stability, small dosage, better pharmacological activity and the like. The preparation method comprises the step of separating and purifying ginsenoside Re and ginsenoside Rg1 as a whole, and the effective part of the ginseng stems and leaves has high ingredient stability, strong quality controllability, simple preparation process and high preparation efficiency, and is suitable for large-scale production.

The invention discloses an improved preparation method of zirconium tetrachloride and the zirconium tetrachloride. The preparation method comprises the following steps: 1), removing metal oxide impurities from zircon sand to obtain purified zircon sand; 2), heating the purified zircon sand together with a carbonaceous reducing agent and chlorine gas, reacting to produce zirconium tetrachloride, silicon tetrachloride, carbon monoxide and carbon dioxide and separating the zirconium tetrachloride. According to the preparation method, the metal oxide impurities in the zircon sand are removed firstand then the purified zircon sand reacts with the carbonaceous reducing agent and the chlorine gas, so that the content of chloride of the metal impurities in an obtained zirconium tetrachloride product is greatly reduced and the chloride of the metal impurities is avoided from entering the produced zirconium tetrachloride product, and thus the purity of the zirconium tetrachloride product is improved, the step of removing the chloride of the metal impurities is omitted, the separating and purifying difficulty of a back-end separation system is reduced, the purity and the quality of the zirconium tetrachloride product are improved, and the quality of a back-end product is improved.

The invention relates to a synthetic method of 2,5-dichlorophenol, and belongs to the technical field of dicamba key intermediate synthesis. 1,2,4-trichlorobenzene generated by pure benzene chlorination can be easily separated from 1,4-dichlorobenzene to avoid high production cost and low production efficiency caused by difficulty in separation. Since the 1,2,4-trichlorobenzene and the 1,4-dichlorobenzene can independently obtain the 2,5-dichlorophenol, the use ratio of raw materials is high, the waste of a by-product is avoided, and therefore, the production cost is greatly lowered. In addition, the 1,4-dichlorobenzene can obtain the 2,5-dichlorophenol through two different methods. The synthetic method has the advantages of simple synthetic process, low production cost, high raw material use ratio, less process byproducts and small three-waste output and is more suitable for large-scale industrial production.

The invention relates to a method for synthesizing a polyquaternary ammonium salt. According to the method, an organic solvent, secondary amine, epihalohydrin, acid, strong-base anion exchange resin and the like serve as raw materials, the polarity of the secondary amine is lowered through increasing chain length of a hydrocabon group carbon chain in the secondary amine, thus, the polarity of thepolyquaternary ammonium salt is lowered, and the polyquaternary ammonium salt with good intermiscibility with epoxy resin and good anti-electrostatic property is synthesized. A polyquaternary ammoniumsalt macromolecular antistat is developed for epoxy resin coating materials. The method has the characteristics that the energy consumption is low, the environmental pollution is light, the production process is simple and is short in rout, the investment of large-scale production is small, and the production efficiency is high, so that the industrialization prospect is good.

The invention discloses a microbial fuel cell for nitrogen and phosphorus removal of a sewage treatment plant and a sewage treatment method. The microbial fuel cell comprises a nitrogen and phosphorus removal pool, the nitrogen and phosphorus removal pool is provided with a water inlet and a water outlet, and a nitrogen and phosphorus removal unit is arranged in the nitrogen and phosphorus removal pool; the nitrogen and phosphorus removal unit comprises an iron pole plate and a carbon felt which are sequentially arranged along the water flow direction in the nitrogen and phosphorus removal tank, a denitrification biological membrane is attached to the carbon felt, a collecting hopper and a sludge hopper are respectively arranged below the iron pole plate and the carbon felt in the nitrogen and phosphorus removal tank, and the iron pole plate is electrically connected with the carbon felt through a wire; and a resistor is connected in series on a lead connected between the iron polar plate and the carbon felt. According to the invention, nitrogen and phosphorus in the wastewater can be removed, the blue iron ore can be recycled, and the treatment target of combining wastewater treatment and resource recycling is achieved.

The invention provides a preparation method of Stendra. The method comprises the following steps that starting materials 4-[(3-chloro-4-methoxyphenyl)methylamino]-2-[(S)-2-hydroxymethyl pyrrole-1-base]pyrimidine-5-carboxylic acid and 2-pyrimidinemethanamine are dissolved into a reactive solvent methylbenzene, a boric acid porphyrin catalyst is aded, heating and stirring are conducted to a reflux state, and the Stendra is obtained through catalysis. Accordingly, boric acid porphyrin serves as the catalyst, catalysis is conducted directly to synthesize the Stendra directly. The dosage of the catalyst is low, the reaction activity is high, operation is relatively simple, after the reaction is finished, a target product is likely to be separated from the catalyst, the difficulty of separationand purification of later products is greatly lowered, the recovered catalyst can be recycled, and the preparation cost can be significantly lowered, and the whole catalytic reaction has the advantages of being simple, environmentally friendly and the like, the input cost such as manpower and raw materials is significantly lowered, and large-scale industrial production is facilitated.