33results about How to "Simple purification method" patented technology

The invention belongs to the technical field of biochemical engineering and the technical field of bioengineering, and discloses a schizochytrium limacinum engineering strain for producing EPA (eicosapentaenoic acid) by prolonging a desaturation path. Part or all of the extended desaturase genes from thraustochytrium sp. And fusarium sp. And saprolegnia are expressed. According to the invention, extended desaturase genes from various sources are integrated into a schizochytrium limacinum genome, so that a schizochytrium limacinum gene engineering strain efficiently expresses the extended desaturase genes, and a heterologous EPA synthesis path with high synthesis efficiency, short culture period, simple purification method and low cost is provided; a basis is provided for producing grease rich in EPA from schizochytrium limacinum, and the problems of non-sustainability, high cost and the like caused by obtaining EPA from fishes are solved.

The invention discloses electronic grade boric acid as well as a purification method and application thereof, and belongs to the technical field of chemical processes. The purification method of the electronic grade boric acid comprises the following steps: S1, oil removal: carrying out oil removal on a boric acid crude product solution through an adsorbent to obtain boric acid oil removal liquid; and S2, ion exchange: purifying the boric acid oil removal liquid through an ion exchanger to obtain the electronic grade boric acid solution. The purification method is simple and efficient, impurities in the boric acid crude product solution can be effectively removed through the steps of oil removal and ion exchange, the electronic grade boric acid solution with low total metal impurity content and low total organic carbon content is obtained, and the electronic grade boric acid solution has stable and good use performance and is suitable for industrial production. And the method is particularly widely applied to the field of nanoscale chip integrated circuits.

The invention relates to the technical field of marine chemical engineering, in particular to thiolated chitosan quaternary ammonium salt containing thiophene groups as well as a preparation method and application of the thiolated chitosan quaternary ammonium salt. The thiolated chitosan quaternary ammonium salt containing the thiophene group has a structure as shown in a formula I in the specification. The preparation method comprises the following steps: further reacting sulfhydrylated chitosan to obtain sulfhydrylated chitosan quaternary ammonium salt, and further introducing thiophene groups into the chitosan quaternary ammonium salt by taking the sulfhydrylated chitosan quaternary ammonium salt as a reaction raw material. Antioxidant activity experiments prove that the obtained thiolated chitosan quaternary ammonium salt derivative has good antioxidant activity, and can be widely researched and applied as an antioxidant in the fields of biological medicine, agriculture and the like. And the # imgabs0 # is shown in the formula 1.

The invention discloses a cobalt complex with cyano-modified tetrapyridine as a ligand, a synthesis method and application thereof. The synthesis method of the cobalt complex with cyano-modified tetrapyridine as a ligand is to dissolve the ligand 4′,4″-dicyano tetrapyridine in a mixed solvent of methanol and dichloromethane, then add a cobalt salt, stir the obtained mixture at room temperature for 24 hours, filter and remove insoluble matter after the reaction, remove the organic solvent by rotary evaporation, and wash the obtained solid with water, ethanol and dichloromethane respectively to prepare the cobalt complex with 4′,4″-dicyano tetrapyridine as a ligand. The synthesis method of the invention has the advantages of simple process, high yield, mild reaction conditions, simple product purification treatment method, etc. The cobalt complex with 4′,4″-dicyano tetrapyridine as a ligand synthesized by the invention has good catalytic activity for the photocatalytic selective reduction of carbon dioxide to formic acid under normal temperature and pressure conditions, and the TON (turnover number) can reach 1048, and has good potential application prospects.

The invention discloses a preparation method and application of a reactive flame retardant containing double DOPO groups and nitrogen heterocycles, and the preparation method of the reactive flame retardant comprises the following steps: adding an amino compound R-NH2 and terephthalaldehyde into a reactor with a stirring device, adding a solvent, adding an acid to adjust the pH value to 6, then heating until the solvent is refluxed, keeping the refluxing temperature to react for a period of time, and cooling to room temperature to obtain the reactive flame retardant containing double DOPO groups and nitrogen heterocycles. Reaction liquid containing an imine intermediate product is obtained; then adding DOPO, controlling the reaction temperature to be the solvent reflux temperature, and keeping the reflux temperature to react for a period of time; after the reaction is finished, cooling, carrying out suction filtration, washing and drying to obtain a reaction type flame retardant containing double DOPO groups and nitrogen heterocyclic rings; the reaction formula is as follows: # imgabs0 # amino compound R-NH2 is 4-aminopyridine or 3-aminopyrazole, namely R is pyridyl or pyrazolyl. The synthesis and purification method of the flame retardant is simple, the reaction yield is high, and the flame retardant effect of epoxy resin can be remarkably improved by adding the flame retardant into bisphenol A epoxy resin through modification.

The invention belongs to the technical field of organic synthesis and drug intermediate preparation, and relates to a resolution preparation method of a monepantel key intermediate. In the first aspect, the invention provides a preparation method of a compound shown as a formula 3, which comprises the following steps: # imgabs0 #, in which R1 is selected from TMS, TES, TBDMS, TIPS, TBDPS or # imgabs1 #, the reaction is as follows: # imgabs2 # comprises the following steps: step 2, reacting a compound shown as a formula 2 with an ammonia source and a cyaniding reagent to obtain the compound shown as the formula 3; according to the method 2, the reaction is as follows: # imgabs3 # comprises the following steps: step 5, a compound shown in a formula 7 is subjected to the action of ammonia gas to obtain a compound shown in a formula 3; on the second aspect, the invention provides a preparation method of a compound shown as a formula 5, and the reaction is as follows: # imgabs4, in which R1 is as described in the first aspect; the method comprises the following steps: step 3, obtaining a compound shown as a formula 5 from a compound shown as a formula 3 under the action of a resolving agent. The method disclosed by the invention is higher in yield, simpler in post-treatment and simple and convenient to operate, and has a good industrial production prospect.

The present invention provides a method for preparing high-purity n-hexane, comprising: adding analytical grade sulfuric acid to industrial grade n-hexane, stirring, and standing to separate the n-hexane; further removing impurities from the n-hexane through a modified molecular sieve; and finally adsorbing the n-hexane using long-wave ultraviolet light modified activated carbon. The industrial grade n-hexane removed impurities by adsorption of analytical grade sulfuric acid is successively subjected to a water vapor modified molecular sieve removal treatment and a long-wave ultraviolet light modified activated carbon adsorption treatment to directly obtain chromatographic grade high-purity n-hexane with a purity of not less than 99.99% and a 215nm ultraviolet transmittance of not less than 98%. The method is simple, easy to operate, stable in operation, and suitable for industrial purification applications.

The invention discloses a bio-based polyamide nanofiltration membrane and application thereof, and belongs to the technical field of synthesis of bio-based polyamide nanofiltration membranes and purification of 5-hydroxymethylfurfural and 2, 5-furandicarboxylic acid. According to the invention, 2, 5-dimethyl furandicarboxylate and hexamethylenediamine are used as raw materials, polydimethyl furandicarboxylate hexamethylenediamine prepared by an amine ester exchange method is used as a film-forming polymer, and a solution phase inversion method is further adopted to prepare the bio-based polyamide nanofiltration membrane polydimethyl furandicarboxylate hexamethylenediamine membrane. The method has the advantages that 5-hydroxymethylfurfural and soluble humin can be selectively separated by the aid of the method, impurities in 2, 5-furandicarboxylic acid sodium salt aqueous solution can be separated, and accordingly the high-purity 5-hydroxymethylfurfural and 2, 5-furandicarboxylic acid can be prepared.

The invention discloses a purification method of vitamin E, and relates to the technical field of bioengineering. Comprising the following steps: extracting a raw material vitamin E with a solvent 1, and filtering to obtain a filter cake; mixing the filter cake, a solvent 2 and silica gel to obtain a mixture; loading the mixture on a silica gel column, eluting with an eluent, and concentrating to obtain a vitamin E crude product; and mixing the vitamin E crude product with the solvent 3, heating, cooling, and taking a vitamin E layer to obtain the purified vitamin E. The vitamin E purification method is simpler and more convenient, the product purity is higher, the yield is higher, the process stability is high, and the repeatability is good.

The present invention relates to the field of semiconductor technology, and in particular to a method for preparing high-purity silicon carbide by chemical vapor deposition, comprising the following steps: (1) distilling and purifying a raw material monomethyltrichlorosilane to make its purity greater than 99.99% and its impurity content less than 5 ppm; (2) mixing the purified monomethyltrichlorosilane with hydrogen, vaporizing, and reacting; (3) cooling the tail gas after the reaction to room temperature, then pressurizing it to 0.6-1.0 MPa, exchanging heat with a refrigerant, and further cooling it to -40°C to form a condensate, and sending the condensate to a distillation and purification process to separate and obtain high-purity monomethyltrichlorosilane; (4) sending the uncondensed tail gas in step (3) to bubbling elution and distillation separation to separate hydrogen chloride from the adsorption-saturated chlorosilane liquid; and (5) subjecting the tail gas after bubbling elution to activated carbon pressure swing adsorption to separate high-purity hydrogen.

The present disclosure relates to a method for preparing a uricase variant and a novel method for purifying a uricase. Specifically, the uricase variant has higher activity and stability than the wild-type uricase; the purification method reconstructs the purification steps compared to the traditional method, and brings about a better purification effect through ammonium sulfate fractionation precipitation, dialysis, chromatography, secondary dialysis, ultrafiltration concentration and freeze drying.

The invention provides a preparation method of N-[4-2-(formylamino acetyl)-5-methoxy-2-phenoxy phenyl)]-methanesulfonamide, which comprises the following steps: carrying out formylation reaction on a compound shown in a formula I and a compound shown in a formula III to obtain N-[4-2-(formylamino acetyl)-5-methoxy-2-phenoxy phenyl)]-methanesulfonamide, the preparation method disclosed by the invention adopts an ester compound as an acylating agent, has the advantages of small solvent dosage, no need of strong acid, high controllability, convenience and easiness in post-treatment operation and the like, and is suitable for industrial mass production.

This invention discloses a purification method for 2-bromo-1-(5-iodothiophene-2-yl)-ethyl ketone. Specifically, it includes the following steps: (1) slurrying crude 2-bromo-1-(5-iodothiophene-2-yl)-ethyl ketone in solvent A; (2) slurrying the product obtained in step (1) in solvent C; and (3) recrystallizing the product obtained in step (2) in solvent D. The purification method of this invention is simple and easy to implement, yields a product with high purity, and is suitable for industrial production.

The present invention relates to a method for synthesizing 2-fluoro-3-formyl-pyridine-4-boric acid pinacol ester. The method mainly solves the technical problem that the compound lacks a synthesis method. The present invention uses conventional and easily available 2-fluoro-4-bromopyridine as a raw material, undergoes a formylation reaction with ethyl formate in tetrahydrofuran and HMPA after LDA dehydrogenation, and then undergoes a coupling reaction with double boron pinacol ester in dioxane and DMSO with 2-isooctanoate as a base under palladium catalysis to obtain 2-fluoro-3-formyl-pyridine-4-boric acid pinacol ester. The present invention has the advantages of easy raw material availability, short synthesis route, simple operation, easy purification, high yield, etc.

The invention relates to the technical field of organic synthesis, and particularly provides a preparation method of polyethylene glycol, which comprises the following steps: S1, reacting triethylene glycol with triphenylchloromethane to generate a first intermediate; s2, reacting the first intermediate with paratoluensulfonyl chloride to generate a second intermediate; s3, reacting the second intermediate with a diol compound to generate a third intermediate; and S4, removing a protecting group at the tail end of the third intermediate to obtain the polyethylene glycol. According to the preparation method provided by the embodiment of the invention, the purification method of the intermediate product is simple, the operation condition is mild and simple, the production cost is reduced, the operation is convenient, and the method is more suitable for industrial production.

The invention discloses a near-infrared fluorescent probe with an aggregation-induced emission enhancement effect. The near-infrared fluorescent probe is used for dual detection of hydrogen sulfide and hydrazine. The fluorescent probe is synthesized by carrying out Knoevenagel condensation reaction on 4-hydroxy-3-(1, 4, 5-triphenyl-1H-imidazolyl) benzaldehyde (I) and 2-(2-methyl-4H-chromene-4-subunit) malononitrile (II) under the catalytic action of piperidine, and the chemical structural formula of the fluorescent probe is as shown in the formula (III). The fluorescent probe shows high selectivity and high sensitivity to both hydrogen sulfide and hydrazine, the detection limits are as low as 50.1 nM and 89.2 nM respectively, and the fluorescent probe can be used for various scenes such as food spoilage monitoring and environmental water sample detection, can be used for biological imaging, and shows important application potential in the aspect of detection of hydrazine and hydrogen sulfide in organisms.

The application discloses a kind of methacrylic acid succinic acid double ester starch and its preparation method and application in corneal defect in situ filling agent, belong to the technical field of biomedical materials.The methacrylic acid succinic acid double ester starch is grafted carboxylation treatment to starch, then graft double bond is prepared.The corneal defect in situ filling agent of the application is composed of methacrylic acid succinic acid double ester starch (StacMA), methacrylated gelatin (GelMA), photo initiator and solvent.The natural biological macromolecule based corneal filling agent of starch and gelatin in the application has good biocompatibility, excellent light response adhesion characteristics and excellent mechanical properties, and the in-situ photocrosslinking of hydrogel is realized by ultraviolet irradiation, while excellent mechanical properties and strong adhesion capacity are generated, to realize the stable adhesion of in-situ forming artificial cornea on corneal implant bed, promote the regeneration of damaged corneal natural structure and the reconstruction of visual function.

An amide-containing aromatic diamine has the following structural formula: where Ar is a group with an aromatic ring structure. The preparation method includes the following steps: (1) mixing and reacting components including aromatic diamine, p-nitrobenzoic acid, alkyl phosphoric anhydride and polar aprotic organic solvent; (2) adding carboxylic acid and halogen-free quaternary ammonium salt to the product obtained in step (1) to obtain a mixed solution, which is placed in the cathode cell of an H-type electrolytic cell; the anode cell and the cathode cell are separated by a Nafion membrane; adding the same polar aprotic organic solvent and halogen-free organic electrolyte as the cathode cell to the anode cell of the H-type electrolytic cell, and adding a metal ion-free reducing agent; and conducting the reaction by electrolysis; (3) purifying the cathode reaction solution obtained in step (2) by post-treatment to obtain the amide-containing aromatic diamine. The yield, purity and whiteness of the amide-containing aromatic diamine are higher.

The present invention discloses a preparation method and application of an OP bidentate imine vanadium complex, and belongs to the technical field of olefin polymerization catalysts. The vanadium complex provided by the present invention is used as a main catalyst, and under the activation of a small amount of a co-catalyst, can catalyze the homopolymerization of ethylene, and has the advantages of high catalytic activity, good thermal stability, long service life, and applicability to a variety of solvent systems; it catalyzes the copolymerization of ethylene and α-olefins, and can obtain a polymer product with a high comonomer content with ultra-high activity catalysis; at the same time, the metal complex can also catalyze the copolymerization of ethylene and a hydroxyl-containing polar monomer to obtain a functionalized polyolefin product.

The invention discloses a preparation method and volumetric three-dimensional application of 4-{[(E)-(2-phenylpropyl-2-yl) nitrogen subunit] methyl} benzene-1, 3-diphenol Schiff base, and particularly, the molecular structure of the Schiff base compound is as shown in the following formula (I): # imgabs0 #, R1 is C1-6 alkyl, R2 is aryl, and R3 is C1-12 alkyl. The Schiff base compound is high in transparency and good in light transmission in media such as solutions and solids, and can be stably stored and used for a long time.

The invention provides a method for producing a spider silk-silk novel composite fiber and improving the performance of bombyx mori silk, which comprises the following steps: according to the N-terminal sequence NT of South African arachnoid main ampulla gland silk protein MaSp1, the repetitive sequence unit W of arachnoid ventricosa meglumine silk protein AcSp1, and the C-terminal sequence CT of arachnoid ventricosa secondary ampulla gland silk protein MiSp1, carrying out a reaction on the N-terminal sequence NT of the South African arachnoid; the method comprises the following steps: constructing a chimera spider silk protein gene sequence of a repetitive sequence unit W containing four AcSp1, artificially synthesizing a gene, and constructing a targeting Donor plasmid through a homologous recombination technology; the method comprises the following steps: carrying out micro-injection, and introducing a targeting Donor plasmid, a Cas9 plasmid for providing Cas9 nuclease, and plasmids of sgRNA1 and sgRNA2 sequences aiming at a silkworm FIB-H No. 2 exon into a fertilized egg within 1-6 hours after silkworm spawning; after silkworm eggs are hatched, screening through fluorescence labeling genes, and carrying out multiple times of culture and continuous generation to obtain a transgenic silkworm breed line capable of stably inheriting the chimera spider silk protein gene; bombyx mori silk glands are used as a bioreactor to secrete chimeric spider silk protein, and the chimeric spider silk protein enters silkworm cocoons along with spinning and cocooning behaviors of bombyx mori.

The invention discloses a preparation method of a carbohydrate compound. The invention provides a preparation method of a carbohydrate compound, which comprises the following steps: in an organic solvent, in the presence of alkali, carrying out hydroxyl protection reaction on a compound 1 and 4, 4-dimethoxytriphenylchloromethane to obtain the carbohydrate compound as shown in a compound 2, the molar ratio of the 4, 4-dimethoxy triphenyl chloromethane to the compound 1 is (0.8 to 1.5): 1. The method has the advantages that by-products are turned into wealth from wastes, the synthesis efficiency is high, the reaction conditions are mild, the specific reaction of target sites can be realized, the conversion rate is high, the by-products are few, the purification method is simple and convenient, and the like. The preparation method has the advantages of simplicity and convenience in operation and post-treatment, high yield, high product purity and the like. # imgabs0 #

The invention discloses a synthesis method of (Z) type conjugated enol phosphate, which comprises the following steps: (1) synthesis of enol phosphate: reacting 4-chloroacetoacetate with phosphite ester, ending LC-MS (liquid chromatography-mass spectrometry) detection, and separating and purifying the product to obtain enol phosphate; and (2) synthesis of (Z) type conjugated enol phosphate: mixing enol phosphate, triethylamine and acetonitrile, stirring at room temperature for reaction, ending LC-MS detection, and separating and purifying the product to obtain the (Z) type conjugated enol phosphate. The method has the advantages of milder reaction conditions, higher efficiency, higher yield and better selectivity.

The invention discloses a method for purifying cefradine, and belongs to the technical field of medicine purification. The method comprises the following steps: (1) suspending to-be-purified cefradine in a mixed solution of purified water and petroleum ether, dropwise adding an acidic reagent under a temperature-controlled stirring condition to adjust the pH value of a system, stirring until the solution is clear, standing for phase splitting, and reserving a water phase and a filtering membrane to obtain a filtrate; (2) adding a dispersing agent into the filtrate obtained in the step (1) to obtain feed liquid, and sequentially crystallizing and growing the feed liquid in four stages of connected crystallization production tanks by simultaneously adjusting the temperature and pH of each stage of crystallization production tank in a gradient manner; and (3) after crystal growing is finished, filtering, washing, vacuum drying and discharging to obtain a white solid of cefradine. The method is simple, energy-saving and environment-friendly, and the obtained cefradine product has the advantages of high content, few impurities and good stability, and is suitable for large-scale industrial production.

The invention discloses a method for purifying a phosphoramidite precursor, and particularly provides a method for purifying a compound as shown in a formula II, which comprises the following step: in a solvent, in the presence of an additive B, carrying out salt forming reaction on the compound as shown in the formula II. The purification method disclosed by the invention is simple, does not need special equipment, and is relatively low in cost, good in repeatability, free of wall sticking and good in yield. # imgabs0 #

The present invention belongs to the technical field of mass spectrometry analysis. The present invention provides a mass spectrometry immunoassay method for disease marker detection. The method comprises the following steps: analyzing precipitation data to obtain a precipitation performance value; comparing the precipitation performance value with a precipitation performance threshold value, judging whether the precipitation is qualified according to the comparison result, acquiring temperature data within a monitoring period, analyzing the temperature data, and obtaining an interference influence value; comparing the interference influence value GR with the interference influence threshold value, judging whether the temperature abnormality is the cause of the unqualified precipitation in the precipitation process according to the comparison result, obtaining a temperature abnormality performance value and a precipitation abnormality performance value, processing the temperature abnormality performance value and the precipitation abnormality performance value to obtain an influence performance ratio, analyzing the influence performance ratio to obtain an influence factor existence judgment value, and determining whether there are other influence factors in the precipitation process according to the influence factor existence judgment value. The present invention realizes the optimization of the purification method in the immunocoprecipitation process.

The invention relates to a method for adjusting the ratio of two configurations 16-R and S in beraprost sodium shown in a formula (I) through recrystallization. The method comprises the following steps: adding a mixed solvent into a beraprost sodium crude product, and stirring to obtain a system, so as to obtain the beraprost sodium crystal. According to the method disclosed by the invention, the 16-R / S ratio of the beraprost sodium crude product can be adjusted to 0.9-1.1 / 1 from about 1.2-1.4 / 1, so that the beraprost sodium API pharmacopoeia standard is met. The invention also provides a crystal of beraprost sodium. The method disclosed by the invention is simple to operate and easy to produce, and can be industrially amplified. # imgabs0 #

The present invention discloses a method for preparing a recombinant duck Tembusu virus E protein domain III protein. The present invention first provides a Pichia pastoris GS115 strain for preparing duck Tembusu virus E protein domain III. The recombinant strain is obtained by intercepting the duck Tembusu virus envelope protein EDIII antigen region, optimizing the codons to obtain the coding sequence of the duck Tembusu virus EDIII protein, and then cloning it into a yeast expression vector pPIC9K and transforming it into a yeast host strain GS115. Under the action of methanol, the duck Tembusu virus EDIII protein is efficiently expressed. At the same time, the protein is used as a coating antigen for a duck Tembusu virus antibody indirect ELISA diagnostic kit, which has high specificity, repeatability and stability, and can be used for the diagnosis of related diseases caused by Tembusu virus.

The invention provides an anti-HER2 (Human Epidermal Growth Factor Receptor 2) nano antibody polymer, and the anti-HER2 nano antibody polymer comprises not less than two anti-HER2 nano antibody monomers which are used for recognizing different epitopes of HER2; the at least two anti-HER2 nano antibody monomers are A9F5 and H2F5, the amino acid sequence of the anti-HER2 nano antibody monomer A9F5 is as shown in SEQ ID NO.1, and the amino acid sequence of the anti-HER2 nano antibody monomer H2F5 is as shown in SEQ ID NO.2. The invention further discloses a preparation method of the anti-HER2 nano antibody. The anti-HER2 nano antibody polymer is easy to express in a eukaryotic system, and the purification mode is simple; different epitopes of HER2 protein can be specifically recognized, and the kit can be used for diagnosis and treatment of HER2 positive tumors. The invention also provides an anti-HER2 nano antibody fusion protein and a pharmaceutical composition containing the anti-HER2 nano antibody fusion protein. The anti-HER2 nano antibody fusion protein and the pharmaceutical composition containing the anti-HER2 nano antibody fusion protein can be used for preparing drugs for treating HER2 positive tumors.

The invention discloses a preparation method of substituted diphenyl porphyrin-2-formaldehyde, belongs to the technical field of preparation of porphyrin derivatives, and solves the problem of excessive operation steps in the existing preparation of formyl porphyrin. The method comprises the following steps: reacting 5-substituted phenyl dipyrromethane and trialkyl orthoformate in an organic solvent system in an oxygen-free environment until the system is in a transparent state; dropwise adding organic acid, and reacting at room temperature under a dark condition until the 5-substituted phenyl dipyrromethene is completely reacted; and adding a pH regulator to regulate the reaction system to be alkaline, mixing until the reaction is quenched, and introducing oxygen for oxidation reaction to obtain the substituted diphenyl porphyrin-2-formaldehyde. According to the method provided by the invention, the preparation method of the substituted diphenyl porphyrin-2-formaldehyde is reduced from four steps to one step, the dosage of reagents is remarkably reduced, the operation is simple and convenient, and the product is easy to separate.