77results about How to "Avoid separation and purification" patented technology

The invention discloses a expansion-type charring agent for a flame-retardant polyolefine material and a synthesis method thereof. The synthesis method comprises the following steps: by using cyanuric chloride as an initial raw material, dropwisely adding amine containing benzene ring, phenol or thiophenol and an acid binding agent into an ice bath to obtain a monosubstituted compound; dropwisely adding aliphatic diamine or aliphatic dibasic alcohol and an acid binding agent, heating to 40-60 DEG C to react, thereby obtaining a disubstituted compound; and finally, dropwisely adding the aliphatic diamine or aliphatic dibasic alcohol and the acid binding agent, heating to 80-110 DEG C, refluxing with a condenser, cooling, washing, and drying to obtain the expansion-type charring agent containing benzene ring, triazine ring and diamino or dialkoxy group. The reaction process adopts a one-pot method, and thus, the invention has the advantages of simple technique, short reaction time and environmental protection in the preparation process; the product has the advantages of high thermal stability, favorable charring effect, low water absorptivity and favorable compatibility with alkene polymers; and after being compounded with ammonium polyphosphate (APP), the product is applicable to polyolefin materials, and has favorable flame-retardant effect.

The invention belongs to the technical field of surfactants, and provides a method for preparing a cationic gemini surfactant (CH3(CH2)m-N(CH3)2-CH2CH(OH)CH2-N(CH3)2(CH2)nCH3.Cl2) by taking epoxy chloropropane and alkyl dimethyl tertiary amine (CH3-(CH2)n-N(CH3)2, wherein n equals to 7, 9, 11, 13, 15 or 17) as raw materials and taking 2-hydroxyl-1.3-propylidene as a linking group. The method provided by the invention overcomes the defect in the prior art that one extremely excessive material is required for improving the reaction yield, dispenses with separation and purification procedures for a finished product, is short in reaction period, leaves no epoxy chloropropane in the finished product, and is suitable for industrial scale production.

The invention discloses a recombinant bacterium and application of the recombinant bacterium to the generation of rebaudioside D by catalyzing rebaudioside A. The recombinant bacterium contains a tomato-derived glycosyltransferase UGTSL2 gene and a potato-derived sucrose synthase StSUS1 gene; the tomato-derived glycosyltransferase UGTSL2 gene is cloned between NdeI and XhoI sites of pRSFDuet-1 to construct a recombinant plasmid pRSFDuet-SL2; then the potato-derived sucrose synthase StSUS1 gene is cloned between NcoI and EcoRI sites of the pRSFDuet-SL2 to construct a recombinant plasmid pRSFDuet-SL2-SUS1; the recombinant plasmid pRSFDuet-SL2-SUS1 is transferred into a host cell to obtain the recombinant bacterium. After the recombinant bacterium is subjected to induction expression, the recombinant bacterium is added into a reaction mixture to catalyze the rebaudioside A to generate the rebaudioside D; in reaction, crude enzyme liquid obtained by crushing the recombinant bacterium is utilized and separation and purification of an enzyme are avoided; lyophilized powder does not need to be produced; UDP (Uridine Diphosphate) or UDP-glucose and any cell penetration agent or other chemical reagents do not need to be added into a reaction solution, so that the recombinant bacterium has a better environment-friendly property. The yield of the rebaudioside D can reach 10.8g / L.

The invention discloses a method for identifying uronic acid-containing polysaccharide in a biological tissue. The method comprises the following steps: 1, extracting crude polysaccharide in the biological tissue; 2, hydrolyzing the crude polysaccharide with trifluoroacetic acid, and removing acid from the obtained hydrolysate; 3, carrying out derivatization on the residues obtained from the step 2 with 1-phenyl-3-methyl-5-pyrazolone to prepare derivatives of sugar; 4, preparing a reference solution from the identified uronic acid-containing polysaccharide by the methods in the step 2 and the step 3; and 5, analyzing and extracting the derivatives of sugar from the step 3 and the reference substance from the step 4 by a liquid chromatogram-mass-spectrometric technique, and identifying the uronic acid-containing polysaccharide in the biological tissue by comparison. According to the method, the polysaccharide in the biological tissue can be directly detected; fussy separation and purification processes are avoided; the used sample amount is relatively low; and the result can be obtained within a relatively short period of time.

The invention discloses a recombinant bacterium and application of the recombinant bacterium to preparation of rebaudioside M2 by catalyzing rebaudioside A. The recombinant bacterium contains a tomato-based glycosyltransferase UGTSL2 gene and a potato-based sucrose synthase StSUS1 gene at the same time; the tomato-based glycosyltransferase UGTSL2 gene is cloned between NdeI and XhoI sites of pRSFDuet-1 and is constructed to obtain a recombinant plasmid pRSFDuet-SL2; then the potato-based sucrose synthase StSUS1 gene is cloned between NcoI and EcoRI sites of the pRSFDuet-SL2 and is constructed to obtain a recombinant plasmid pRSFDuet-SL2-SUS1; the recombinant plasmid pRSFDuet-SL2-SUS1 is transferred into a host cell to obtain the recombinant bacterium. After the recombinant bacterium is subjected to induced expression, crude enzyme liquid is taken and is added into a reaction mixture to catalyze the rebaudioside A to generate the rebaudioside M2; in a reaction process, the crude enzyme liquid obtained by crushing the recombinant bacterium is utilized and separation and purification of an enzyme are avoided; lyophilized powder is also not needed and substrates including rebaudioside D and UDP or UDP-glucose and any cell penetration agent or other chemical reagents do not need to be added, so that the environmental friendliness is better. The yield of the rebaudioside M2 reaches 11.09g / L.

The invention discloses a method for removing residual bimetallic catalyst in a polyether polyol product with low degree of unsaturation, which is characterized by adopting the adsorption method to remove the catalyst, and can greatly simplify the process flow, reduce impurities introduced into the product, realize high purification rate, improve the stability of late-stage storage of the polyether polyol with low degree of unsaturation, improve the product quality and be widely applied in the purification of the polyether polyol with low degree of unsaturation.

The invention discloses a glycosyltransferase UGTZJ1 mutant. The amino acid sequence of the mutant is shown as any one of SEQ ID NO.2-4, and a gene for encoding the mutant and a preparation method ofthe mutant are also disclosed. The invention also discloses a vector, a cell and a genetically engineered bacterium containing the mutant encoding gene. The invention also discloses applications of the glycosyltransferase UGTZJ1 mutant, the gene for encoding the mutant, the vector and a cell line comprising the mutant encoding gene, particularly the genetically engineered bacterium containing theglycosyltransferase UGTZJ1 mutant, and the like in the aspect of catalyzing rebaudioside A to generate rebaudioside D. The yield of the rebaudioside D, which is generated by catalyzing the rebaudioside A through the genetically engineered bacterium containing the mutant, is increased by about 4 times compared with that of a wild type, and the yield of the rebaudioside D can reach 47.56 g / L under the optimal reaction condition.

The invention belongs to the field of electrochemical organic synthesis, and particularly relates to a device and method for device and method for coupled electro-catalytic hydrogen peroxide production and selective organic matter oxidation. According to the invention, the reaction device is composed of an anode chamber, a cathode chamber and an organic catalysis chamber, wherein the cathode chamber contains a catalyst for hydrogen peroxide production through oxygen reduction; the anode chamber contains a water oxidation or hydrogen oxidation catalyst; the organic catalysis chamber contains an organic matter oxidation catalyst; the anode chamber and the organic catalysis chamber are separated by a cation exchange membrane; and the cathode chamber and the organic catalysis chamber are separated by an anion exchange membrane. During working of the device, oxygen or air is introduced into the cathode chamber, hydrogen or water is introduced into the anode chamber, and an organic reactant is introduced into the organic catalysis chamber; and under an electrifying condition, a cathode is subjected to oxygen reduction to obtain OOH<->, an anode is subjected to water oxidation or hydroxide reaction to obtain H< + >, the H<+> enters the middle organic catalysis chamber through the corresponding anion and cation exchange membranes to form H2O2, and organic matters are further oxidized under the action of the catalyst. According to the invention, low-concentration hydrogen peroxide generated by oxygen reduction is directly used for oxidation of the organic matters, so problems in separation, concentration, storage and transportation cost and safety of H2O2 are avoided, and remarkable economic benefits are achieved. When the device is used for phenol oxidation, benzyl alcohol oxidation, furfuryl alcohol oxidation and cyclohexanone conversion, the selectivity of target products including benzenediol, benzaldehyde, furfural and cyclohexanone-oxime is greater than 98%, and corresponding total current efficiency is 21-49%.

The invention discloses a synthetic method of a cyclic enamine-3-formic acid ester compound and belongs to the field of organic synthesis technology. The main point of the technical scheme is as shown in the specification. In comparison with the prior art, the invention has the following advantages: (1) by the adoption of one-pot cascade reaction, tedious intermediate separation purification process is avoided, waste emission is decreased, and environmental burden is reduced; (2) raw materials are easily available; (3) the reaction is carried out at the temperature of minus 100 DEG C, condition is mild, and operation is simple; (4) the application range of a substrate is wide; and (5) atom economy of the reaction is high.

The invention discloses a process for recycling and regenerating lithium cobalt oxide in a waste lithium cobalt oxide battery, which comprises the steps of firstly separating a collector and a cathodematerial in a positive pole plate of the lithium cobalt oxide battery by using an organic solvent N-methyl-2-pyrrolidinone (NMP), then removing residual impurities such as acetylene black and polyvinylidene fluoride (PVDF) in the cathode material by means of calcination, leaching cobalt and lithium elements in the cathode material by citric acid, and finally directly regenerating LiCoO2 from a leaching solution by adopting a sol-gel method, wherein citric acid plays a dual role of a leaching agent and a chelating agent in the process. According to the invention, a one-step technology route coupling an organic acid leaching method and a sol-gel method is adopted to recycle and regenerate LiCoO2, thereby avoiding the damage of organic acids to the environment, simplifying the recycling andregenerating process, reducing the cost, and achieving harmless treatment requirements while recycling the waste lithium cobalt oxide battery.

The invention discloses a novel expansion-type charring agent for a flame-retardant polyolefine material and a synthesis method thereof. The synthesis method comprises the following steps: by using cyanuric chloride as an initial raw material, dropwisely adding amine containing benzene ring, phenol or thiophenol and an acid binding agent into an ice bath to obtain a monosubstituted compound; dropwisely adding aliphatic diamine or aliphatic dibasic alcohol and an acid binding agent, heating to 40-60 DEG C to react, thereby obtaining a disubstituted compound; and finally, dropwisely adding the aliphatic diamine or aliphatic dibasic alcohol and the acid binding agent, heating to 80-110 DEG C, refluxing with a condenser, cooling, washing, and drying to obtain the novel expansion-type charring agent containing benzene ring, triazine ring and diamino or dialkoxy group. The reaction process adopts a one-pot method, and thus, the invention has the advantages of simple technique, short reaction time and environmental protection in the preparation process; the product has the advantages of high thermal stability, favorable charring effect, low water absorptivity and favorable compatibility with alkene polymers; and after being compounded with ammonium polyphosphate (APP), the product is applicable to polyolefin materials, and has favorable flame-retardant effect.

The invention relates to a hydrolysis method of astilbin. The method for preparing texifolin by hydrolyzing astilbin comprises the following steps: taking 48-52 parts by weight of astilbin, adding 300-1050 parts by volume of a 0.5-2.8 mol / L citric acid water solution while stirring, and carrying out hydrolysis at 85-135 DEG C for 1.2-3.8 hours to obtain a hydrolysate; filtering the hydrolysate while the hydrolysate is hot, concentrating the filtrate to 180-220 parts by volume, standing for at least 12 hours, crystallizing, filtering, and respectively collecting the filter cake and the filtrate, wherein the filter cake is a texifolin crude product; and recrystallizing the texifolin crude product to obtain the texifolin. The method avoids using the macroporous resin for separating and purifying the texifolin, thereby lowering the production cost and being beneficial to industrial production. Another hydrolysate-rhamnose of the astilbin is separated and purified, thereby enhancing the utilization ratio of the astilbin. The acid used by hydrolysis can be recovered and recycled, thereby avoiding the problems of waste of resources, environmental pollution and the like.

The invention discloses a synthetic method for pyrroline-3-formic ether compounds, and belongs to the technical field of organic synthesis. The technical key point of the synthetic method is disclosed in the following diagram. Compared with the prior art, the synthetic method has the following advantages: (1) one-pot cascade reaction is adopted so as to avoid a complex intermediate separation and purification process, reduce waste emission and lower environment burdens; (2) raw materials can be easily obtained; (3) reaction is carried out below 100 DEG C, conditions are moderate, and operation is simple; (4) the applicable range of a substrate is wide; (5) the economy of reacting atoms is high.

The invention relates to a preparation method of a PDMS-PP composite membrane and application of the PDMS-PP composite membrane to MDI waste brine treatment. The preparation method comprises the following steps: pretreating a PP supporting base membrane, performing plasma treatment, preparing a silicone rubber membrane solution, coating the PP supporting base membrane with thesilicone rubber membrane solution, and drying to obtain the composite membrane. Waste brine treatment comprises the following steps: 1), conveying MDI waste brine into an extracting membrane tube of membrane extraction equipment, conveying an extractant into a shell layer of the membrane extraction equipment, and extracting to obtain crude brine, wherein the extracting membrane tube is produced from the PDMS-PP composite membrane; 2), mixing the crude brine with an oxidant, sending into an oxidation reactor, and reacting to obtain refined brine; 3), reducing excess oxidant in the refined brine by using a reducingagent to obtain qualified brine. A treatment method has the advantages of low energy consumption, simple technological process, low equipment investment and the like; by the treatment method, TOC in the waste brine can be treated till the concentration is lower than 10 ppm.

The invention discloses a one-pot method for preparing a hydrophilic phytosterol / stanol derivative, and belongs to the technical fields of food, cosmetics, medicine and chemical engineering. Phytosterol / stanol and diacid or diacid anhydride react for a period of time under the action of ionic liquid to generate the high-purity intermediate product phytosterol / stanol diacid monoester; a hydrophilic modifier is directly added to the reaction system for further reaction without separating the intermediate product, so that a high-purity hydrophilic phytosterol / stanol derivative is prepared. The hydrophilic phytosterol / stanol derivative with purity over 95% can be obtained through extraction separation. The two phases of esterification reaction are conducted in one pot, technological operation is simple, usage and separation of a solvent are reduced, the technological process is short, and energy consumption is reduced. The obtained hydrophilic phytosterol / stanol derivative is high in purity, high in yield and low in cost, and the method is good for industrial production.

The invention discloses a method for efficient synthesis of difructose anhydride III. According to the method, saccharose is converted into inulin firstly by means of inulin sucrose without glycan separation, and then inulin is converted by means of inulin fructotransferase to generate functional disaccharide difructose anhydride III through synthesis. The technology is simple, efficiency is high, and the conversion rate of inulin for synthesis of difructose anhydride III can reach 40-54%. To obtain high-purity difructose anhydride III, micromolecule monosaccharide in reaction liquid is removed by means of yeast, and the finally obtained high-purity difructose anhydride III is easy to separate and purify and has broad market prospects.

The invention discloses a method for separating and purifying deoxynucleoside triphosphate, which comprises the following steps: when the temperature is below 4 DEG C, depositing deoxynucleoside triphosphate biosynthesized reaction solution directly with an organic solvent to obtain a solid mixture of the deoxynucleoside triphosphate, wherein the volume ratio of the deoxynucleoside triphosphate biosynthesized reaction solution to the organic solvent is between 1:1 and 1:25; when the temperature is below the 4 DEG C, dissolving the solid mixture in ultrapure water, adjusting the pH value to between 0.1 and 2 by using acidic aqueous solution, and using the organic solvent to perform deposition again to obtain a solid matter of the deoxynucleoside triphosphate; and dissolving the solid matter in the ultrapure water, adjusting the pH value to between 5 and 11 by using sodium hydroxide alkaline aqueous solution, and performing liquid nitrogen frozen and freeze-drying to obtain a sodium salt product of the deoxynucleoside triphosphate. The method has the advantages of quick separation, good purification effect, production cost reduction, water resource pollution reduction, process energy consumption reduction, and applicability to industrial production.

The invention relates to a method for extracting ice structuring protein from clovers. The invention aims to solve the problems of the prior art that the extraction raw materials of the ice structuring protein are limited, the extraction process is complex, the cost is relatively high, and the extracted ice structuring protein can not be widely used in frozen food and medical science. The extraction method comprises the following steps: (1) taking dry leaves of the clovers, and grinding and sieving; (2) preparing an ice ball of which the diameter is 2cm; (3) mixing alfalfa meal and a phosphate buffer solution, and centrifuging; (4) adding the ice ball into supernatant liquid, and extracting; and (5) extracting the ice structuring protein again. The method provided by the invention has the advantages that the extraction concentration is high, impurities are few, the cost and time are saved, the molecular weight can be determined by directly performing SDS-PAGE, cold induction is not needed, the raw materials are convenient and easy to obtain, the cost is low, and the extraction process is simple and can be universally applied to frozen food. The method is suitable for extracting the ice structuring protein from the clovers.

The invention discloses a synthesis method for preparing chiral polysubstituted 1,2-dihydropyridine as well as polysubstituted pyridine and chiral piperidine derived from chiral polysubstituted 1,2-dihydropyridine by using a "one-pot serial connection method". The method comprises the following step: by taking an imine compound and an aldehyde compound as raw materials, performing an asymmetric Mannich reaction, a Wittig reaction and an intramolecular ring-closing reaction in sequence, so as to synthesize a chiral 1,2-dihydropyridine compound with high three-dimensional selectivity. The product does not need to be purified, and a polysubstituted pyridine compound can be prepared through oxidation aromatization through further "one-pot serial connection", and a polysubstituted chiral piperidine compound can be also prepared through catalytic hydrogenation after separation and purification. The method starts from simple and easily obtained raw materials, separation and purification of anintermediate are avoided, and compounds of 1,2-dihydropyridine, polysubstituted pyridine and chiral piperidine are efficiently synthesized through simples steps of operation. Nitrogenous six-memberedring frameworks which are synthesized by using the method and disclosed by the invention are all common in many natural products and medicine molecules, and have great significances for acceleratingmedicine research and development.

The present invention discloses new 1,3-dihydroxy-3,7-dimethyl-6-octen-2-one synthesis method, which comprises racemic synthesis and enantioselective synthesis. According to the present invention, commercially available 6-methyl-5-hepten-2-one (CAS:110-93-0) is adopted as a starting material, two one-pot series connection reaction systems are adopted, simple operations are performed, the separation purification of the intermediate is effectively avoided, the high-yield racemic synthesis of the 1,3-dihydroxy-3,7-dimethyl-6-octen-2-one is achieved, and the asymmetric synthesis method for enantioselective synthesis of (R)-1,3-dihydroxy-3,7-dimethyl-6-octen-2-one and (S)-1,3-dihydroxy-3,7-dimethyl-6-octen-2-one is developed. The present invention further discloses an intermediate compound.

The invention discloses a preparation method of a lithium ion battery positive electrode composite material and a precursor thereof, and in particular relates to a novel method for preparing a high-purity low-cost binary or ternary precursor and preparing a high-performance lithium ion battery binary or ternary positive electrode composite material by utilizing the precursor, belonging to the technical field of new energy materials and the preparation thereof. The method comprises the following specific steps: (1) putting salt-type solid raw materials of two or three of nickel, cobalt and manganese with crystal water into a reactor, and heating the materials to the molten state; (2) introducing ammonia under the protection of inert gas, supplementing a small amount of water or no water according to the solubility of salts at different temperatures, stirring and reacting; (3) evaporating ammonium salt after full reaction, taking the solid out, and drying so as to get the amorphous binary or ternary positive electrode composite material precursor; and (4) mixing the precursor with lithium carbonate according to a certain ratio, and further preparing the lithium ion battery positive electrode composite material through a two-section sintering method. The precursor synthetic method is simple, sodium hydroxide is avoided from being used, separation and purification are not required, and the high-purity positive electrode composite material precursor which has no impurities basically can be obtained; furthermore, no industrial waste water is discharged, and the by-product ammonium salt can further generate economic benefit; and the positive electrode composite material prepared by the precursor has excellent performances, and is convenient for industrialization.

The invention relates to a method for preparing asenapine. Specifically, the invention relates to a method for preparing a medicinal asenapine free alkali and a crystal form thereof, and also relatesto a preparation method of an intermediate compound used in the method.

The invention discloses a method for synthesizing 3-acyl hydrogenated azepine compounds, and belongs to the technical field of organic synthesis. The method comprises the steps of: adopting a seven-membered cyclic amine compound and 2-oxo-2-aryl acetic acid as raw materials, and performing a one-pot serial reaction to obtain the 3-acyl hydrogenated azepine compound directly, and the method comprises the specific operation steps of: dissolving the seven-membered cyclic amine compound 1 and 2-oxo-2-aryl acetic acid 2 in an organic solvent, then adding a copper salt catalyst and an oxidizing agent, and performing heating to raise the temperature for a reaction to obtain the 3-acyl hydrogenated azepine compound 3. The method has the advantages of a convenient operation process, mild conditions, a wide application range of the substrates and a potential prospect suitable for industrial amplification.

The invention discloses a catalyst and a method for preparing an asymmetric substituted aryl compound or a terphenyl derivative by a one-pot tandem reaction under the catalysis of functionalized imidazole salt and palladium salt. The catalyst mainly comprises the functionalized imidazole salt and the palladium salt in a ratio of 1:2 to 6:1. The method comprises the following steps: using the catalyst to respectively carry out one-pot tandem reactions between Heck / Suzuki, Heck / Heck, and Heck / Sonagashira by using aryl halides or a derivative thereof as a substrate in organic solvent; and directly preparing the asymmetric substituted aryl compound because intermediate products need not to be separated. A prepared chlorinated biphenyl compound can also carry out a Suzuki or Buchwald-Hartwig reaction for preparing the terphenyl derivative and an amino biphenyl compound. The catalyst has simple preparation and extremely low consumption and can catalyze more than two different coupling reactions, thereby having high efficiency and low cost; and the one-pot tandem reaction method has simple and convenient operation and mild conditions, avoids pollution, reduces waste, obtains high-yield valuable products and can be widely applied to the fine chemistry industry, the pharmaceuticals industry, and the like.

The invention discloses a one-pot method for preparing a hydrophilic phytosterol / stanol derivative, and belongs to the technical fields of food, cosmetics, medicine and chemical engineering. Phytosterol / stanol and diacid or diacid anhydride react for a period of time under the action of ionic liquid to generate the high-purity intermediate product phytosterol / stanol diacid monoester; a hydrophilic modifier is directly added to the reaction system for further reaction without separating the intermediate product, so that a high-purity hydrophilic phytosterol / stanol derivative is prepared. The hydrophilic phytosterol / stanol derivative with purity over 95% can be obtained through extraction separation. The two phases of esterification reaction are conducted in one pot, technological operation is simple, usage and separation of a solvent are reduced, the technological process is short, and energy consumption is reduced. The obtained hydrophilic phytosterol / stanol derivative is high in purity, high in yield and low in cost, and the method is good for industrial production.

The invention relates to a Baeyer-Villiger monooxygenase and an application of the Baeyer-Villiger monooxygenase in synthesis of briracetam. The Baeyer-Villiger monooxygenase is preferably selected from any one of polypeptides with an amino acid sequence as shown in SEQ ID No: 1, SEQ ID No: 2, SEQ ID No: 3, SEQ ID No: 4 or SEQ ID No: 5. Under the catalysis of the Baeyer-Villiger monooxygenase disclosed by the invention, (R)-4-propyl-dihydrofuran-2-ketone can be synthesized economically, efficiently and environmentally friendly, and on the basis, a Briracetam bulk drug with high optical purity can be prepared through a one-step reaction. The route for preparing the briracetam provided by the invention avoids chiral resolution and tedious separation and purification used in the traditional process, is suitable for industrial production, and has a remarkable cost advantage.