39results about How to "The synthesis process is simple and green" patented technology

The invention belongs to the fields of utilization of lignocelluloses and energy and chemical industry application, and discloses a green method for increasing enzymolysis efficiency of cellulose in rice straws through stepwise pretreatment with two deep co-melting solvents. The method includes the steps of: with one deep co-melting substance as a solvent, pre-treating the rice straws, and performing filtration and separation to obtain a residue; drying the residue and pre-treating the residue with the other one deep co-melting solvent in the same way, thus finally obtaining pre-treated rice straws; enzymolyzing the rice straw residue, as a substrate, with cellulase to finally obtain a saccharide liquid mainly comprising glucose. The method increases the enzymolysis efficiency of the rice straws, increases yield of fermentable reduced saccharide (glucose), overcomes defects that an ionic liquid pretreatment process is high in cost and is not environment-friendly, and also solves a problem of poor pretreatment effect with single deep co-melting solvent. The method also expands application range and increases utilization rate of some green deep co-melting solvents.

The invention belongs to the fields of lignocellulose utilization and energy and chemical application, and discloses a green method for increasing a cellulose enzymolysis efficiency in rice straws by utilizing lactic acid / guanidine hydrochloride to extract hemicellulose. The green method includes: taking the lactic acid / the guanidine hydrochloride as a solvent to preprocessing the rice straws, filtering and separating to obtain residues, and drying to obtain preprocessed rice straws; taking the rice straw residues as a base material, and subjecting the base material to enzymolysis by cellulose so as to obtain a liquid sugar which mainly comprises glucose. The green method has the advantages that the enzymolysis efficiency of the rice straws can be increased effectively, a yield rate of fermentable reducing sugar is increased, and the defects of high cost and environmental unfriendliness of an ionic liquid preprocessing process are overcome.

The invention relates to a synthesis method of a pyrrole [1,2a] quinoxaline derivative. The method comprises the steps: dissolving a cuprous complex, 2-bromoaniline, a pyrrole formaldehyde compound and an alkali in an organic solvent, carrying out a reaction, and carrying out separation and purification to obtain the pyrrole[1,2a] quinoxaline derivative, wherein the molar ratio of the cuprous complex to the 2-bromoaniline to the pyrrole formaldehyde compound to the alkali is (0.01-0.03): 1.0: 1.0: 1.5, the reaction temperature is 50-65 DEG C, and the reaction time is 6-8 hours. Compared with the prior art, the method has the advantages of mild reaction conditions, high yield, high substrate universality, less waste and the like.

The invention relates to a ruthenium complex containing a carboranyl benzimidazole structure as well as a preparation method and application of the ruthenium complex. The preparation method of the ruthenium complex comprises the following steps: 1) adding a n-BuLi solution into a carborane solution, and performing a reaction at room temperature for 30-60 min; 2) adding bromobenzimidazole, and performing a reaction at room temperature for 6-8 h; and 3) adding [(p-cymene)RuCl2]2, performing a reaction at room temperature for 3-5 h, and performing post treatment to obtain the ruthenium complex. The ruthenium complex is used to catalyze self-oxidative coupling of primary amines to prepare imine compounds. Compared with the prior art, the method provided by the invention uses the dinuclear ruthenium compound [(p-cymene)RuCl2]2 as a raw material, and the [(p-cymene)RuCl2]2 is reacted with the n-BuLi and o-carbonboryl benzimidazole to obtain the bivalent half-sandwich ruthenium complex containing the o-carbonboryl benzimidazole structure; and the ruthenium complex provided by the invention has stable physicochemical properties and thermal stability, is still stable at high temperature of300 DEG C, has a simple and green synthetic process, and exhibits excellent activity in the reaction of catalyzing the self-oxidative coupling of primary amines to prepare the imine compounds.

The invention belongs to the field of nano material preparation and biological medical application and particularly relates to a nuclear magnetic imaging and photodynamic / chemotherapy degradable silicon-based nano diagnosis agent and a preparation method thereof. The nano diagnosis agent disclosed by the invention is a SiO2-TA-Mn<+>-medicine-PEI compound nano particle; under a low pH and high GSHenvironment stimulation, a TA-Mn<+> structure in the compound nano particle can perform protonation and reduction reaction, a net structure is deconstructed, and medicine and metal ions for nuclear magnetic imaging are released out. Therefore, the nuclear magnetic imaging and photodynamic / chemotherapy degradable silicon-based nano particle nano diagnosis agent disclosed by the invention has the characteristics that the SiO2-TA-Mn<+>-medicine-PEI compound nano particle nano diagnosis agent has tumor position degradation response, magnetic resonance imaging, medicine response control release andthe like, and photodynamic therapy and chemotherapy combined synergistic oncotherapy under nuclear magnetic resonance imaging guidance is achieved.

The invention relates to a palladium complex containing an ortho-position carborane based benzimidazole structure, a preparation method and application thereof. The palladium complex is prepared by the following method of: dropwise adding an n-BuLi solution into a carborane solution and carrying out stirring reaction, then adding bromo-benzimidazole for continuous reaction, then adding PdCl2 intoa reaction system for continuous reaction, performing separation at the end of the reaction to obtain a palladium complex containing an ortho-position carborane based benzimidazole structure, and applying the complex to catalyzing the reaction of alkyne, carboxylic acid and olefin to prepare the alpha-methylene-gamma-butyrolactone compounds by a one-pot method. Compared with the prior art, the palladium complex disclosed by the invention is high in catalytic efficiency, and the lactone compound can be synthesized by utilizing simple and cheap raw materials under mild conditions.

The invention relates to an iridium complex containing a carboryl benzimidazole structure and a preparation method and application thereof. The preparation method of the iridium complex comprises the following steps: 1) adding the n-BuLi solution to the carborane solution, and then React at room temperature for 30-60min; 2) Add bromobenzimidazole and react at room temperature for 6-8h; 3) Add [Cp*IrCl 2 ] 2 , and react at room temperature for 3‑5h, after post-treatment to obtain the iridium complex; the iridium complex is used to catalyze the asymmetric reduction of aryl ketones to prepare chiral alcohols. Compared with prior art, the present invention uses binuclear iridium compound [Cp*IrCl 2 ] 2 As a raw material, it is reacted with n-BuLi and ortho-carboryl benzimidazole to obtain a trivalent iridium complex containing an ortho-carboryl benzimidazole structure. The iridium complex has stable physical and chemical properties and Thermal stability, and the synthesis process is simple and green. It catalyzes the asymmetric reduction reaction of aryl ketones to synthesize chiral alcohols under mild conditions. It has excellent catalytic activity, enantioselectivity and high yield.

The invention relates to a ruthenium complex containing a carboranyl benzimidazole structure as well as a preparation method and application of the ruthenium complex. The preparation method of the ruthenium complex comprises the following steps: 1) adding a n-BuLi solution into a carborane solution, and performing a reaction at room temperature for 30-60 min; 2) adding bromobenzimidazole, and performing a reaction at room temperature for 6-8 h; and 3) adding [(p-cymene)RuCl2]2, performing a reaction at room temperature for 3-5 h, and performing post treatment to obtain the ruthenium complex. The ruthenium complex is used to catalyze self-oxidative coupling of primary amines to prepare imine compounds. Compared with the prior art, the method provided by the invention uses the dinuclear ruthenium compound [(p-cymene)RuCl2]2 as a raw material, and the [(p-cymene)RuCl2]2 is reacted with the n-BuLi and o-carbonboryl benzimidazole to obtain the bivalent half-sandwich ruthenium complex containing the o-carbonboryl benzimidazole structure; and the ruthenium complex provided by the invention has stable physicochemical properties and thermal stability, is still stable at high temperature of300 DEG C, has a simple and green synthetic process, and exhibits excellent activity in the reaction of catalyzing the self-oxidative coupling of primary amines to prepare the imine compounds.

The invention relates to a method for synthesizing a beta-(N-pyrazolyl) ketone compound by base catalysis, which comprises the following steps of dissolving pyrazole and alpha, beta-unsaturated ketonein an organic solvent, adding base, reacting at a room temperature for 6-12 hours, and separating and purifying to obtain the beta-(N-pyrazolyl) ketone compound. Compared with the prior art, the method has the advantages of simple and green synthesis process, excellent selectivity, higher yield and wide substrate range, and has the wide application value in the fields of biology, pharmaceutical chemistry industry and the like.

The invention discloses a composite photocatalyst doped in a heterojunction interface and a preparation method. The prepared Bi12O17Cl2 / g-C3N4 composite photocatalyst doped in a heterojunction interface has extremely strong capability in converting carbon dioxide into methane under visible light. Since g-C3N4 and Bi12O17Cl2 nanosheets are adopted to be combined, a large-area heterojunction can be more easily formed, and thereby the separation of current carriers is promoted; by thermal diffusion, bismuth atoms on Bi12O17Cl2 at the heterojunction interface are successfully doped into a g-C3N4 crystal lattice, consequently, a super strong electric field at the heterojunction interface is induced, and super performance in reducing carbon dioxide under the visible light is achieved; the extremely large specific surface area and countless pores of porous g-C3N4 provide convenience for interface doping; the flow direction of current carriers is successfully controlled by matched band-gap structure and interface doping, selectively reducing carbon dioxide into methane is realized, and the recyclability of the photocatalyst is enhanced; material synthesis is simple and green, the scale is large, and the industrial application prospect is good.

The invention relates to a binuclear rhodium complex containing an ortho-carborane structure and its preparation and application. The preparation method of the rhodium complex comprises the following steps: 1) adding n-BuLi solution to the ortho-carborane solution, Then react at room temperature for 30-60min; 2) add selenium, and react at room temperature for 1-2h; 3) add [Cp*RhCl 2 ] 2 , and react at room temperature for 3‑6h, and obtain the rhodium complex after post-treatment; the rhodium complex is used to catalyze the N-methylation reaction of arylamine to prepare arylamine N-methylated derivatives. Compared with the prior art, the preparation method of the binuclear semi-sandwich rhodium complex containing the ortho-carborane structure in the present invention is simple and green, has excellent selectivity and higher yield, and the prepared rhodium complex is stable at room temperature It has high catalytic activity, can be used to catalyze the N-methylation reaction of arylamines to prepare N-methylated derivatives of arylamines, has high catalytic reaction yield, and has wide industrial application prospects.

The invention discloses a preparation method of a photostable antistatic polyformaldehyde material. In the method, 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxygen free radical (TEMPO), which has photostability and is used as a hydrogen bond donor and a hydrogen bond receptor, is used for preparing a photostable antistatic low-cofusion reagent, which is then mixed with an antistatic agent and polyformaldehyde uniformly, and the mixture is subjected to extruding granulation in a twin-screw extruder to obtain antistatic master batches; the antistatic master batches are uniformly mixed with a thermal stabilizer, an antioxidant and pure polyformaldehyde, and the mixture is subjected to extruding granulation in the twin-screw extruder; the granules finally are dried and injection-moulded to form the photostable antistatic polyformaldehyde material. The photostable antistatic polyformaldehyde material can significantly improve antistatic performance and photostability of a material in the field of electronics industry.

The invention relates to a method for synthesizing enamine under catalysis of a palladium imine complex containing pyridine ligands. The method comprises steps as follows: phenylacetylene and secondary amine are taken as raw materials, the palladium imine complex containing the pyridine ligands is taken as a catalyst, a hydroamination reaction is performed in a solvent, aftertreatment is performed, and enamine is obtained. Compared with the prior art, the method for preparing enamine compounds through the hydroamination reaction of phenylacetylene under the catalysis of a divalent palladium imine complex containing the pyridine ligands is provided, raw materials are simple and easy to obtain, a synthesis process is simple and green, the method has excellent selectivity and high yield, theatom economy is high, three wastes are reduced, and the method is environmentally friendly, simple and convenient to operate and suitable for industrial synthesis of the high-value enamine compounds.

The invention belongs to the fields of lignocellulose utilization and energy and chemical application, and discloses a green method for increasing a cellulose enzymolysis efficiency in rice straws by utilizing lactic acid / guanidine hydrochloride to extract hemicellulose. The green method includes: taking the lactic acid / the guanidine hydrochloride as a solvent to preprocessing the rice straws, filtering and separating to obtain residues, and drying to obtain preprocessed rice straws; taking the rice straw residues as a base material, and subjecting the base material to enzymolysis by cellulose so as to obtain a liquid sugar which mainly comprises glucose. The green method has the advantages that the enzymolysis efficiency of the rice straws can be increased effectively, a yield rate of fermentable reducing sugar is increased, and the defects of high cost and environmental unfriendliness of an ionic liquid preprocessing process are overcome.

The invention relates to a method for catalytically synthesizing an N-arylated derivative of pyrimidine-2-amine, which comprises the following steps: by taking an N, N-coordinated meta-carborane ligand-containing cuprous complex as a catalyst and taking pyrimidine-2-amine compounds and aryl halide compounds as raw materials, carrying out coupling reaction at room temperature to obtain the N-arylated derivative of pyrimidine-2-amine. The N-arylation derivative of the pyrimidine-2-amine is obtained. Compared with the prior art, the preparation method disclosed by the invention has the advantages that the N, N-coordinated cuprous complex containing the meta-carborane ligand is used as the catalyst, has higher catalytic activity under a mild condition, can be used for catalyzing Buchwald-Harwig coupling reaction of the pyrimidine-2-amine compound and the aryl halide compound to prepare the N-arylated derivative of pyrimidine-2-amine, is good in universality, and can be used for preparing the N-arylated derivative of pyrimidine-2-amine. The method has the advantages of mild reaction conditions, high catalytic efficiency, few byproducts, lower cost and easiness in separation of products.

The invention provides a method for preparing enamine compounds by catalyzing the hydroamination reaction of cyclohexylacetylene, which is characterized in that, under the catalysis of the catalyst, cyclohexylacetylene and secondary amine undergo hydroamination reaction in a solvent , to obtain enamine compounds; the molecular formula of the catalyst is [R 1 R 2 C(C 5 h 4 N) 2 ] Pd=NPh, wherein, R 1 and R 2 independently selected from H, CH 3 and Ph, the solvent is an aromatic hydrocarbon, the reaction temperature is 60-100°C, and the reaction time is 6-12h. The invention has mild reaction conditions, high catalytic efficiency, high atom economy, low cost, easy separation of products, no large amount of waste residue, and is suitable for industrial production.

The invention relates to single-phase samarium titanate nano-powder prepared by using a solution method, and a method for preparing the single-phase samarium titanate nano-powder. The method comprisesthe following steps: firstly dispersing a samarium source and a titanium source into a solvent according to a molar ratio of 1 to (1.1-1.3) to obtain a solution A; adjusting the pH value of the solution A to be neutral to obtain a milk-white mixed solution B; separating the milk-white mixed solution B to obtain white powder; drying the powder obtained in the third step, and then calcining to obtain the single-phase samarium titanate nano-powder. According to the method, the aim of accurately controlling the stoichiometric ratio of ternary Sm-Ti-O chemical elements is achieved by fully dissolving and dispersing the samarium source and the titanium source in a solvent medium as well as mixing and reacting the samarium source and the titanium source at an atomic scale, so that other impurities are prevented from appearing, and the aim of preparing the single-phase Sm2Ti2O7 is further realized.

The invention provides a large-steric-hindrance trivalent rhodium imide complex containing a rhodium-nitrogen dual-key structure. The large-steric-hindrance trivalent rhodium imide complex is characterized by including the following structure shown in the description. A synthesis technology is simple and green, and has excellent selectivity and a high yield. The large-steric-hindrance trivalent rhodium imide complex has the features of stable physical and chemical properties and thermal stability, and has excellent activity and regional selectivity in an anti-Markovnikov hydroamination reaction of olefins.

The present invention relates to N,N-coordinated palladium complexes containing meta-carborane ligands and preparation and application thereof. The preparation method of palladium complexes comprises the following steps: 1) adding n-BuLi solution to meta-carbon In the borane solution, react at room temperature for 30-60min; 2) add 3-chloromethylpyridine, and react at room temperature for 3-5h; 3) add PdCl 2 , and reacted at room temperature for 2-5 h, and the palladium complex is obtained after post-treatment; the palladium complex is used to catalyze the arylamine formylation reaction to prepare the arylamine carboxamide compounds. Compared with the prior art, the synthesis process of the palladium complex in the present invention is simple and green, and has excellent selectivity and high yield; the palladium complex has the characteristics of stable physical and chemical properties, thermal stability, etc. It exhibits excellent catalytic activity in the acylation reaction.

The invention relates to a nickelous imine complex with a nickel nitrogen double-bond structure and preparation and application of the nickelous imine complex. The preparation method of the nickelousimine complex comprises the following steps that 1, a phenyldipyridine ligand solution is added into a zero-valent nickel precursor solution for a reaction for 3-5 hours at room temperature; 2, azidobenzene is added for a reaction for 2-5 hours at room temperature, and through aftertreatment, the nickelous imine complex is obtained. The nickelous imine complex is used for catalyzing an anti-Markovnikov hydroamination reaction of styrene to prepare a linear-chain amine compound. Compared with the prior art, the synthesizing technology is simple and green, the selectivity and the yield are high,the nickelous imine complex prepared by using the method has the advantages of stable physicochemical properties, thermal stability and the like, and the nickelous imine complex can show excellent activity and regioselectivity in the reaction of catalyzing the anti-Markovnikov hydroamination reaction of the styrene.

The present invention relates to the application of a kind of binuclear rhodium complex in fatty amine N-methylation reaction, with binuclear rhodium complex as catalyst, with CH 3 I, as a methylating agent, catalyzes the N-methylation reaction of fatty amines in an organic solvent to prepare N-methylated derivatives of fatty amines. Compared with the prior art, the binuclear rhodium complex in the present invention has higher catalytic activity at room temperature, and can be used to catalyze the N-methylation reaction of fatty amines to prepare N-methylated derivatives of fatty amines, and the catalytic reaction The yield is high (90‑97%), the reaction conditions are mild, no strong base is required, all reagents are stable to air and water, the requirements for reaction equipment are not high, and there is a wide range of industrial application prospects.

The invention relates to the application of a palladium complex in fatty carbamylation reaction, using N,N-coordinated palladium complex containing meta-carborane ligand as catalyst, and N,N-dimethyl Formamide is used as a formylating reagent and solvent to catalyze the formylation reaction of fatty amines to prepare fatty amine formamide compounds. Compared with the prior art, in the present invention, the divalent palladium complex containing meta-carborane ligands coordinated by N,N has higher catalytic activity under mild conditions, and can catalyze the formylation reaction of aliphatic amines , DMF is used as a formylating reagent and a solvent at the same time, it is cheap, low-toxic and easy to separate, and the yield is high (88‑96%).

The invention relates to a method for catalyzing and synthesizing enamines by utilizing palladium imine complexes containing pyridine ligands. , the hydroamination reaction occurs in the solvent, and the enamine is obtained after post-treatment. Compared with the prior art, the present invention provides a method for preparing enamine compounds by utilizing a divalent palladium imine complex containing a pyridine ligand to catalyze the hydroamination reaction of phenylacetylene. The raw materials are simple and easy to obtain, and the synthesis process is simple and green. , has excellent selectivity and high yield, high atom economy, reduces the generation of three wastes, is environmentally friendly, easy to operate, and is suitable for industrial synthesis of high-value enamine compounds.