294results about How to "Mild reaction temperature" patented technology

The invention relates to a silicon-acrylic three-block copolymer with low surface energy and a process for preparation, which relates to the synthesis of silicon-acrylic low-surface-energy three-block copolymer. The invention provides a silicon-acrylic three-block copolymer with low surface energy, whose structure of reaction product is accurate, and the original skeleton construction of each block is kept. The invention relates to a dimethyl silicone polymer-b- polymethyl methacryate-b-poly n-butyl methacrylate. And the process for preparation comprises first, preparing dimethyl silicone polymer macromolecule initiating agent of the dead ends of bromine atoms, second, preparing two-block macromolecule initiating agent of copolymer dimethyl silicone polymer-b-polymethyl methacryate, third, preparing two-block copolymer macromolecule initiating agent of dimethyl silicone polymer-b- polymethyl methacryate, finally, preparing three-block novel copolymer of dimethyl silicone polymer-b- polymethyl methacryate-b-poly n-butyl methacrylate.

The invention discloses a synthesis process of chiral pyrrolidine and intermediates. The synthesis process adopts 2, 5-difluorohalobenze or 5-fluoro-3 halogenated pyridine as the raw material substrate, and employs a chiral catalyst to induce chiral reaction so as to reduce a ketone compound into a corresponding chiral alcohol compound, and then carries out substitution reaction to introduce an easily leavable group to an alcoholic hydroxyl group so as to facilitate ring formation reaction (or carry out ring formation reaction directly). The process provided by the invention has the advantagesof significant increase of product yield and reduction of cost, also the reaction temperature is mild, and the process is easy to control and industrialize.

The invention relates to a preparation method of hydrofluoroether. The preparation method comprises the following steps: (1), dissolving an alkali compound in fluorine-containing alkanol, adding a solvent, adding fluorinated olefin, and heating and stirring for reaction to obtain a mixed solution; (2), washing the mixed solution obtained in the step (1) by using water, standing for demixing, collecting an organic phase solution of a lower layer, and rectifying to obtain a hydrofluoroether product. According to the preparation method, the generation of double-bond impurities can be inhibited, and a reaction product from which a target product is easily purified can be obtained; the reaction temperature and the reaction pressure are relatively mild, the safety coefficient is high, and more satisfactory reaction speed can be obtained; the solvent is easily recycled, the cost is lowered, and a plurality of wastes are prevented from polluting the environment.

The invention relates to a fluorine-silicon three-block copolymer and a process for preparation, which relates to the synthesis of fluorine low-surface three-block copolymer. The invention provides a fluorine-silicon three-block copolymer and a process for preparation, whose reaction condition is moderate, the structure of the reaction products is accurate, the original skeleton construction of each block is kept, the production has micro-phase separation structure, and the operation is simple and convenient. The invention is named as dimethyl silicone polymer-b-polymethyl methacryate-b-poly seven-fluorine butyl methacrylate ester, the process for preparation comprises first, preparing dimethyl silicone polymer macromolecule initiator of the sealing end of bromine atom, second, preparing two-block copolymer macromolecule initiator of the dimethyl silicone polymer-b-polymethyl methacryate, finally, preparing the fluorine-silicon three-block copolymer of the dimethyl silicone polymer-b-polymethyl methacryate-b-poly seven-fluorine butyl methacrylate ester.

The invention relates to a method for extracting low-molecular-weight lignin from biomass. The preparation method comprises the following steps of (1) preparing an extraction agent: preparing cholinechloride and hydrogen bond donors into a mixed solution at a certain mol mass ratio; then, performing reaction under a certain condition to form a uniform solution, namely the extraction agent; (2) adding the extraction agent into the biomass raw materials; adding catalysts; performing reaction for a certain time under the stirring condition at a certain temperature; performing filtering; adding deionized water; performing precipitation and centrifugation to obtain solid substances; then, cleaning the solid substances by absolute ethyl alcohol and deionized water; performing drying; obtaininga finished product. According to the method, poplar, bamboo-willow, wheat straw and the like are used as the biomass raw materials; the solvent prepared at a specific proportion under the specific conditions is used as the extraction agent for extracting the low-molecular-weight lignin. The method has the advantages that the reaction conditions are mild; the process is simple; green effect and high efficiency are realized; the extraction cost is low; the method is suitable for large-scale production application.

The invention discloses a method for preparing a tribromophenol, which is characterized in that bromine is generated by the hydrogen peroxide reaction between a hydrogen bromide and an oxidant, and then the bromine continues to react with a phenol to synthesize a tribromophenol, and the method can be finished with no middle steps. A crude product passes through water, a sodium bicarbonate liquor and a sodium bisulfite liquor, then after the simple treatments of water washing, impurity removal and filtration, the product can be got. The method has the advantages of simple and convenient process, easy operation, high reaction safety, less pollution and simple post processing. The yield ratio can reach to more than 96 percent. The product has a high purity, is easy to realize industrial production and has a strong practicality.

The invention discloses an organic ligand and a Pd/Pb-based bi-metal organic framework as well as a synthetic method and application of the organic ligand and the Pd/Pb metal organic framework. A structural formula of the Pd/Pb-based bi-metal organic framework (Pd/Pb-MOF) is [Pb4(C42H28N8O8Pd)(C2O4)Br4]n, wherein n is a nonzero natural number. The Pd/Pb-based bi-metal organic framework (Pd/Pb-MOF) is used as a catalyst to be applied to catalyzing benzyne homocoupling and catalyzing three-component coupling reaction of benzyne, boracic acid and allyl halohydrocarbon. The MOF catalyst with active sites can be used for replacing some heavy metals to achieve a catalytic effect, so that the harm of the heavy metals to the environment is reduced. The MOF catalyst with the active sites is used for catalysis, so that heterocatalysis is realized; additionally, the bi-metal organic framework catalyst can be recycled for more than four times, and the catalyst is easy to recycle, so that the utilization rate of the catalyst is increased, and the cost is reduced.

The invention discloses an organic ligand L for synthesizing a Co (II) based metal organic framework, a Co (II) based metal organic framework Co-MOF-1 and a Co (II) based metal organic framework Co-MOF-2. The metal organic framework Co-MOF-1 is synthesized by virtue of the ligand L at first, and then crystals of the Co-MOF-1 are placed in the air for 24 hours at room temperature and then are subjected to constant-temperature treatment for 2 hours at 70 DEG C to obtain a novel catalyst Co-MOF-2 with active spots. The catalyst can be used for effectively catalyzing cyclohexane oxidation reaction, and a heavy metal is not needed to serve as a catalyst for reaction, so that the harm of the heavy metal to the environment is reduced, the reaction temperature is mild, the reaction time is relatively short, the usage amount of the catalyst is small, other additives are avoided, and the catalyst can be repeatedly used for more than 5 times relative to a free heavy metal salt.

The invention discloses an enzymatic beating process for natural-color bagasse pulp. Xylanase is used in the enzymatic beating process for the natural-color bagasse pulp. The process comprises the steps of sizing agent defibering, enzyme treatment, washing, PFI beating, sheet making and physical detection. By adopting the process, the beating energy consumption of the natural-color bagasse pulp can be lowered effectively; the beating degree can be increased greatly up to 19.2 percent when enzyme treatment is performed on the xylanase at the dry pulp dosage of 30IU/g; meanwhile bagasse pulp cellulase can be protected from being damaged, and the process has important significance to the production of industrial paper from bagasse pulp.

The invention discloses a flexible electrochromic film based on tungsten oxide, and a preparation method and an application of the flexible electrochromic film. The flexible electrochromic film is made from amorphous tungsten oxide, has a loose and porous nano-morphology, and has the thickness of 200-400nm and the average pore diameter of about 100-300nm. The flexible electrochromic film has a loose and porous structure, so that the permeation and contact of an electrolyte are facilitated, and a path of charge transfer is shortened; and therefore, the flexible electrochromic film is good in electrochromic performance and wide in optical modulation range. The flexible electrochromic film based on the tungsten oxide has the characteristics of being flexible and bendable; and the flexible electrochromic film still has the electrochromic performance when being bent for more than 90 degrees. The preparation method is simple in preparation process, mild in reaction temperature and low in cost; and a possible preparation method is provided for industrial production of the tungsten oxide-based flexible electrochromic film.

The invention discloses an organic ligand L for synthesizing a triphase catalyst UiO-67-IM and the triphase catalyst UiO-67-IM. The triphase catalyst UiO-67-IM has the structural formula of [Zr6O4(OH)4L6]n, wherein n is a nonzero natural number. A preparation method of the triphase catalyst UiO-67-IM comprises the steps that the organic ligand L, ZrCl4 and acetic acid are dissolved into DMF, heat preservation is conducted for 24 hours at 120 DEG C, the temperature is lowered to room temperature, and then the metal organic framework UiO-67-IM is obtained. The catalyst can effectively catalyze a benzyl chloride azidation reaction, heavy metal salt does not need to serve as the catalyst, heterogeneous catalysis is achieved, the catalyst can be repeatedly utilized 5 times or above and is easy to recycle, the utilization rate of the catalyst is increased, and the cost is reduced; meanwhile, the catalyst is mild in reaction temperature, short in reaction time, low in dosage, free of other additives and beneficial for industrialized application and popularization.

The invention discloses a method for synthesizing organosilicon-modified ultrafine aluminum hypophosphite, which comprises the following steps: 1) preparing sodium hypophosphite aqueous solution; 2) preparing aluminum sulfate aqueous solution; 3) preparing organosilicon-modified ultrafine aluminum hypophosphite : First add a dispersant to the sodium hypophosphite solution, then slowly add the aluminum sulfate aqueous solution to the sodium hypophosphite solution dropwise, and continue to stir for 0 to 3 hours; After stirring for 0-1h, cool to room temperature, wash and test the filtrate with a certain concentration of barium chloride solution, and wait for no white precipitate to appear in the filtrate, then place it in an oven for drying to obtain organosilicon-modified ultrafine aluminum hypophosphite product . The present invention uses organic silicon as a modifier to make organic silicon modified aluminum hypophosphite and high molecular compound more tightly combined, improve the interfacial binding force between the flame retardant and high molecular material, the reaction conditions are mild, and the yield is high , which is more suitable for industrialization.

The invention relates to a preparation method of valnemulin hydrochloride. The preparation method comprises the following steps: reacting pleuromutilin with p-toluenesulfonyl chloride, substituting with 1-amino-2-methyl propyl-2-mercaptan hydrochloride so as to obtain [(2-amino-1,1-dimethyl S, 6S, 8R,9R, 9aR, 10R)-6-vinyl decahydro-5-hydroxyl-4,6,9,10-tertamethyl-1-oxo-3a, 9-propanol-3aH-cyclopentacyclooctene-8-yl ester for later use; reacting D-valine with methyl acetoacetate; synthesizing the product with isobutyl chloroacetate so as to generate anhydride; and reacting anhydride with [(2-amino-1,1-dimethyl ethyl) sulfenyl] acetic acid (3aS, 4R, 5, 6S, 8R,9R, 9aR, 10R)-6-vinyl decahydro-5-hydroxyl-4,6,9,10-tertamethyl-1-oxo-3a, 9-propanol-3aH-cyclopentacyclooctene-8-yl ester so as to generate amide, and then carrying out deprotection with hydrochloric acid so as to prepare valnemulin hydrochloride. The method has the advantages that (1) reaction temperature is mild, thereby being applicable to large-scale production; (2) post-treatment is simple, thereby directly obtaining the product; (3) used solvents are less, thereby reducing environmental pollution; and (4) the valnemulin hydrochloride content and yield of the obtained product are high.

The invention provides a preparation method for a 4-aryl isoquinoline-1,3(2H,4H)-diketone compound. The preparation method comprises the following steps: in a solvent, with imide as shown in a formula(II) which is described in the specification as a raw material, and in the presence of a palladium catalyst, a ligand and alkali, allowing the imide to react with substituted aromatic hydrocarbon asshown in a formula (III) which is described in the specification so as to generate the 4-aryl isoquinoline-1,3(2H,4H)-diketone compound as shown in a formula (I) which is described in the specification. The preparation method provided by the invention has the advantages of stable operation, high yield, low production cost, etc.; preparation of a target object can be completed by a one-step reaction; the operation is simple and convenient; the yield is high and generally reaches 90% to 99%; the use of an expensive and hazardous reagent is avoided; a synthetic method with large-scale preparationvalues is realized; conditions are stable; the yield is high; and a selection for a novel preparation method is provided for development and application of an isoquinoline diketone compound. The preparation method provided by the invention has a synthetic route as described in the specification.

The invention relates to a preparation method of a biomass-based phenolic resin. According to the invention, a biomass monomer 2,5-diformyl furan and phenol are adopted as raw materials; under the catalyzing of alkali, a temperature of 30-200 DEG C, and nitrogen gas protection, the raw materials are subjected to a addition and condensation reactions for 1-10h; and water and other impurities in the reaction system are removed with a vacuum distillation method, such that a novel phenolic resin high-quality product with 2,5-diformyl furan for substituting formaldehyde is obtained. With the method, the prepared product has the advantages of high yield, easy separation, and environment-friendliness. The method has good application prospect.

A method of molysite-catalyzed atom transfer radical polymerization under natural light irradiation belongs to the technical field of high polymer chemical reaction methods. A monomer, an initiator, a molysite catalyst, a ligand of ferric salt and a reducing agent for radical polymerization are combined into a polymerization reaction system according to certain proportion for atom transfer radical polymerization under the natural light irradiation and in presence of oxygen to obtain a polymer after the reaction. The obtained polymer has the characteristics of living polymerization. The method is simple in conditions, easy in operation and energy-saving, and provides a simple-cost living polymerization technology.

The invention discloses a preparation method of a sulfur dioxide and epoxide copolymer. According to the method, a novel polysulfone material is prepared through copolymerization of sulfur dioxide and epoxide under the catalytic action of SalenMX, epoxide and SalenMX are sequentially added to a high-pressure reaction kettle, sulfur dioxide is introduced and has a reaction at the temperature of 50-100 DEG C for 8-48 h, then, a product, namely, the sulfur dioxide and epoxide copolymer is obtained, the product is dissolved with chloroform, a hydrochloric acid and methanol mixed solution is used for precipitation, amber precipitates are filtered and repeatedly washed with methanol for 2-4 times, the washed product is transferred to a vacuum drying box and dried in vacuum at the room temperature for 8-24 h, and the sulfur dioxide and epoxide copolymer with higher stereoregularity can be obtained. The preparation method is simple, few catalysts are used, the reaction temperature is mild, the yield is high, the structure regularity of the product is good, the cost is low, and industrial production is easy to realize.

The invention provides a pyrogallic acid production method. The pyrogallic acid production method comprises the following steps of: mixing gallic acid and paranitroaniline in a mass ratio of 100: (2-2.5), putting the mixture in a reaction kettle, slowly heating to 140 DEG C till the mixture is melted completely; transferring the molten material to a subliming kettle, standing still for 20-30 minutes, opening a vacuum system, heating the subliming kettle, slowly warming up, controlling the temperature at 130 DEG C to 150 DEG C, and collecting a distilled subliming product till no subliming product is distilled, and thus the distilled subliming product is pyrogallic acid. The pyrogallic acid production method has the advantages that a special decarboxylation reagent, namely, the paranitroaniline, is selected, so that the gallic acid is subjected to a decarboxylation reaction at the temperature of 130-150 DEG C so as to generate the pyrogallic acid, the conversion rate of the gallic acid reaches above 98%, the yield of the high-quality product (analytical pure and chemical pure) reaches above 80%; and the reaction temperature in the method is mild, and the whole working procedure time is short.