32results about How to "Synthetic process green" patented technology

The invention provides a method for preparing anisic aldehyde. The method comprises the following steps: dissolving p-hydroxy benzaldehyde in an organic solvent, under the action of a catalyst composition, implementing methylation reaction with dimethyl carbonate, filtering and distilling the obtained reaction liquid, thereby obtaining anisic aldehyde, wherein the catalyst composition comprises a first catalyst as a phase transfer catalyst and a second catalyst selected from an alkaline catalyst, an acid catalyst or a biological enzyme catalyst; the mole ratio of p-hydroxy benzaldehyde, dimethyl carbonate and the first catalyst to the second catalyst is (0.5-1):1.24:(0.05-0.1):(0.2-0.75); the phase transfer catalyst is tetramethylammonium chloride, tetramethyl ammonium bromide or tetrabutylammonium bromide. The yield of a final target product of the method is greater than 90%, the product purity is greater than 99%, the utilization rate of dimethyl carbonate is 61%, and the process is safe, economic and environment-friendly.

The invention discloses a synthetic process of an imidazo phenanthroline compound shown in a formula (III), which comprises the following steps: mixing phenanthroline diketone shown in a formula (I) with aldehyde and ammonium salt shown in a formula (II), and conducting condensation reaction after evenly grinding the mixture, thus obtaining the imidazo phenanthroline compound shown in the formula(III) after complete reaction. In the synthetic process, without the presence of catalyst acid, the synthesis of an imidazole ring is realized by grinding and reacting the phenanthroline diketone with the aldehyde and the ammonium salt under solvent-free conditions, so that the synthetic process has the characteristics of being green and efficient, and is suitable for industrial production.

The invention relates to a method for synthesizing metoxyl acetophenone. The high-yield and high-purity metoxyl acetophenone is synthesized from anisole and acetic anhydride in the presence of zinc chloride serving as a catalyst and dichloromethane serving as a solvent through Friedel-Crafts acylation reaction under normal temperature condition. The method is simple in synthesis process, low in cost and gentle in reaction condition, the synthesis yield is improved to 90%, the purity is 99.5%, and meanwhile waste liquid is well used to prepare the zinc chloride. The method is free of environmental risk, remarkable in economic benefits and applicable to large-scale production.

The invention relates to a method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol. 2-methyl-3-butene-2-alcohol takes Saucy-Marbet reaction with 2-alkoxylpropylene in the near critical state to obtain methyl heptenone. The synthesis method has the advantages that the use of catalysts is not needed; the selectivity of the product of methyl heptenone can be improved.

The invention discloses a process for synthesizing ethyl chloride. In a closed reactor, an ethyl chloride product can be obtained from ethanol and hydrogen chloride gas under the catalytic effect of AlCl3-ZnCl2 double component catalyst by gradually heating for reaction, releasing step by step and recovering. The high activity of AlCl3-ZnCl2 double component catalyst is used in the method, reaction temperature and by-product diethyl ether are reduced, and the yield of the ethyl chloride is increased to above 95%; by the use of the hydrogen chloride for replacement of industrial hydrochloric acid, mother liquor and distillate are directly continuously applied, energy consumption for distillation distillate recovery and hydrogen chloride loss are effectively reduced, environment pollution caused by production of a lot of high salt wastewater and organic waste acid can be avoided; in addition, by use of a closed staged heating reaction way, a catalytic substitution reaction is performed in a liquid phase system, substrate contact reaction time is increased, ethanol conversion rate reduction caused by too fast escaping of excessive hydrogen chloride from the reactor can be avoided, the consumption increase of the hydrogen chloride is avoided, and the atmospheric pollution is reduced.

The invention discloses a synthesis method of an ethyl maltol intermediate, which is characterized in that ethyl chloride is used instead of bromoethane, and the solvent for Grignard reaction is 2-methyltetrahydrofuran or a mixed solvent containing 2-methyltetrahydrofuran. The invention has the following advantages: (1) the ethyl chloride is cheaper than the bromoethane, and has higher atomic economical efficiency than bromoethane, thereby reducing the generation of three wastes and having small hazards on the environment; and (2) the 2-methyltetrahydrofuran has poor water solubility and proper boiling point, and thus, has the advantages of high use safety and high recovery rate, thereby lowering the production cost and facilitating the industrialized application.

The invention discloses a synthesis process of a sulfonic-group rhodamine compound. The process comprises the steps: mixing saccharin and a protonic acid catalyst, performing heating for a reaction soas to obtain a compound shown in a formula (I), performing a reaction between a compound shown in a formula (II) and resorcinol through heating under the action of the protonic acid catalyst so as toobtain a compound shown in a formula (III), performing a reaction between the compound of the formula (I) and the compound in the formula (III) through heating under the action of a Lewis acid catalyst under the conditions of nitrogen protection and light shielding so as to obtain the sulfonic-group rhodamine compound shown in a formula (IV). Through the synthesis process, the use of thionyl chloride in a conventional process is avoided, the operation is simplified, the production safety is improved, the pollution to the environment is little, the reaction can be carried out under normal pressure, and the reaction has a high selectivity; and the chemical structural formulas of the compounds represented separately by the formula (I), the formula (II), the formula (III) and the formula (IV)are shown.

The invention discloses a preparation method of ketoprofen. The method takes m-bromobenzoic acid and benzene as starting raw materials, and the ketoprofen is prepared through the steps of acylating, protecting a carbonyl group, taking a Grignard reagent, reacting with propylene oxide, oxidizing, de-protecting and the like. The method disclosed by the invention has the characteristics of short reaction route, easiness of obtaining the raw materials, high yield and low cost.

The invention relates to a vulcanizing activator and a preparation method thereof. The vulcanizing activator is prepared by the following steps: putting zinc oxide, benzoic acid and an alkane solventof which the boiling point is 100-150 DEG C into a reaction container in a mass ratio of 1:(0.05-0.1):(3-6), stirring for 30 minutes, adding glycerinum in a mole ratio to the zinc oxide of 1:(1.15-1.2), heating to 100-150 DEG C under stirring, enabling the components to react for 120-180 minutes, cooling, carrying out suction filtration, and drying a filter cake, thereby obtaining the vulcanizingactivator, wherein the content of zinc in the vulcanizing activator is 45-47%. The vulcanizing activator provided by the invention is capable of replacing zinc oxide in an equal mass fraction and hasa remarkable zinc reduction effect. The vulcanizing activator is simple in preparation method, convenient to operate and gentle in reaction condition.

The invention discloses waterborne polyurethane drug-loaded slow-release spray with opposite charges as well as a preparation method and application thereof. The waterborne polyurethane drug-loaded slow-release spray is composed of an anionic waterborne polyurethane drug-loaded sustained-release emulsion A entrapping hydrophobic effective components of a pesticide and a cationic waterborne polyurethane drug-loaded sustained-release emulsion B entrapping hydrophobic effective components of the pesticide. According to the invention, the deposition rate of spray droplets is effectively improved by utilizing the mutual attraction acting force and hydrogen bond interaction between anionic and cationic waterborne polyurethane particles and the reduction effect of the anionic and cationic waterborne polyurethane particles on the surface energy of the droplets; meanwhile, the effective components of the pesticide can be effectively protected, and the slow release performance, rain wash resistance and the like of the pesticide are improved; and the components of the spray are simple and environment-friendly, the spray has good dispersibility and storage stability, and a carrier is safe, non-toxic, less in environmental pollution, safe and efficient.

The invention relates to a synthetic method of p-methoxyacetophenone. Under normal temperature conditions, p-methoxyacetophenone with high yield and high purity was synthesized by Friedel-Crafts acylation reaction using anisole and acetic anhydride as raw materials, zinc chloride as catalyst and dichloromethane as solvent. The process has the advantages of simple synthesis process, low cost, mild reaction conditions, increased synthesis yield up to 90%, purity up to 99.5%, and maximal use of waste liquid to produce zinc oxide. No ecological environment risk, significant economic benefits, suitable for large-scale production.

The invention relates to an organic zinc vulcanizing activator and a preparation method thereof. The organic zinc vulcanizing activator is prepared through the following method: zinc hydroxide and benzoic acid are added into a reactor according to a molar ratio of (1.6 to 1.7) to 1, an alkane solvent with mass 1-50 times of that of the zinc hydroxide and a boiling point of 80-120 DEG C is added, reflux reaction is carried out for 30-120 min, after evaporation or cooling is conducted, suction filtration is conducted to recover the solvent, after drying is conducted, the white powdery organic zinc vulcanizing activator is obtained, and the zinc content of the organic zinc vulcanizing activator is 40-42%. The organic zinc vulcanizing activator can replace oxide zinc with an equal mass fraction, the content of zinc in a rubber product is greatly reduced, and the zinc is reduced by 50%, so that the organic zinc vulcanizing activator has the advantage of volume cost; the preparation method is simple, the reaction is mild and easy to control, the solvent can be recovered, no three waste is generated, and the preparation method of the organic zinc vulcanizing activator is a green synthesistechnology.

The invention discloses a Si (at) void (at) C embedded three-dimensional porous carbon network negative electrode material and preparation and application thereof. According to the invention, commercialized nano silicon particles are used as a research system, and the composite material with the core-shell structure Si (at) void (at) C embedded into the three-dimensional porous carbon network is controlled and synthesized by adopting a mode of combining photosensitized polymerized styrene silicon nano ion emulsion, high-temperature calcination heat treatment and hydrothermal treatment. The styrene is polymerized through ultraviolet irradiation to form polystyrene, the carbon source is formed through high-temperature pyrolysis, the synthesis process is simple and green, and the price of the styrene monomer is low. According to the invention, the introduction of a complicated template involved in the research work of the conventional core-shell structure Si (at) void (at) C and the damage of corrosive HF to the environment are avoided, the cyclic specific capacity and stability of the Si nano-powder are effectively improved, the material cost is reduced, and commercialized large-scale production is expected to be realized.

The invention relates to the technical field of organic synthesis of medical intermediates, in particular to a synthesis process of MOC-L-valine, which comprises the following steps: sequentially adding water and an acid-binding agent into a reaction kettle, starting stirring, controlling the kettle temperature to be not higher than 20 DEG C, adding L-valine, and stirring until the solid is completely dissolved; the temperature in the reaction kettle is controlled to be 5-20 DEG C, N-succinimido methyl carbonate is added in batches under stirring, the temperature is controlled, the reaction is finished when L-valine is smaller than or equal to 2%, after the reaction is finished, a solvent is added, acid adjustment, layering, washing and concentration are performed, and the target product MOC-L-valine is obtained through crystallization and separation. Compared with the prior art, the method has the characteristics of safety, environment friendliness, mild reaction conditions, easiness in operation and high purity of the prepared product, and is suitable for industrial mass production.

The invention provides a preparation method of diethyl malonate. Ethyl chloroacetate, alcohol and magnetic silica support metal complex and ammonium hydroxide are mixed to be uniform in a reaction vessel, carbon monoxide is used for replacing air in the reaction vessel for 3-6 times, the carbon monoxide is introduced, the pressure is maintained at 0.5-3 MPa, stirring is performed, a mixture inside the reaction vessel is heated to 30-70 DEG C to be subjected to a reaction for 1-6 h, diethyl malonate can be prepared, cooling and filtering are performed, and separation and rectification are performed to obtain the product diethyl malonate. The functional magnetic silica support metal complex material is adopted as the catalyst, reaction raw materials are simple, and operation is convenient; the catalyst is high in activity and small in consumption; the catalyst is good in stability and can be conveniently recycled; the preparation method is simple, the product yield is high, reaction conditions are mild, the preparation method of diethyl malonate is efficient and environmentally friendly, and large-scale industrial production is promoted.

The invention discloses a method for preparing a polyaniline material with a three-dimensional graded micro-nano structure, and belongs to the field of preparation of high polymer materials. The preparation method comprises the following steps: respectively dissolving an aniline monomer and an oxidizing agent in a strong acid solution, freezing the aniline monomer or oxidizing agent solution into ice, pouring the pre-cooled oxidizing agent or aniline monomer solution onto an ice layer, freezing the materials into ice, finally transferring the frozen ice blocks into a low-temperature environment to carry out polymerization reaction, and obtaining the three-dimensional hierarchical polyaniline materials with different morphologies. According to the method, soft and hard templates are not needed, an organic solvent is not needed, and the reaction time is shorter. The polymerization reaction is carried out in a strong acid environment, the conductive characteristic of polyaniline is ensured, and the hierarchical structure can be regulated and controlled by changing the adding sequence of reactants and the size of an ice layer or adopting a multi-layer freezing mode. The method is simple and controllable in preparation process, high in sample purity, unique in morphology and suitable for large-scale preparation, and has wide application potential in the fields of energy storage materials, adsorption materials, sensing materials, electromagnetic shielding materials, conductive functional materials and the like.

The invention provides a preparation method of an aralkyl salicylic acid derivative. The method is characterized in that styrene or a derivative thereof reacts with salicylic acid or a derivative thereof in the presence of an ionic liquid catalyst. The method overcomes the disadvantages of present aralkyl salicylic acid synthesis technologies, and is an efficient and green aralkyl salicylic acid synthesis technology. The catalyst adopted in the invention settles to the bottom of a reactor after the reaction ends, is convenient to separate, and also has the advantages of multi-time repeated use, no emission of waste acids, and environment protection benefiting in case of guaranteeing good yield.

The invention provides a continuous synthesis method of 2-chloropyrimidine-4-formic acid compounds. 2-chloropyrimidine-4-formic acid compound has the structure shown in formula I: in formula I formula I, R 1 and R 2 independently selected from hydrogen, alkoxy, aryl, benzyl or fluorine; the synthesis method comprises the following steps: S1, under the action of a non-noble metal catalyst, compound A and methyl Grignard reagent B are continuously methylated Reaction, obtain compound C; Compound A is, compound C is, R 1 and R 2 Have the same definition as above, the non-precious metal catalyst is one or more in iron salt, cobalt salt, nickel salt; S2, compound C is carried out continuous oxidation reaction under the effect of oxygen, oxidation catalyst and additive, obtains 2-chloro Pyrimidine‑4‑carboxylic acid compounds. Synthesizing 2-chloropyrimidine-4-carboxylic acid compounds by adopting the process provided by the invention can take into account aspects such as cost, yield, and environmental protection.

The invention relates to a method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol. 2-methyl-3-butene-2-alcohol takes Saucy-Marbet reaction with 2-alkoxylpropylene in the near critical state to obtain methyl heptenone. The synthesis method has the advantages that the use of catalysts is not needed; the selectivity of the product of methyl heptenone can be improved.

The invention relates to a molybdenum disulfide catalyst with adjustable phase composition and large interlayer spacing, and a preparation method and application thereof, the molybdenum disulfide catalyst prepared by combining phase engineering and intercalation ion introduction strain effect and using an ethanol preferential reduction strategy has high 1T phase content (73.5%) and additional ammonium ion intercalation, ammonium ion intercalation, and the molybdenum disulfide catalyst can be used for preparing a molybdenum disulfide catalyst with adjustable phase composition and large interlayer spacing. The molybdenum disulfide catalyst has a large interlayer spacing (0.95 nm), more active sites and a faster charge transfer rate. In addition, the insertion of ammonium ions causes local tensile strain of a basal plane, so that hydrogen adsorption of sulfur atoms on the surface of the catalyst is further optimized. Finally, the prepared molybdenum disulfide catalyst has lower overpotential at 10mA cm <-2 > and 100mA cm <-2 > (170mV and 211mV), excellent hydrogen evolution reaction (HER) performance is realized, and the molybdenum disulfide catalyst exceeds most reported molybdenum disulfide-based non-noble metal electrocatalysts.

The invention relates to a synthesis method of 3,4,5-trimethoxybenzoic acid. Under the condition of 110 to 120 DEG C, N, N-dimethylformamide is used as a solvent; under the catalysis condition of potassium carbonate, gallic acid and dimethyl carbonate are added in one step; the 3,4,5-trimethoxybenzoic acid is synthesized through methylation. The process has the advantages that the synthesis process is simple; the cost is low; the yield reaches 95 percent or higher; the product purity reaches 100.0 percent, and the like. The green methylation reagent of dimethyl carbonate is used for replacing highly toxic dimethyl sulfate; the high risk factor of the process is overcome; the process safety is improved to the maximum degree; the economic benefits are obvious; the method is suitable for large-scale industrial production.

The invention discloses a preparation method of 3-methyl flavone-8-carboxylic acid, which comprises the following steps of: rearranging methyl salicylate serving as an initial raw material under the action of Lewis acid to generate propionyl methyl salicylate, and finally cyclizing and hydrolyzing to generate the 3-methyl flavone-8-carboxylic acid. According to the technology, methyl salicylate is adopted for acylation rearrangement reaction, generation of dimer impurities and isomer impurities in the rearrangement process is reduced, the purity is 99.9% or above, and the preparation method is short in technological process, small in production risk, low in technological cost and suitable for large-scale preparation of 3-methyl flavone-8 carboxylic acid.

The invention discloses a method for laser synthesis of a magnetic graphene -PEG-gamma-Fe2O3 compound. The method comprises the following steps: (1) by taking a blocky iron target as a raw material, polishing the surface of the target, performing ultrasonic washing with diluted hydrochloric acid to remove an oxidation layer of the target, further performing ultrasonic washing with deionized waterto remove residual diluted hydrochloric acid, and drying for later use; (2) putting the dried target into a flask, and adding a graphene-PEG (Polyethylene Glycol) solution; (3) powering on a nanosecond laser emitter, and ablating the iron target with focused light of a wavelength of 1064nm for 30-40 minutes; (4) after the laser action, taking out the solution, and performing centrifugal drying onthe solution, thereby obtaining a compound powder product. By adopting the method, the magnetic graphene -PEG-gamma-Fe2O3 compound with in-situ combination can be prepared rapidly at one step, in theprocess of laser synthesis of the compound, only the iron target, the deionized water and the graphene-PEG solution with cell compatibility are used, and no other organic reagent or complexing agent is used, so that the product is free of other toxic impurity, and the synthesis process is green and simple.

The invention relates to an oligopeptide / silicon dioxide / hyaluronic acid composite hydrogel preparation method and belongs to the technical field of medical hydrogel materials. The oligopeptide / silicon dioxide / hyaluronic acid composite hydrogel has the characteristics of improving the strength of hydrogel dressings, having an anti-bacteria function, improving wound healing and being easy to combine with functional molecules. The preparation method comprises the steps of firstly self assembling amphipathic oligopeptide in water solution to form a stable self assembly; mixing silicon dioxide precursor with assembled oligopeptide solution to react in the appropriate condtion to obtain oligopeptide / silicon dioxide hydrogel; compositing the oligopeptide / silicon dioxide hydrogel with hyaluronic acid solution of the certain concentration to obtain the oligopeptide / silicon dioxide / hyaluronic acid composite hydrogel. The preparation method is used for preparing organic / inorganic composite hydrogel with higher mechanical strength, and the organic / inorganic composite hydrogel can be used as a three-dimensional support material of the medical dressings.

The invention discloses a process for synthesizing ethyl chloride. In a closed reactor, an ethyl chloride product can be obtained from ethanol and hydrogen chloride gas under the catalytic effect of AlCl3-ZnCl2 double component catalyst by gradually heating for reaction, releasing step by step and recovering. The high activity of AlCl3-ZnCl2 double component catalyst is used in the method, reaction temperature and by-product diethyl ether are reduced, and the yield of the ethyl chloride is increased to above 95%; by the use of the hydrogen chloride for replacement of industrial hydrochloric acid, mother liquor and distillate are directly continuously applied, energy consumption for distillation distillate recovery and hydrogen chloride loss are effectively reduced, environment pollution caused by production of a lot of high salt wastewater and organic waste acid can be avoided; in addition, by use of a closed staged heating reaction way, a catalytic substitution reaction is performed in a liquid phase system, substrate contact reaction time is increased, ethanol conversion rate reduction caused by too fast escaping of excessive hydrogen chloride from the reactor can be avoided, the consumption increase of the hydrogen chloride is avoided, and the atmospheric pollution is reduced.

A water-based polyurethane drug-loaded slow-release spray with opposite charges, its preparation method and application. It consists of anionic water-based polyurethane drug-loaded slow-release emulsion A with hydrophobic pesticide active ingredients and cationic water-based polyurethane drug-loaded slow-release emulsion B with hydrophobic pesticide active ingredients. The present invention utilizes the mutual attractive force between the anionic and cationic waterborne polyurethane particles, the hydrogen bonding effect and the reducing effect on the surface energy of the droplet to effectively improve the deposition rate of the sprayed droplet, and at the same time, effectively protect the active ingredients of the pesticide, Improve pesticide slow-release performance, rain erosion resistance, etc., and have simple components, good dispersion and storage stability, safe and non-toxic carrier, less environmental pollution, safe and efficient.

The invention discloses a preparation method of a praseodymium oxide particle modified lithium ion battery positive electrode material, and belongs to the technical field of lithium ion battery electrode materials. The method comprises the following steps: dissolving praseodymium nitrate in an aqueous solution containing the lithium ion positive electrode material, then adjusting the pH value of the mixed solution and the cross-linking coupling effect of the solution to enable the praseodymium nitrate to generate praseodymium hydroxide, precipitating the praseodymium hydroxide on the surface of the positive electrode material, and then carrying out centrifugal cleaning and annealing treatment to obtain the praseodymium oxide particle modified lithium ion battery positive electrode material. The invention provides a synthesis strategy for improving the conductivity and the material interface compatibility of the lithium ion battery material and relieving the transition metal dissolution of the active material by using the metal oxide, and the synthesized praseodymium oxide modified LiCoO2 positive electrode material is uniformly dispersed; the scheme is simple and efficient, the high-temperature and high-pressure electrochemical performance of the material can be remarkably improved, and certain guiding significance is achieved for commercial modification production of the positive electrode material.

The invention relates to a method for synthesizing a water-soluble conductive polymer by using a nano black selenium peroxide mimic enzyme as a catalyst, belonging to the technical field of preparation and application of nano materials. The nano black selenium peroxide mimic enzyme is nano black simple substance selenium prepared from selenium dioxide under solvothermal conditions by using concentrated sulfuric acid as a reducer. The substance has similar catalytic activity to peroxidase, and can be used for catalyzing synthesis of the water-soluble conductive high-molecular polymer. According to the synthesis method, a polymer monomer is used as a raw material, the nano black selenium is used as the catalyst, water is used as a reaction medium, and ambient oxygen is used as an oxidizer to obtain the water-soluble conductive polymer in a buffer solution with the pH value of 2.2-4.2. The method has the advantages of green synthesis technique and no pollution, and overcomes the defects in the traditional chemical process which needs non-environment-friendly persulfate oxidizers and organic solvents.