52results about How to "Meet the development requirements of green chemistry" patented technology

The invention belongs to the technical field of green organic synthesis chemistry, and particularly relates to a method using a choline type deep-eutectic solvent to catalyze to synthesize aspirin. The method comprises the following steps of adding the choline type deep-eutectic solvent, salicylic acid and acetic anhydride into a reaction container; heating to react for 15 to 40min at the temperature of 70 to 80 DEG C; purifying a crude product after reaction, so as to obtain the aspirin. The method using the choline type deep-eutectic solvent to catalyze to the synthesize aspirin has the advantages that the operation is simple, the reaction condition is mild, the side effect is small, and the environment-friendly effect is realized; when the deep-eutectic solvent is prepared, the utilization rate of atoms is 100%; the purifying of the deep-eutectic solvent is not needed, the deep-eutectic solvent can be recycled, the green chemical development requirement is met, and the wide industrial production application prospect is realized.

The invention relates to a vanadyl phosphate catalyst as well as a preparation method and application thereof. The method comprises the following steps: 1) mixing a vanadium source, a choline chloride-organic carboxylic acid eutectic solvent and an alcohol, and performing a reaction, wherein the alcohol is benzyl alcohol, or a mixture of a C3-C8 monohydric alcohol and the benzyl alcohol; 2) mixingthe obtained reaction product with a phosphorus source, raising temperature until the temperature is higher than a melting point of the eutectic solvent, and continuing a reaction to obtain a vanadylphosphate precursor; and 3) performing calcination to obtain the vanadyl phosphate catalyst. The method provided by the invention uses the green cheap eutectic solvent to intensively prepare the vanadyl phosphate catalyst, and overcomes the disadvantages that a vanadyl phosphate catalyst relies on precious metals to improve performance, secondary pollution is generated, costs are high and a preparation process is complicated; and the vanadyl phosphate catalyst provided by the invention improves the difficult problems of a low yield and poor selectivity when being used for catalyzing a reaction of preparing maleic anhydride by selective oxidation of n-butane, and overcomes the disadvantages of high costs and large pollution in a conventional catalyst improving method.

The invention relates to a VOPO4 catalyst as well as a preparation method and an application thereof. The method comprises the steps as follows: 1) a vanadium source, a deep-eutectic solvent and alcohol are mixed to react; 2) an obtained product is mixed with a phosphorus source, the mixture is heated to the temperature higher than the melting point of the deep-eutectic solvent to react continuously, a precursor is obtained and roasted, and the VOPO4 catalyst is obtained. The deep-eutectic solvent is any one of or a combination of at least two of urea-polyethylene glycol, urea-metal chloride,urea-choline chloride or thiourea-polyethylene glycol; the alcohol is benzyl alcohol or a mixture of C3-C8 monohydric alcohol and benzyl alcohol. The method overcomes the defects that VOPO4 catalystsdepend on precious metals to improve the performance of the VOPO4 catalysts, cause secondary pollution, are high in cost and complex to prepare and the like. The problems of low yield, poor selectivity and the like are solved and the defects of high costs and severe pollution in traditional catalyst improvement methods are overcome when the VOPO4 catalysts are applied to catalyze a reaction for preparing maleic anhydride through n-butane selective oxidation.

The invention discloses flame-retardant furan epoxy resin and a preparation method thereof, and belongs to the technical field of polymer compounds. The flame-retardant furan epoxy resin is prepared from furan epoxy resin monomers which are prepared through derivation of hydroxymethylfurfural. The preparation method comprises the specific steps: performing melting and uniform mixing on the furan epoxy resin monomers of different structures and curing agents of different types, and then performing injection molding, heating and solidification so as to obtain the flame-retardant furan epoxy resin with superior performance. A bulk solidification method is adopted directly, the operation flow is simple, the curing time is short, and the obtained bio-based epoxy resin polymer material has excellent performance.

The invention provides a process for preparing Guerbet alcohol. The process comprises the following steps: (a) weighing 100-200g of a fatty alcohol, a solid base catalyst and a nickel-based catalyst, adding into a three-necked flask which is provided with a thermometer, a water distributor, a reflux condensing tube, a nitrogen introducing tube and a magnet stirrer, introducing nitrogen into the three-necked flask continuously, increasing temperature to 200 DEG C rapidly, carrying out reaction for 1.5 hours, decreasing temperature after reaction, filtering a product of reaction at room temperature, separating the catalysts from the product of reaction, and distilling an obtained filtrate by reducing pressure to obtain a product, wherein the weight of the solid base catalyst is 5-15% of that of the fatty alcohol, and the weight of the nickel-based catalyst is 0.5-5.5% of that of the fatty alcohol; and (b) adding the product obtained in the step (a) and a nickel-based catalyst into a sealed reactor, replacing air in the reactor with nitrogen, controlling the pressure at 0.1-2.0MPa and the temperature at 120-280 DEG C with hydrogen, carrying out reaction under pressure for 1-3 hours, cooling a product of reaction to normal temperature, filtering to obtain a high-purity product, and measuring the iodine number, wherein the weight of the nickel-based catalyst is 1-5% of that of the product obtained in the step (a). The process provided by the invention has the advantages of strong operability, simple post-treatment process and significant improvement of product purity and is suitable for industrial production.

The invention relates to a novel method for preparing a porous crosslinked chitosan microsphere, and in particular relates to a method for preparing a crosslinked chitosan microsphere by using 1,2-cyclohexanediol diglycidyl ether as a crosslinking agent. According to the novel method, commercially available chitosan, 1,2-cyclohexanediol diglycidyl ether and chlorinated paraffin are used as raw materials, and the porous crosslinked chitosan microsphere is prepared by dissolution, dispersion into spheres, hole preparation, crosslinking and drying. The method has the characteristics of mild reaction conditions, simple preparation steps, high comprehensive resource utilization rate, no harmful substances and the like. The crosslinked chitosan microsphere prepared by using the method has the characteristics of capability of biodegradation, good acid-alkali resistance, good adsorption effect on acid ions and proteins, strong load capacity on heavy metal ions and the like, and can be applied to the field of food, medicine, chemical industry and the like.

The invention relates to a vanadyl phosphate catalyst, an intensified preparation method by low congruent melting solvent, and application of the vanadyl phosphate catalyst. The method comprises the following steps: 1) mixing a vanadium source, low congruent melting solvent, benzyl alcohol and C3-C8 monohydric alcohol to obtain mixed materials, and reacting, wherein the low congruent melting solvent is formed by choline chloride and organic polyhydric alcohols; 2) mixing a reaction product obtained in 1) with a phosphorus source, raising the temperature to 100-200DEG C, and continuously reacting to obtain a vanadyl phosphate precursor; 3) roasting to obtain the vanadyl phosphate catalyst. The method is characterized in that green and low-price low congruent melting solvent is subjected tointensified preparation to obtain the vanadyl phosphate catalyst, the defects of secondary pollution, high cost, complex preparation process and the like since the performance of the vanadyl phosphatecatalyst is improved on the basis of noble metal are overcome. When the vanadyl phosphate catalyst is used for catalytic normal butane selectivity oxidation maleic anhydride reaction, the difficulties including low yield, poor selectivity and the like, are solved, and defects of high cost and serious pollution in a traditional catalyst improvement method are overcome.

The invention relates to a biomass reinforced graphite phase carbon nitride catalyst preparation method, which comprises: 1) adding a precursor and biomass into water according to a certain ratio, magnetically stirring, and heating to 80 DEG C until moisture is evaporated to achieve a dry state to obtain a mixture; and (2) putting the mixture obtained in the step (1) into a quartz crucible, sealing with aluminum-foil paper, heating to 500-800 DEG C in a nitrogen atmosphere, and continuously reacting for 2-24 h to obtain the graphite-phase carbon nitride catalyst. According to the invention, the graphite phase carbon nitride catalyst is prepared by using the environmentally-friendly and cheap renewable biomass raw material, so that the disadvantages that the performance of the graphite-phase carbon nitride is improved through precious metal deposition, semiconductor compounding and ion doping, the cost is high, the reparation process is complex, large-scale preparation is difficult andthe like are overcome; and with the application of the graphite-phase carbon nitride in photocatalytic degradation of organic pollutants, the problems of low degradation rate, low degradation speed and the like are solved, and the defects of high cost and complex process in the traditional catalyst improvement method are overcome.

The invention discloses an oxidation cleaning disinfector which comprises the following raw materials in parts by weight: 1-3 parts of peracetic acid, 8-24 parts of hydrogen peroxide, 7-21 parts of acetic acid, 2-8 parts of iminodisuccinic acid, 1-3 parts of sodium dodecyl diphenyl ether disulfonate and 60-90 parts of deionized water. The oxidation cleaning disinfector is easily soluble in water,low in foaming, convenient to use, quick and thorough in sterilization, high in cleaning efficiency and good in disinfection effect; no residual toxicity is available on a disinfected article; a decomposition product is innocuous to a human body; and the disinfector has high cost performance, is convenient to popularize and apply and can achieve good economic benefits.

The invention relates to a method for preparing a rare earth-based hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst. The method comprises the following steps: preparing a vanadium-phosphorus-oxygen precursor; preparing a rare earth-based hydrotalcite auxiliary agent by dissolving a water-soluble inorganic zinc source, an inorganic magnesium source, an inorganic aluminum source and rare earth salt into water, adding an alkali source, carrying out heating to 65-200 DEG C for a reaction, conducting cooling, then performing aging for 6-12 hours, conducting filtering, washing and drying, and carrying out roasting at 350-550 DEG C, wherein a ratio of the total molar amount of zinc and magnesium in the inorganic zinc source, the inorganic magnesium source, the inorganic aluminum source and the rare earth salt to the total molar amount of aluminum and rare earth elements is (1-4): 1; and mixing the rare earth-based hydrotalcite auxiliary agent with the vanadium-phosphorus-oxygen precursor according to a mass ratio of (1-10): 100, carrying out heating to 300-500 DEG C, and performing roasting to obtain the vanadium phosphorus oxide catalyst.

A preparation method suitable for large-area production of a low-cost and environment-friendly tungsten oxide electrochromic film comprises the following steps: sequentially putting FTO glass into anFTO cleaning solution, deionized water and an ethanol solution, carrying out ultrasonic cleaning for 15 min, then taking the FTO glass out, and drying in the air; dissolving tungsten acid in hydrogenperoxide with a certain mass fraction, stirring uniformly, and adding PVP powder, to obtain a precursor; 1) carrying out spin coating on the FTO by a precursor solution, and drying at the temperatureof 100-280 DEG C to form a film; 2) carrying out blade coating on the FTO by the precursor solution, and drying to form a film in an environment of 60-180 DEG C; placing the prepared film on a heatingplate, carbonizing, to obtain a black film sample, then carrying out heat treatment in a muffle furnace, carrying out heat preservation for 2-4 h, and thus obtaining a porous tungsten oxide film. Theutilization rate of raw materials for preparing the tungsten oxide electrochromic film is increased, and the process is green and environmentally friendly and suitable for large-area production.

The invention discloses a method for coupling preparing ethylene glycol by photocatalyzing formaldehyde and methanol. The methanol and the formaldehyde have photocatalytic reaction in the presence ofa light catalyst to prepare the ethylene glycol. For a photocatalytic coupling system, the generation rate of the ethylene glycol can be apparently improved in an independent methanol or formaldehydesystem, the method is mild in reaction condition, the process flow is simple, the cost is low, the atom economical performance is high, and the green and chemical development requirement can be met.

The invention discloses a bio-based flame-retardant magnolol epoxy monomer, a preparation method thereof and application of the monomer in flame-retardant epoxy resin. The preparation method of the bio-based flame-retardant magnolol epoxy monomer comprises the following steps: (1) stirring a mixed solution of magnolol, sodium hydride and tetrahydrofuran under the protection of inert gas, and reacting an obtained mixture with diphenyl phosphinyl chloride to obtain an intermediate as shown in a formula II; and (2) reacting the solution of the intermediate as shown in the formula II with m-chloroperoxybenzoic acid to obtain the bio-based flame-retardant magnolol epoxy monomer as shown in the formula I. The bio-based flame-retardant magnolol epoxy monomer as shown in the formula I is prepared for the first time, is a novel bio-based phosphorus-containing epoxy structure, is also a good flame-retardant aid, is low in use amount, has excellent compatibility in epoxy resin, is free of phosphorus removal after participating in curing, is high in safety and has great market application value.

The invention discloses a chitosan-based multifunctional macromolecular rubber anti-aging agent, and a preparation method and application thereof. The chitosan-based multifunctional macromolecular rubber anti-aging agent is prepared by carrying out chemical reaction on active amino groups on chitosan and a carboxyl-containing phenolic anti-aging agent in the presence of a solvent, a dehydrating agent and a catalyst. The chitosan-based multifunctional macromolecular rubber anti-aging agent provided by the invention is environment-friendly and not easy to migrate, not only can remarkably improve the thermo-oxidative aging resistance of a rubber material, but also has excellent extraction resistance, can play a lasting thermo-oxidative aging resistance role on the rubber material, can also promote rubber vulcanization and remarkably reduce the positive vulcanization time TC90, and reduces the consumption of a vulcanization accelerator.

The invention relates to a preparation method of a hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst with assistance of hydrotalcite. The preparation method comprises the following steps: preparing a vanadium-phosphorus-oxygen precursor: mixing a vanadium source, benzyl alcohol and C3-C8 monohydric alcohol to obtain a mixture, adding a phosphorus source, carrying out heating to 100-200 DEGC, continuing reacting, and filtering and drying a product to obtain the vanadium-phosphorus-oxygen precursor; preparation of a hydrotalcite additive: dissolving a water-soluble inorganic zinc source, an inorganic magnesium source and an inorganic aluminum source in water, adding an alkali source, carrying out heating to 65-200 DEG C for a reaction, conducting cooling, then performing aging for 6-12 hours, conducting filtering, washing and drying, and carrying out roasting at 350-550 DEG C to obtain the hydrotalcite additive; and preparation of the hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst: mixing the hydrotalcite additive with the vanadium-phosphorus-oxygen precursor according to a mass ratio of (1-10): 100, carrying out heating to 300-500 DEG C, and conducting roasting to obtain the hydrotalcite-assisted vanadium-phosphorus-oxygen catalyst.

The invention relates to a phosphorus-silicon-nitrogen ternary synergistic flame retardant and a preparation method thereof, a traditional preparation method of a multi-element synergistic flame retardant has the problems that steps are tedious, a large number of solvents and catalysts are possibly used, and large-scale industrial production is difficult, most thermosetting resins are poor in flame-retardant effect, and if the flame retardance of the thermosetting resins needs to be improved, a large number of flame retardants need to be added to improve the flame retardance of the thermosetting resins, according to the preparation method, the novel phosphorus-silicon-nitrogen ternary synergistic high-efficiency flame retardant is prepared from amino-containing alkoxysilane, trialkoxyphosphate and diethanolamine (and derivatives thereof) by a "one-pot method" under the conditions of no solvent and no catalyst, and the phosphorus-silicon-nitrogen ternary synergistic flame retardant meets the development requirements of green chemistry. The preparation method has the beneficial effects that no solvent or catalyst is used in the reaction process, the reaction time is short, the operation is easy, the cost is low, the used equipment is simple, and the practicability is strong.

The invention discloses a preparation method and application of an anti-ultraviolet dendritic silicon dioxide nanomaterial. The dendritic silicon dioxide nanomaterial loaded with an organic ultraviolet (UV) absorbing group is formed in situ through a simple liquid phase method, and the prepared anti-ultraviolet dendritic silicon dioxide nanomaterial has dual effects of UV shielding and absorption, is good in anti-ultraviolet aging effect, does not generate side reactions for accelerating polymer degradation, is an efficient, multifunctional and environment-friendly plastic additive, has important application prospects in the plastic industry, meets the development requirements of green chemistry, and is beneficial for environmental protection.

The invention discloses a preparation method of petaloid sodalite at room temperature and belongs to the technical field of zeolite materials. The method comprises the following steps: weighing sodium hydroxide and an aluminum source, adding deionized water, and heating and stirring the mixture till the raw materials are fully dissolved to prepare a solution A; weighing a silicon source, adding deionized water, and heating and stirring the mixture till the raw materials are fully dissolved to prepare a solution B; uniformly mixing the solutions A and B; crystallizing the mixture at room temperature; and after crystallization, washing the mixture till the pH of the washing solution is 8-9, and drying the filter cake at 80-120 DEG C for 12-36h to obtain sodalite. The preparation method disclosed by the invention is performed at room temperature, and is mild in condition, free of organic additives and pollution-free; the preparation method is simple in synthesizing step, short in consumed time and low in cost; and the product is high in crystallizing property and high in purity, and the synthesized sodalite has a shape of sodalite, so that the adsorptive action thereof is facilitated, and the sodalite is suitable for scaled production.

The invention discloses a P / N / Si multi-element synergistic integrated nano flame retardant as well as a preparation method and application thereof. The flame retardant comprises a transition metal organic framework, and a phytic acid coating layer and a SiO2 coating layer which sequentially coat the transition metal organic framework. The preparation method comprises the following steps: preparing the transition metal organic framework MOF; dropwise adding a certain amount of phytic acid into a MOF uniform suspension, carrying out stirring reaction at room temperature, and after the reaction is finished, centrifuging, washing and drying to obtain MOF@PA; and growing SiO2 on the surface of the MOF@ PA by taking the MOF@ PA as a core and adopting a sol-gel method. The flame retardant combines excellent characteristics of flame-retardant elements such as P, N, Si, transition metal and the like, not only can play a synergistic role to improve the flame-retardant effect and effectively inhibit release of toxic smoke, but also can be widely applied to high polymer materials such as polyurethane, epoxy resin, polypropylene and the like to improve the flame-retardant property of the high polymer materials and reduce the possibility of casualties.

The invention relates to a phosphorus-silicon-nitrogen ternary synergistic flame retardant and a preparation method thereof. Compared with the traditional multi-element synergistic flame retardant preparation method, the steps are cumbersome, a large amount of solvents and catalysts may be used, and it is difficult for large-scale industrial production; and most The flame retardant effect of thermosetting resin is relatively poor. To improve its flame retardancy, it is necessary to add a large amount of flame retardant to improve its flame retardant performance. The present invention utilizes amino-containing alkoxysilane, trialkoxy phosphate and diethanolamine (and its derivatives), a new type of phosphorus-silicon-nitrogen synergistic high-efficiency flame retardant is prepared under the condition of no solvent and no catalyst by "one-pot method", and it meets the development requirements of green chemistry. The beneficial effect of the invention is that no solvent and catalyst are used in the reaction process, the reaction time is short, the operation is easy, the cost is low, the equipment used is simple, and the practicability is strong.

The invention relates to a cyclic phosphamide derivative with a biaryl skeleton and a synthesis method and application thereof, belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing the cyclic phosphamide derivative with the biaryl skeleton by utilizing an electrochemical catalysis intramolecular phosphine amination reaction. The method has good applicability to mono-substituted or di-substituted electron withdrawing groups and electron donating groups on ortho, meta and para positions on a ring A and a ring B in a biaryl phosphamide compound structure, and a substituent R can be an electron donating alkyl group or an electron withdrawing group, so that the method has small influence on the yield of the corresponding product. Compared with the prior art, on one hand, the method has wide substrate universality, good reaction selectivity and high molecular conversion rate and yield; on the other hand, reaction conditions are mild, a catalytic mode is green and efficient, and operation steps are simple. The cyclic phosphamide derivative with the biaryl skeleton prepared by the method can be used for preparing various organic PN ligands and organic photoelectric materials through chemical conversion.

The invention provides a method for high sensitivity detection of mercury ions by using nitrogen-sulfur doped carbon quantum dots. The method includes the following steps: a carbon source, a nitrogensource and a sulfur source are mixed, a mode of liquid phase mixing is used to uniformly mix the three sources, a microwave preliminary reaction is carried out to realize initial doping of hetero atoms, and then a one-step reaction of hydrothermal microwave is carried out to directly prepare the nitrogen-sulfur doped carbon quantum dots. The carbon quantum dots are used for detection of mercury ions and show high sensitivity and an extremely low detection line. The preparation method does not use any toxic and harmful substances and is a completely green synthetic route.

The invention relates to a vanadyl phosphate catalyst, its preparation method and application. The method comprises: 1) mixing and reacting a vanadium source, a deep eutectic solvent and an alcohol; 2) mixing the obtained product with a phosphorus source, raising the temperature to a temperature higher than the melting point of the deep eutectic solvent, continuing the reaction to obtain a precursor, and roasting , to obtain the vanadyl phosphate catalyst; the deep eutectic solvent is any one or at least two of urea-polyethylene glycol, urea-metal chloride, urea-choline chloride, or thiourea-polyethylene glycol A combination of species; the alcohol is benzyl alcohol, or C 3 ~C 8 A mixture of monohydric alcohols and benzyl alcohol. The method overcomes the shortcomings of the vanadyl phosphate catalyst relying on noble metals to improve its performance, causing secondary pollution, high cost, and complicated preparation process. When the vanadyl phosphate catalyst is used to catalyze the selective oxidation of n-butane to maleic anhydride, it overcomes the problems of low yield and poor selectivity, and overcomes the shortcomings of high cost and large pollution in traditional catalyst improvement methods.