108 results about "Synthesis Period" patented technology

The invention relates to a preparation method of VO2(M) nano powder and film through spray pyrolysis. The preparation method comprises the following steps: adding ammonium meta-vanadate into a glycol solvent, heating and stirring to form a transparent and uniform precursor solution with a concentration of 0.02 to 1 mol/L finally, then atomizing the precursor into droplets by an atomizer, spraying the droplets to a heated substrate by carrier gas, decomposing precursors on the substrate, after the products deposit for a while, and collecting the products namely VO2(M) nano powder or film; wherein a doping agent is added during the preparation process of precursor so as to reduce the phase change temperature of vanadium dioxide to room temperature. The operation of the preparation method is simple, the cost is largely reduced, the synthesis period of vanadium dioxide (M) is effectively shortened, and the preparation method can be applied to large-scale industrial production.

The invention relates to a method for preparing carbonyl iron powder in a high-pressure circulating way, comprising the following steps of: carrying out synthetic reaction between a porous sponge iron material and carbon monoxide to generate pentacarbonyl iron and synthesized residue, enabling the synthesized residue to enter a recycling flow, freezing the pentacarbonyl iron, freezing and fine-filtering the separated reaction gas by a water freezing machine, conveying into a synthesis kettle by a circulation compressor and circulating, filtering and purifying the pentacarbonyl iron, and decomposing the pentacarbonyl iron into micrometer-grade carbonyl iron powder by vaporization and thermal decomposition. Compared with the general process, the high-pressure air circulation and synthesis technology improves the carbonylation ratio, greatly reduces the carbon monoxide consumption per ton of the carbonyl iron powder, shortens the synthesis period to 3 days, improves the productivity by 55 percent, improves the working environment and the labor intensity of personnel simultaneously and reduces the environment pollution.

The present invention provides a method for preparing a submicron all-silicon DD3R molecular sieve. The method comprises the following steps: 1) mixing a silicon source, amantadine, water and an auxiliary template agent to obtain crystal synthesis mother liquor and stirring and ageing the crystal synthesis mother liquor; and 2) adding 0.01-5% by mass of seed crystals into the crystal synthesis mother liquor and heating the crystal synthesis mother liquor with the seed crystals at 120-220 DEG C, wherein the auxiliary template agent is one or more selected from the group consisting of tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetraethyl ammonium fluoride, tetraethyl ammonium bromide, tetrabutyl ammonium hydroxide and tetrabutyl ammonium bromide. According to the present invention, by adopting the method of mixing the template agent and adding the seed crystals, an induction period in a crystallization process is greatly shortened, a crystallization rate is increased and a synthesis period of the DD3R molecular sieve is shortened, so that the synthesis period of the submicron all-silicon DD3R molecular sieve is shortened from 25 days in the prior art to 3 hours; and the prepared DD3R molecular sieve is uniform in crystal size, has a particle size less than 1 micrometer, has a yield rate close to 100%, and has great application potential in adsorption and separation fields.

The invention provides a nitrogen doped graphene quantum dot/mesoporous titanium dioxide photocatalyst and a preparation method thereof. According to the invention, nitrogen doped graphene quantum dots are distributed to the volume surface and the interior of titanium dioxide solid microspheres; the nitrogen doped graphene quantum dot/mesoporous titanium dioxide is of a spherical shape and has a diameter of 400 to 600 nm and a mesoporous structure; and the titanium dioxide is pure anatase type titanium dioxide. The preparation method provided by the invention comprises the following steps: synthesis of the nitrogen doped graphene quantum dots, and in-situ synthesis of the graphene quantum dot/mesoporous titanium dioxide by adopting a sol-gel method. According to the invention, the graphene quantum dots interact with a structure directing agent due to static electricity, and are gradually distributed to the volume surface and the interior of titanium dioxide microspheres with the structure directing agent in the hydrolysis process of a titanium source; and the graphene quantum dots are used as electron acceptors and transfersomes of the titanium dioxide, thereby enlarging the separation time of electrons and holes, and achieving the purpose of strengthening the photocatalytic performance of a material. The method provided by the invention has the advantages of simple operation, short synthesis period and easy control; and the hydrogen production rate of the material can reach 0.5 mmol<h-1>.

The invention discloses a ferrocene triazole ionic-type nitrogen-enriched energetic metal complex and a preparation method thereof. The ferrocene triazole ionic-type nitrogen-enriched energetic metalcomplex adopts a structural formula as follows: FORMULA, wherein M represents Cu<2+> or Zn<2+>, L is 1, 1, 3, 3-tetracyanoacrylate ion, picrate ion or trinitroresorcinate ion, and n is 1 or 2. The ferrocene triazole ionic-type nitrogen-enriched energetic metal complex is high in nitrogen content; through introduction of carbon-nitrogen double bonds, the conjugacy of a whole system is increased; the ferrocene triazole ionic-type nitrogen-enriched energetic metal complex is unlikely to volatilize under a natural condition, is good in thermal stability, has relatively high formation heat and combustion heat and extremely low vapor pressure and volatility, and has relatively good combustion catalyzing effect on main components, namely ammonium perchlorate and hexogen, of a composite solid propellant. The preparation method of the ferrocene triazole ionic-type nitrogen-enriched energetic metal complex preparation method is simple, the cost is low, the yield is high, and the defects that theexisting ferrocene-type combustion catalyst synthesizing process is cumbersome, the cost is high, the synthesis period is long and the like are overcome.

This invention relates to reaction system and synthesis method for continuously producing chloropropyl triethoxy silane by esterification reaction. This invention solves the problems of long synthesis period, high energy consumption, high production cost and high HCl content in the crude product faced by the present chloropropyl triethoxy silane synthesis reaction. The liquid outlet at the bottom of the ethanol storage tank of the reaction system is through connected with the liquid inlet of the second heat exchanger. The gas outlet of the second heat exchanger is through connected with the gas inlet at the lower part of the stripping column. The gas outlet at the top of the stripping column is through connected with the gas inlet of the third heat exchanger. The gas outlet of the third heat exchanger is through connected with the gas inlet of the first ceramic suction pump. The liquid out of the third heat exchanger is through connected with the liquid inlet of the esterification reactor. This invention has such advantages as simple apparatus structure, easy operation and low space occupation.

The invention discloses a preparation method of a porous carbon coated MnO nanocrystalline composite material. The method comprises the following steps: (a1) in a temperature environment of 20-25DEG C, dripping mixed solution of ethyl alcohol of trimesic acid and water into a mixed solution of manganese acetate tetrahydrate, ethyl alcohol of polyvinylpyrrolidone and water, stirring evenly, standing for 20-30h, and carrying out centrifugalization to obtain a precursor Mn-BTC micro-sphere; (a2) putting the precursor Mn-BTC micro-sphere into a tube-type crucible furnace, raising the temperature to 500-700DEG C at a rate of 7-13DEG C/min in inert gas, then, calcining at the temperature for 1-3h, and naturally cooling to 20-25DEG C to obtain the porous carbon coated MnO nanocrystalline composite material. The preparation method has the advantages that a complex is directly calcined in nitrogen to prepare the carbon coated MnO composite material, and technical steps for preparing the carbon coated MnO composite material are effectively simplified. In addition, the preparation method has the advantages of simple and efficient preparation technology, safety, easiness in realization and short synthesis period, and is hopefully subjected to popularization and industrial production.

The invention discloses AgInSe2 nanocrystalline and a preparation method thereof. The preparation method comprises the following steps: mixing and uniformly stirring silver nitrate, indium chloride and/or indium chloride tetrahydrate, selenium dioxide, polyvinylpyrrolidone and dimethyl formamide to obtain a precursor liquid; allowing the precursor liquid to have a constant-temperature reaction in a high-pressure kettle at the temperature of 160-220 DEG C for 3-20 hours to obtain the AgInSe2 nanocrystalline, wherein the AgInSe2 nanocrystalline is a metastable orthorhombic crystal system of which the space group is Pna21 and is soluble in water. The preparation method disclosed by the invention adopts simple and cheap raw materials and is simple in process, short in synthesis period, good in repeatability and environment-friendly; and the prepared AgInSe2 nanocrystalline can be well dispersed in a water phase and has application advantages in the fields such as biomedicines and water-phase optical catalysis.

The invention belongs to the field of benzoxazine resin in polymer synthetic materials and discloses side-chain phthalonitrile modified benzoxazine resin, a preparation method and an application. The resin has a general structural formula shown in a formula I, wherein n is an integer larger than or equal to 1. By means of the characteristic of strong molecular structure design of a benzoxazine monomer, a polymerizable phthalonitrile group is introduced into an aromatic diamine compound through a conventional chemical reaction, then the aromatic diamine compound carrying the phthalonitrile group, paraformaldehyde and bisphenol A have condensation polymerization, and the side-chain phthalonitrile modified benzoxazine resin is prepared. Phthalonitrile which is a polymerizable group is introduced into benzoxazine, so that phthalonitrile can participate in curing, the crosslinking density of polybenzoxazine resin can be further increased, and the thermal stability of polybenzoxazine can be further improved. The preparation method is simple and convenient, a synthesis period is short, the yield is high, and raw materials are easy to obtain.

The invention relates to a mesoporous platinum-palladium bimetallic nanoparticle and a preparation method thereof. The particle size of the mesoporous platinum-palladium bimetallic nanoparticle is 30-100nm, and the surface of the nanoparticle has a porous structure whose aperture is uniform, and the aperture is 2-3nm. The preparation method is as follows: (1) sodium tetrachloropalladate, chloroplatinic acid and a surfactant are dissolved in water, the materials are stirred uniformly at 30-90 DEG C, and a mixed solution containing bimetal is obtained; (2) a reducing agent solution is added into the mixed solution containing bimetal obtained in the step (1), a reaction is continued to carry out for 2-5 hours, an obtained reaction solution is centrifugal and separated, and the mesoporous platinum-palladium bimetallic nanoparticle is obtained by post-treatment. The invention provides a simple method for synthesis of the mesoporous precious metal nanoparticle with simple process and short synthesis period; the synthesized mesoporous precious metal nanoparticle is used as a catalyst for an industrial nitrobenzene hydrogenation reaction with very high activity.

The invention belongs to the field of modified carbon nanomaterials and discloses a preparation method of a two-dimensional porous boron-nitrogen double-doping carbon nanomaterial and application thereof. The preparation method disclosed by the invention comprises the following steps: taking urea as a structure template, taking 1-butyl-3-methylimidazolium tetrafluoroborate as a pore forming substance and a doping agent, taking glucose as a carbon source, calcining and performing hydrothermal treatment, thereby obtaining the product. The method disclosed by the invention is simple in operation,short in synthesis period, excellent in repeatability, low in cost and convenient for industrial implementation. The porous boron-nitrogen double-doping carbon nanosheets prepared by the method disclosed by the invention have a uniform and porous thin-layer structure and large specific surface area. Meanwhile, due to introduction of boron atoms, the conductivity is enhanced, the redox activity can be enhanced by virtue of doping of the nitrogen, and ay capacitance is improved. When serving as an electrode material of a supercapacitor, the carbon nanomaterial has high electrochemical energy storage activities including high specific capacitance and excellent cycling stability. When charging/discharging current density is 0.1A/g, the highest specific capacitance can reach 550F/g, and the specific capacitance is much higher than that of most of the carbon-based materials.

The invention discloses a preparation method of an N-doped porous carbon-coated Co3O4 composite nano material. The method comprises the following steps of: dispersing N-doped carbon-coated metal cobalt into ionized water to obtain a dispersion system; adding H2O2 into the dispersion system to obtain a solution system; setting the solution in a condition at a temperature of 180 DEG C for reaction for 24h; performing washing and drying of reacted solution to obtain a product. The present invention further discloses an N-doped porous carbon-coated Co3O4 composite nano material and the applicationthereof. The method is simple in preparation process, uniform in material morphology and large in specific surface, and has a great application potential in the aspects of lithium ion batteries, electrochemical energy storage, catalysis and the like. The method is simple, efficient, safe and feasible, short in synthesis period, can perform large-scale preparation and is hopeful to be popularizedand industrially applied.

The invention belongs to the technical field of biochemical polypeptide synthesis and relates to a method for preparing linaclotide. The method mainly solves the problem that the existing synthesis method has complicated steps of synthesis, high raw material cost, long synthesis period, low yield and more impurity and is unsuitable for industrial production. The method comprises that (1) Fmoc-Tyr(tBu)-OH and a carrier resin undergo a reaction to produce Fmoc-Tyr(tBu)-resin, (2) the Fmoc-Tyr(tBu)-resin and other amino acids with Fmoc protecting groups are coupled one by one through an activator so that linaclotide linear peptide resin is obtained, (3) the linaclotide resin is subjected to deprotection and cracking agent-based cracking to form linaclotide linear peptide, (4) three disulfide bonds of the linaclotide linear peptide is cyclized in an ammonium hydroxide/DMSO system to form linaclotide crude peptide, and (5) the linaclotide crude peptide is purified in an alkaline buffer solution and then is subjected to freeze-drying so that pure linaclotide is obtained.

The invention relates to a method for preparing an efficient polycarboxylate graft copolymer super plasticizer through the microwave-assisting method. The super plasticizer is formed by a polymer monomer A, a polymer monomer B, a polymer monomer C, a polymer monomer D, a polymer monomer E, a polymer monomer F and a polymer monomer G in a copolymerization mode. The method for preparing the efficient polycarboxylate graft copolymer super plasticizer through the microwave-assisting method comprises the steps that firstly, a certain temperature and a certain microwave radiation power are set; secondly, the polymer monomers are added in microwave radiation, and namely, a long polyether, polyester, and a heteroatom side chain is introduced to a polymer chain; thirdly, the pH value is neutralized and adjusted. The water-soluble polycarboxylate concrete super plasticizer prepared according to the method has the advantages of being high in water-reducing rate, small in disperse index of molecular weight, good in overall performance, and good in compatibility with cement. The water-soluble polycarboxylate concrete super plasticizer further has the advantages that synthesis is environmentally friendly, the synthesis period is short, the technology is simple, cost is low, the price is reasonable, and the water-soluble polycarboxylate concrete super plasticizer is suitable for popularization and application.

The invention provides a preparation method of a CuO/Cu2O/Cu ternary composite material. The preparation method comprises following steps: a copper salt solution and an alkali solution are prepared respectively; yeast is added into water for culturing, after culturing, the copper salt solution and the alkali solution are added successively so as to obtain a mixed solution; the mixed solution is subjected to heating reaction so as to obtain a reaction solution; the reaction solution is dried, is calcined, and is cooled to room temperature, and is calcined for another time so as to obtain the CuO/Cu2O/Cu ternary composite material. According to the preparation method of the CuO/Cu2O/Cu ternary composite material, yeast is taken as a micro chemical reactor, in carbon thermal reduction synthesis process, yeast is taken as a carbon source, and is capable of regulating and controlling precursor morphology; the technology is simple; and the synthesis period is short.

The invention discloses a preparation method of an MCM-48 mesoporous molecular sieve. In the preparation method, cetyl trimethyl p-toluenesulfonate salt (CTATos) is used as a cationic surfactant, and the molar ratio of raw materials is as follows: SiO2/CTATos/NaOH/H2O = 1:(0.05-0.07):(0.5-0.67):(80-200). The preparation method comprises the specific steps: firstly dissolving silicon sol in an aqueous solution containing sodium hydroxide and stirring at the constant temperature of 60 DEG C for 1 hour; then adding dropwise the solution to an aqueous solution containing the surfactant and then further stirring at the constant temperature of 60 DEG C for 2 hours; after cooling to room temperature, transferring to a sealed reactor, and crystallizing at the temperature of 80-130 DEG C for 15 to28 hours; and finally filtering the crystallized product, washing, drying and then baking at the temperature of 550-900 DEG C for 3-6 hours to obtain the MCM-48 molecular sieve. Compared with the prior art, the preparation method disclosed by the invention has the most significant advantage that: CTATos is used as the cationic surfactant, thus greatly reducing the use amount of the surfactant in a synthesis system; in addition, the synthesis method provided by the invention has short synthesis period, low cost and good reproducibility; the synthesized product has extremely high hydrothermal stability; and the synthesis method is environmentally friendly.

The invention relates to a method for preparing flexible iron sesquioxide/ferroferric oxide and nitrogen doped carbon composite nano-fibers. The method has the advantages that the problem of poor toughness and electric conductivity of existing metal oxide can be solved by the aid of the method; flexible macromolecules are used as supports and are subjected to composition with metal organic gel precursors with plasticity to obtain precursors, and the precursors are subjected to pyrolysis in inert atmosphere and air atmosphere to obtain the flexible iron sesquioxide/ferroferric oxide and nitrogen doped carbon composite nano-fibers which are flexible metal oxide and nitrogen doped carbon composite nano-fibers; the problems of complicated and harsh conditions for preparing flexible metal oxide and carbon composite materials, high costs and difficulty in large-scale production at present can be solved by the aid of the method; raw materials for the flexible iron sesquioxide/ferroferric oxide and nitrogen doped carbon composite nano-fibers are low in cost, processes for preparing the flexible iron sesquioxide/ferroferric oxide and nitrogen doped carbon composite nano-fibers are simple, and the method is short in synthesis period, good in repeatability and high in yield, and industrial production can be facilitated; the flexible iron sesquioxide/ferroferric oxide and nitrogen doped carbon composite nano-fibers can have characteristics of bendable properties and excellent electrochemical performance, accordingly, the method has an extremely broad application prospect in the field of wearable electronic devices, and the like.

The invention discloses a method for preparing a black alpha-Bi2O3 powder material and belongs to the technical field of synthesis of photoelectric materials. According to the key points of the technical scheme of the invention, the method comprises the following steps: maintaining the temperature of bismuth nitrate pentahydrate in a muffle furnace to be 500 DEG C for 6 hours, naturally cooling, grinding, thereby obtaining a yellow alpha-Bi2O3 powder material; adding the obtained yellow alpha-Bi2O3 powder material into a reaction container, adding deionized water and hydrogen peroxide, irradiating by using a mercury lamp with the power of 300W under the magnetic stirring condition for an hour, standing, pouring the supernatant liquor, and drying the precipitate in a drying oven, thereby obtaining the target product, namely the black alpha-Bi2O3 powder material. According to the method disclosed by the invention, the preparation process is simple and feasible, the synthesis period is short, and the prepared black alpha-Bi2O3 powder material has the absorption edge of 1902nm, has the optical wave utilization rate higher than that of the yellow alpha-Bi2O3 material, and has potential application values in the photoelectric material aspect.

The invention discloses a halogen-free non-phosphorus silicon-containing flame retardant and a preparation method thereof. The flame retardant is a hyperbranched silicon resin containing multiple maleimide groups, has the branching degree of 0.5-0.6 and the molecular weight of 2500-3400 and is liquid at normal temperature. The preparation method comprises the following steps: synthesizing a trialkyl silane solution containing maleimide, performing controlled hydrolysis, and performing suction filtration, reduced pressure distillation and drying, thereby obtaining the halogen-free non-phosphorus silicon-containing flame retardant. The flame retardant contains the maleimide groups and can be copolymerized with an imide ring at a certain temperature, good interaction is obtained when the reactivity is controlled, and the storage stability, reactivity control and flame retardant property of the modified resin are fully exerted. The flame retardant contains multiple maleimide groups and a flexible Si-O-Si chain, so that the modified resin has the outstanding advantages of rigidity, toughness and heat resistance. The preparation method of the flame retardant is environment-friendly, simple, feasible, short in synthesis period, rich in raw material source, wide in applicability and high in yield.

The invention discloses a cubic strontium sodium niobate red fluorescent powder and a preparation method thereof. The method includes the steps of: 1) weighing SrCO3 and Nb2O5 as raw materials according to the molar ratio of (0.625-0.875):1, placing the weighed raw materials in a mortar, and grinding the raw materials at room temperature until the raw materials are mixed uniformly for later use; 2) placing an Al2O3 crucible in a furnace, maintaining the temperature at 1100-1200 DEG C for 3-9 h, cooling the crucible to 300 DEG C at the rate of 2 DEG C/min, cooling the crucible along with the furnace to room temperature and taking the crucible out. The cubic strontium sodium niobate powder having dispersed appearance and uniform distribution is produced in a molten salt manner. Compared with other methods, the molten salt method is easy to carry out and is controllable in granularity, has good crystal morphology and high physical-phase purity, and is short in synthesis period. The method is suitable for preparing cubic particle powder which is dispersed uniformly. Through the molten salt method, the cubic strontium sodium niobate (Na0.5Sr0.25NbO3) powder is completely crystallized, has dispersed appearance and uniform particles, and is high in color purity.

The invention relates to a synthesis method of cefprozil. The synthesis method comprises the following steps: under the existence of an enzyme, enabling parent nucleus 7-APRA and a D-4-hydroxyphenylglycine ester derivative to react with each other, and before the precipitation of cefprozil, adding cefprozil, with the purity greater than 99%, taken as a seed crystal, into a reaction system. According to the invention, the reaction efficiency is improved, the synthesis period is shortened, the conversion rate of 7-APRA is increased, and the purity of the obtained cefprozil is improved; the method is an enzymatic method, and the enzymatic catalysis is only required, water is taken as a solvent, and any organic solvent is not required during the reaction process, so that the environment friendliness is achieved, the route is simple, the product yield is high, and the purity is high.

The invention belongs to the field of catalytic material preparation, and more specifically relates to a nanometer hollow H type ZSM-5 molecular sieve, and a preparation method thereof. The preparation method comprises following steps: a Na type molecular sieve is added into an inorganic aqueous alkali for treatment, ice-water cooling, centrifugation washing, and drying are carried out, ammonium exchange is adopted, sintering is carried out so as to obtain the H type ZSM-5 molecular sieve (HZSM-5) with a nanometer hollow structure. The preparation method is short in synthesis period, and simple in technology process. The H type ZSM-5 molecular sieve prepared using the preparation method possesses a nanometer scale meso pore-micropore multistage pore composite structure; the specific surface area and the exterior surface area are larger; and the H type ZSM-5 molecular sieve can be used in a plurality of catalytic reactions as a catalyst or an active component carrier material.

The invention relates to a lithium ion battery positive pole material, and particularly relates to a method for preparing a lithium iron phosphate positive pole material through a hydrothermal method. The method aims at solving the problems of nonuniform granule, irregular crystal, wide size distribution range, high reaction temperature, long synthesis period, poor product batch stability and material property stability influence in the prior art. In order to solve the problems in the prior art, the technical scheme is as follows: the method for preparing the lithium iron phosphate positive pole material through the hydrothermal method sequentially comprises the following steps of: (1) weighing LiOH.H2O and 85% H3PO4, dissolving the LiOH.H2O into deionized water, slowly dripping strong phosphoric acid into an LiOH.H2O solution, centrifugalizing to obtain Li3PO4 white precipitates, and carrying out vacuum drying to obtain Li3PO4 powder; (2) weighing Li3PO4 and (NH4)2Fe(SO4)2.6H2O, adding the deionized water to dissolve in a beaker, adding reducing agent glucose at the same time, and uniformly stirring; and (3) reacting, then cooling to room temperature, carrying out microwave oscillation, centrifugalizing a lotion for separation, and drying to obtain LiFePO4 powder.

The invention discloses a method for synthesizing a negative electrode material Fe2SSe of a lithium-ion battery by a one-pot solid-phase method. A heat treatment procedure is mild; the standing time at 400 DEG C is relatively long; and a reaction failure or a great loss of a sulfur element caused by the phenomenon that raw material sublimed sulphur is easily sublimed at a high temperature to cause a quartz tube rupture is avoided. The operation steps are simple; the cost is low; the product purity is very high; the equipment requirements are simple; the synthesis period is short; the method is suitable for expanded production; a new way is provided for batch synthesis of the Fe2SSe; the obtained Fe2SSe is blocky-shaped particles; the microstructure is in a two-dimensional layer form; the agglomerate phenomenon is avoided; and the Fe2SSe with the two-dimensional layer structure is beneficial to intercalation and deintercalation of lithium ions in the charging and discharging processes when used as a lithium-ion negative electrode material.

The invention belongs to the field of veterinary drugs, particularly relates to a method for the synthesizing ormetoprim. The method comprises the following steps of: (A), adding 3-methoxypropionitrile in a sodium methoxide solution for a condensation reaction by taking 4,5-dimethoxy-2-methyl-benzaldehyde as a raw material; (B), adding guanidine hydrochloride into the reaction mixture obtained in the step (A), and preform a cyclization reaction to obtain the ormetoprim. According to the one-pot method for synthesizing the ormetoprim, the low-cost 3-methoxypropionitrile replaces the virulent acrylonitrile, so that the synthesis process is environment-friendly, less in reaction step, and short in synthesis period; and the raw material is readily available, low in cost and simple in operation, and the method has broad prospects for large-scale industrial application.