58results about How to "Optimize synthesis conditions" patented technology

The present invention discloses a kind of polyimide fiber and its preparation process. The preparation process includes the following steps: 1. reacting 4, 4í»-diamino diphenyl ether and pyromellitic dianhydride in the weight ratio of 1 to 1.02 with N, N-dimethyl acetylamide solution of 15-20 % concentration at 0-5 deg.c to obtain polyamic acid solution; 2. wet spinning the polyamic acid solution and imidation reaction of the polyamic acid fiber to obtain polyimide fiber through dewatering and cyclization; and 3. mixing the polyimide fiber with acetic anhydride and triethylamide, flushing with acetone, soaking and drying to obtain the polyimide fiber. The present invention has positive effects of optimized synthesis condition of spinning solution, prolonged solidification period of initially formed fiber in the solidification bath, and fiber with ideal mechanical performance.

The invention relates to a method for preparing zinc molybdate ultrafine anti-bacterial powder by adopting a molten-salt growth method. The method comprises the following steps that: sodium molybdate and zinc nitrate serving as raw materials and sodium nitrate serving as a salt material are mixed in a mortar in the proportion of 1:1:8-18; a proper amount of absolute alcohol is added in the mortar to grind for 1 to 2 hours to ensure that the raw materials and the salt material are mixed sufficiently and uniformly; the mixture is dried for 2 to 4 hours at 90 DEG C in a crucible, and is melted and calcined for 3 to 7 hours in an electric furnace at the temperature of between 320 and 360 DEG C; and the calcined curing product is sufficiently soaked and washed with distilled water, is filtered and dried to remove residual fused salt to obtain the ultrafine zinc molybdate powder. Researches prove that the ultrafine zinc molybdate anti-bacterial powder prepared by the molten-salt growth method has bacteria resistance superior to the anti-bacterial powder synthesized by a chemical precipitation method under the same testing condition, and avoids the problems of high cost and color change by using a silver antibacterial agent. The method can be widely applied in the fields of plastics, ceramics, paints and the like.

The invention relates to a method for preparing an inclusive agent of a polylactic acid or hydroxyapatite composite bone tissue restoring material, which comprises the following steps: getting processed hydroxyapatite by refluxing hydroxyapatite in the alcohol solution with surface modifier as the coupler for 12-48 hours; dissolving polylactic acid macromole monomer with terminal ethenyl and the processed hydroxyapatite in the organic solvent with initiating agent; protecting with nitrogen; extracting after extracting and drying the reactor; separating and purifying no-grafted polylactic acid macromole monomer; extracting the remainder; drying; getting the inclusive agent. The inclusive agent has the wide application, the low cost, the simple method, the mild synthesis condition, the strong utility and the easy industry production, which provides the boundary interaction of the organic or inorganic phase in polylactic acid or hydroxyapatite composite bone tissue restoring material, and improves the ergology property of bone tissue restoring material.

The invention relates to an application method of MIL-100(Fe) catalyst in NH3-SCR (Selective Catalytic Reduction) reaction, which belongs to the technical field of atmospheric pollution control smoke denitrification. The invention relates to a Fe-MOFs catalyst for NH3-SCR reaction and a preparation method thereof. The method comprises the following steps of tabletting and pulverizing the measured Fe-MOFs catalyst powder not less than 0.3g, sieving the Fe-MOFs catalyst powder to obtain 20-mesh to 40-mesh Fe-MOFs catalyst for the NH3-SCR reaction; arranging the Fe-MOFs catalyst onto silica wool in a reaction pipe, and blowing mixed gas into the reaction pipe, wherein the reaction temperature is 25 to 300 DEG C, the mixed gas is the mixture of NO, NH3, O2 and N2, the flow rate of the mixed gas is 100ml / min, the concentration ratio of the NH3 and NO is 1:(1-1.2), the concentration of O2 is 1 to 10 percent of the flow rate of the mixed gas, and N2 is used as the reaction balance gas. The Fe-MOFs catalyst is primarily applied to the NH3-SCR catalyst, and the denitrification effect is good.

The invention relates to a method for synthesizing a titanium silicalite molecular sieve TS-1 for catalytic hydrogen peroxide oxidation. The method comprises the following steps of (1) uniformly mixing a titanium source with a silicon source through stirring, so as to obtain clear liquid; (2) mixing an organic template agent with the first clear liquid, hydrolyzing through drastic stirring till clear liquid is formed again, warming to remove glycol so as to obtain second clear liquid, wherein the pH is 11-14; (3) slowly dripping an ammonia solution of ammonium fluoride into the second clear liquid, and stirring while dripping, and finally obtaining clear mother liquid with the same pH as the second clear liquid; (4) crystallizing the clear mother liquid for 12-36 hours at 130-190 DEG C under autogenous pressure, then separating, drying and burning so as to obtain solid powder TS-1 molecular sieve. Compared with the prior art, the method has specific process steps, reduces the particlesize of the crystal due to introduction of fluoride, and improves the catalysis performance.

The invention provides a preparation method and application of a rod-like ozone catalyst Cu-OMS-2. The preparation method includes: providing a first solution, wherein the first solution comprises a Mn<2+> solution [such as manganese acetate (Mn(CH3COO)2), manganese chloride (MnCl2 4H2O), manganese nitrate (Mn(NO3)2) and manganese sulfate MnSO4 H2O], copper chloride dihydrate (CuCl2 2H2O) and a dispersing agent; providing a second solution, wherein the second solution comprises a second solvent and potassium permanganate (KMnO4) powder evenly dispersed in the second solvent; dropwise adding the second solution into the first solution, and stirring and performing ultrasonic treatment to obtain a mixture; placing the mixture into a high-temperature reaction kettle to perform reaction, centrifuging, drying, grinding, and calcining at high temperature to obtain the Cu-OMS02 ozone compound catalyst. Cu<2+> is doped into an OMS-2 crystal structure and then used for ozone catalysis, metal iondissolution after traditional metal catalyst reaction is lowered effectively, and catalyst activity and stability are increased.

A method of producing carbon nanotubes, comprising, in a reaction chamber: evaporating at least a partially melted electrode comprising a catalyst by an electrical arc discharge; condensing the evaporated catalyst vapors to form nanoparticles comprising the catalyst; and decomposing gaseous hydrocarbons in the presence of the nanoparticles to form carbon nanotubes on the surface of the nanoparticles. Also a system for producing carbon nanotubes, comprising: a reactor comprising two electrodes, wherein at least one of the electrodes is at least a partially melted electrode comprising a catalyst, the reactor adapted for evaporating the at least partially melted electrode by an electrical arc discharge and for condensing its vapors to form nanoparticles comprising the catalyst, wherein the electrodes are disposed in a reaction chamber for decomposing gaseous hydrocarbons in the presence of the nanoparticles to form carbon nanotubes on the surface of the nanoparticles.

The invention relates to a PM catalyst for high intensity synthetic diamond, the percentage by weight of each component in terms of Co: 12 ~ 17%, Mn: 5 ~ 10%, C: 1 ~ 5%, surplus is Fe. Preparation, with metal powder and ball mill will be fully mixed toner, pre-Cold molding. Metal powder was spherical particle size of 100 to 300 head. After sintering and grinding the catalyst tablets treat the need size. In the actual production, the invention used as a catalyst at the high-pressure high-temperature (1300deg.C, 5.3MPa) complex synthetic diamond 40-60 coarse granularity in more than 85%, peak output static strength >= 13kg, in the proportion of 57% and above, the maximum static pressure Strength to 35. The oxygen content of catalyst <150PPm, is conducive to the growth of diamond-shaped, effectively raising the grade synthetic diamond. The massive iron replacement nickel, the overall price is lower than existing technology in the nickel manganese cobalt catalyst.

The invention discloses a low-cost hierarchical pore SAPO-34 molecular sieve and a preparation method and application thereof, and belongs to the technical field of molecular sieve synthesis. The invention provides preparation method of the SAPO-34 molecular sieve by taking lithium silicon powder waste as a raw material. The preparation method comprises the following steps: washing lithium siliconpowder with acid, drying and sieving to obtain powder; uniformly mixing water with a phosphorus source to obtain a phosphorus source solution; mixing the powder with a phosphorus source solution, adding a template agent, and uniformly mixing to obtain a mixed solution; aging the mixed solution at room temperature, heating, and carrying out hydrothermal crystallization to obtain a crystallizationsolution; and cooling, washing, filtering, drying and calcining the crystallization liquid to obtain the SAPO-34 molecular sieve. According to the invention, resource utilization is carried out on a large amount of waste residue lithium silicon powder piled up at present, and the SAPO-34 molecular sieve has a micro-mesoporous hierarchical pore structure by controlling the consumption of each material and optimizing the synthesis condition, so that the defect of a single microporous structure is effectively overcome, and the SAPO-34 molecular sieve can be used as a carrier material of a low-temperature denitration catalyst.

The invention relates to silicate blue light fluorescent powder having an expression formula of Gd4.67Si3O13:xBi<3+>, wherein doped Bi<3+> is an active ion, and x ranges from 0.01 to 0.2. According to the fluorescent powder, a small amount of Bi<3+> ions are introduced into a Gd4.67Si3O1 matrix, and under irradiation of ultraviolet light with the peak value being about 370nm, and bandwidth emission close to 450nm can be generated. The preparation method of the blue light fluorescent powder comprises the following steps: respectively weighing elementary substances, oxides, halides or corresponding salts of Gd, Si and Bi according to amounts of substances in the expression formula; grinding and fully mixing in an agate mortar, putting in a corundum crucible and covering, and heating in a high-temperature furnace to 1200-1400 DEG C, holding the temperature at 1200-1400 DEG C constantly for 2-8 hours; and then, naturally cooling to room temperature, taking out and smashing to obtain the adjustable blue light emission fluorescent powder.

The invention discloses a microwave preparation method of high-quality aluminum nitride powder. The microwave preparation method comprises the following steps of: mixing an aluminum source with a carbon source in a C / AL molar ratio of (3-6):1; adding calcium carbonate with an Al / Ca molar ratio of 100:(1-5) for uniformly mixing; carrying out microwave synthesis in a microwave reaction device under a nitrogen-containing atmosphere, wherein the heating rate for the microwave synthesis is 3 DEG C / min-20 DEG C / min, the temperature is 1200 DEG C-1600 DEG C, and the thermal insulation time is 0-10 hours; and cooling the obtained product to obtain the high-quality finished product aluminum nitride powder. Different from a conventional heating way by convection, conduction or radiation, the microwave preparation method is used for generating heat by coupling a special wave band of the microwave with a base structure of the material, and used for heating in an integral material heating way by virtue of medium loss of the material; moreover, the microwave preparation method of the high-quality aluminum nitride powder has the advantages of good synthesis quality, low synthesis temperature, short synthesis time, low synthesis energy consumption and the like.

The invention relates to a method for preparing a titanium sol carrier zinc and copper ion-adsorbing antibacterial agent by microwave heating. The method comprises the following steps of: dripping 8mL of butyl titanate into 20mL of ethanol for uniformly mixing under certain condition, and adding 2mL of glacial acetic acid to prepare solution A; stirring 60mL of ethanol and 2mL of distilled water and adding nitric acid to regulate the pH value to be 2-3 so as to prepare solution B; dripping the solution B into the solution A at a dripping speed of 50 to 60 drops per minute, stirring, regulating the pH value to be 2-3, and heating the solution in a microwave oven for 20 to 90 seconds so as to prepare titanium sol; dripping 0.3mol / L solution of copper nitrate and zinc nitrate into the titanium sol, stirring for 1 to 2 hours at the temperature of 30 DEG C, and performing microwave heating for 20 to 50 seconds so as to prepare titanium gel for absorbing the zinc and copper ions, wherein the ion addition is 8:100 (the molar ratio of total ions to the butyl titanate) and the molar ratio of zinc ions to copper ions is 2:1; drying, grinding and calcining the gel, keeping the temperature at 450 DEG C for 30 to 60 minutes, and finally taking the product out so as to prepare the needed antibacterial agent. Researches prove that: the antibacterial agent has excellent performance, and simultaneously solves the problems that a silver antibacterial agent has high cost and an antibacterial material changes color and has single function.

The invention discloses a preparation method of an LiNixCoyMn1-x-yO2 / Li2O.B2O3 (x is larger than 0 and is smaller than or equal to 0.6, and y is larger than 0 and is smaller than or equal to 0.4) composite anode material. The preparation method comprises the following steps: preparing a NixCoyMn1-x-yCO3 precursor by adopting a coprecipitation method, then sufficiently mixing with a lithium source,finally preparing an LiNixCoyMn1-x-yO2 anode material by adopting a high temperature solid phase method, enabling the surface of a particle to be manganese-rich and nickel-poor to be beneficial for improving the stability of the material, and then preparing the LiNixCoyMn1-x-yO2 / Li2O.B2O3 composite anode material by adopting a wet chemistry method. The material has relatively high specific capacity, high in high rate performance, and high in cycle performance, and can be applied in fields such as various portable electronic equipment, electric vehicles and energy storage equipment.

The invention relates to a microwave synthesis method for aluminum nitride powder. In the method, microwave synthesis is performed by using aluminum powder as a raw material and comprises the following steps of: thoroughly and uniformly mixing the aluminum powder with particle size smaller than 0.5 millimeters and ammonium salt according to a proportion; placing the mixture according to a figure 1 and putting the mixture into a microwave synthesis reaction cavity, wherein the microwave frequency is 2, 450 MHz, the pressure is the normal pressure and the synthesis temperature is between 600 DEG C and 1,300 DEG C; introducing nitrogen-containing atmosphere for microwave synthesis; keeping the temperature for 0 to 5 hours; and cooling the synthesized product to obtain the finished product of the aluminum nitride powder. In the microwave synthesis method, heat is generated by coupling a special wave band of the microwave and a basic structure of the material and the dielectric loss of the material makes the material heated in an integral heating way which is different from the conventional heating way through convection, conduction or radiation; and the method has the advantages of low synthesis temperature, short synthesis time, low energy consumption of synthesis, high yield, high product performance, simple process and the like and can realize large-scale industrial production.

The method for preparing 6-methyl-1,2-3-oxathiazine-4-(3H)-keto-2,2-dioxopotassium salt includes the steps of acetoacetylation of aminosulfuryl fluoride by means of diketene, cyclopolymerization in the methyl alcohol solution of sodium hydroxide or potassium hydroxide and purification, in which the acetoacetylation step is implemented in the presence of alkali metal salt of organic weak acid, andunder the condition of that the product crude is potassium salt said purification step can be implemented by using alcohol water recrystallization method, and under the condition of that the product crude is other salt except for potassium salt said purification step can be implemented by using organic solvent extraction method and alcohol water recrystallization method.

The invention discloses a method for measuring amino group contents of chitosan derivatives on the basis of headspace gas chromatography. According to the method, excess ninhydrin is reacted with a standard substance containing an amino group; sodium hydrogencarbonate is reacted with the remaining ninhydrin to generate carbon dioxide; the standard substance is not added in a control group; the peak area of carbon dioxide is measured through the headspace gas chromatography; the relative reduction of the carbon dioxide is in a linear relationship with the mass of the standard substance; a standard curve is established and the standard substance is replaced by a chitosan derivative, the amino group content of which is to be measured; and the peak area of the carbon dioxide is detected; the mass of the corresponding standard substance at the moment is obtained according to the standard curve; and calculation is carried out to obtain the amino group content at the moment. When the method is compared with the traditional conductometric titration method, the relative errors do not exceed 13.03%, and for the detection of a same sample, the maximum relative standard deviation is 4.83%, sothe results are objective and accurate and the method is higher in speed when being compared with the traditional measuring methods.

The invention discloses a preparation method of sodium vanadium trifluorophosphate serving as a positive electrode material of a sodium-ion battery and belongs to the technical field of battery material synthesis. The preparation method comprises the following steps: (1) dissolving raw materials such as a carbon source, a vanadium source, a phosphorus source, a fluorine source and a sodium source;(2) removing free water under a heating condition to obtain wet sol; (3) carrying out vacuum drying on the wet sol to obtain dry gel; (4) grinding the dry gel to obtain a powdery precursor; and (5) under the protection of a flowing inert atmosphere, presintering and roasting the precursor, and cooling along with the furnace. The sodium vanadium trifluorophosphate serving as a positive electrode material of a sodium-ion battery prepared by the method is high in purity, a low working voltage platform of about 3.3V (vs.Na<+> / Na) caused by a miscellaneous phase is eliminated, and the working voltage and the energy density of the positive electrode material are improved. The preparation method is simple to operate and good in reproducibility, and the prepared material has relatively high energy density and excellent rate and cycle performances and can meet the requirements of practical application of the sodium ion battery.

The invention discloses a covalent organic framework material BM-SO3H with acid-base dual functions as well as a preparation method and application thereof, the material has a structure as shown in a formula (I), and the preparation method comprises the following steps: firstly, synthesizing a benzimidazolyl covalent organic framework material BM under the catalysis condition of a photocatalyst; then, the BM and 1, 3-propane sultone are subjected to a ring-opening N atom alkylation reaction, and the covalent organic framework material BM-SO3H is obtained. The material has benzimidazole and propane sulfonic acid structures, so that the material has acid-base dual functions. BM-SO3H is used as a heterogeneous catalyst to catalyze a tandem decarboxylaldehyde Knoevenagel condensation reaction, and the yield can reach 95%-99%. The heterogeneous catalyst BM-SO3H shows excellent catalytic performance, thermal stability and recycling performance, and has a good application prospect.

The invention relates to a method for preparing an inclusive agent of a polylactic acid or hydroxyapatite composite bone tissue restoring material, which comprises the following steps: getting processed hydroxyapatite by refluxing hydroxyapatite in the alcohol solution with surface modifier as the coupler for 12-48 hours; dissolving polylactic acid macromole monomer with terminal ethenyl and the processed hydroxyapatite in the organic solvent with initiating agent; protecting with nitrogen; extracting after extracting and drying the reactor; separating and purifying no-grafted polylactic acidmacromole monomer; extracting the remainder; drying; getting the inclusive agent. The inclusive agent has the wide application, the low cost, the simple method, the mild synthesis condition, the strong utility and the easy industry production, which provides the boundary interaction of the organic or inorganic phase in polylactic acid or hydroxyapatite composite bone tissue restoring material, and improves the ergology property of bone tissue restoring material.

The invention relates to polyester resin as well as a preparation method and application thereof. The polyester resin is prepared by firstly subjecting polybasic acids, polyol and 3-hydroxyalkanoate to esterification reaction under the action of esterification catalysts and then subjecting polybasic acids, polyol and 3-hydroxyalkanoate to polycondensation under the actions of polycondensation catalysts and stabilizing agents, wherein the feed molar ratio of polybasic acids to polyol to 3-hydroxyalkanoate is 1 to (1.3-1.6) to (0.25-0.65); the polybasic acids are terephthalic acid and isophthalic acid; the feed molar ratio of terephthalic acid to isophthalic acid is 1 to (0.88-0.91); polyol is selected from one or a composition of more of glycol, 1,2-propanediol, 1,4-butanediol, neopentyl glycol and 1,6-hexanediol. The polyester resin can be biologically degraded, has a low melting point, is stable, is insoluble in water and can be better stored at room temperature.

A method for rapid screening a high-selectivity methanol-to-olefin catalyst includes filling catalyst powder into a reactor and enabling the upper portion and the lower portion of the reactor to be filled with inert silicon carbide particles; vacuumizing the reactor and then heating the reactor to the temperature of 50-300 DEG C at a speed rate of 5-30 DEG C / min; injecting mixed gas of ethylene / inert gas and propylene / inert gas within a volume ratio range of (20 / 80)-(80 / 20) into the reactor in a pulsing manner, measuring stopping time of ethylene and stopping time of propylene in a reactor bed layer, and judging average diolefin selectivity of the catalyst according to the stopping time. The method for rapid screening the high-selectivity methanol-to-olefin catalyst has the advantages of simplicity in operation, short time and high accuracy.

The invention discloses a preparation method of a phenyl boryl modified covalent affine magnetic solid phase extractant. The method comprises the following steps: using ferroferric oxide as a magneticcore; coating the magnetic core with silicon dioxide by using triethoxysilane as a silicon source; reacting under the condition of sodium carbonate by taking bromobenzyl bromide as a raw material; grafting bromobenzene outside a silicon dioxide coating layer; lastly, preparing the phenyl boryl modified covalent affine magnetic solid phase extractant from biborate serving as a raw material under the catalysis of dichloroferrocene palladium chloride. The covalent affine magnetic solid phase extractant disclosed by the invention belongs to a new generation of magnetic solid phase extractant. Compared with the conventional solid phase extractants, the covalent affine magnetic solid phase extractant has the advantages of easiness and convenience in synthesis, milder synthesis conditions and moderate particle size.

The invention provides a preparation method of rosuvastatin calcium. A rosuvastatin calcium side chain is prepared by using allene as a raw material and is used to synthesize rosuvastatin calcium. According to the method, a hydrogen peroxide-heteropoly acid oxidation system is used to oxidize the side chain from olefin to aldehyde, thereby avoiding harsh conditions of low-temperature reaction in the prior art and being more beneficial to industrial production.

The invention provides a method for synthesizing an MCM-49 type zeolite molecular sieve under the condition of no organic template agent. Silica-alumina gel is formed by stirring and mixing an alkalimetal oxide source, an aluminum oxide source and a silicon dioxide source at room temperature, so that the composition of the silica-alumina gel has the following molar ratio relationship: Na2O / SiO2 =0.017-0.19, SiO2 / Al2O3 = 10-50, and H2O / SiO2 = 3-15. The preparation method comprises the following steps: carrying out aging treatment on silica-alumina gel, adding the MCM-49 type zeolite molecularsieve as a seed crystal, and carrying out hydrothermal treatment to obtain a crystal product; and cooling the product at room temperature, washing to be neutral, drying and calcining to obtain MCM-49type zeolite molecular sieve powder. According to the synthesis method provided by the invention, an organic template agent does not need to be added, so that the environmental pollution caused by hexamethylene imine is avoided while the cost is reduced. The MCM-49 type zeolite molecular sieve product obtained by the method provided by the invention can be used as a seed crystal and can be continuously used in a new round of MCM-49 type molecular sieve synthesis process.

The invention discloses a method for synthesizing carbon dots and detecting copper ions in a water body, and relates to the technical field of carbon dot synthesis, and the method is technically characterized by comprising the following steps: synthesizing fluorescent carbon dots by taking tea as a raw material and adopting a hydrothermal method, and optimizing synthesis conditions; with the synthesized fluorescent carbon dots as probes and by means of the fluorescence of the carbon dots, detecting copper ions in the water body, opetimizing the conditions for detecting the copper ions, and detecting the Cu<2+> in the water body by virtue of a linear relationship between the fluorescence intensity of the fluorescent carbon dots and the Cu<2+> concentration. According to the preparation method, the tea is taken as a raw material, the fluorescent carbon dots are synthesized by adopting a hydrothermal method, and synthesis conditions are optimized, so that the preparation operation of the carbon dots is simple, the preparation efficiency is high, and meanwhile, the synthesized carbon dots are good in fluorescence property, photobleaching resistance and salt resistance; and besides, the synthesized fluorescent carbon dots are used for detecting Cu<2+> in a water body, Cu<2+> in the water body is detected by utilizing a fluorescence spectrophotometric method, the detection sensitivity is high, the selectivity is good, and simple and rapid detection of heavy metal ions in an environmental water sample can be realized.

The invention discloses a method for measuring the amino group content of chitosan derivatives based on headspace gas chromatography. The method is to use excess ninhydrin to react with an amino group-containing standard substance, and then use sodium bicarbonate to react with the remaining ninhydrin The reaction generates carbon dioxide. No standard substance is added to the control group. The peak area of ​​carbon dioxide is measured by headspace gas chromatography. The relative reduction of carbon dioxide is linear in relation to the quality of the standard substance. A standard curve is established, and then the standard substance is replaced by the standard substance to be tested. Chitosan derivatives with amino content, and detect the peak area of ​​its carbon dioxide, obtain the quality of the corresponding standard substance according to the calibration curve, and calculate the amino content at this time. Compared with the traditional conductometric titration method, the relative error is no more than 13.03%, and for the detection of the same sample, the relative standard deviation is at most 4.83%, so the result is objective and accurate, and faster than the traditional determination method.

An inorganic millipore nickel cabolt phosphate molecular sieve is prepared through proportionally mixing the inorganic or organic metal salts of Ni and Co, ethyldiamine, ammonia water, phosphoric acid and hydrofluorie acid, crystallizing, separation, washing and drying.