60results about How to "Good experimental reproducibility" patented technology

The invention relates to a preparation method of three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres, and relates to the technical field of multi-level structured nano-grade catalyst materials. First, nickel nitrate hexahydrate and cobalt nitrate hexahydrate are adopted as a nickel source and a cobalt source, a deionized water-isopropanol mixed phase with a proper proportion is adopted as a solvent, methanol is adopted as a reactant, and no additional base precipitating agent is adopted; a three-dimensional flower-shaped nano-sheet microsphere precursor is prepared in a Ni<2+>-Co<2+>-NH3-NH4<+>-SG<n->-H2O-IPA-CH3OH system (SG<n-> is CO3<2-> or HCOO<->); the temperature is increased to 300-400 DEG C in an air atmosphere with a speed of 1 DEG C/min, and the precursor is calcined for 2-3h, such that the three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres are obtained. According to the invention, co-precipitation of the formulated cobalt and nickel in the raw materials is realized. The prepared three-dimensional flower-shaped nickel cobaltate nano-sheet mesoporous microspheres are spinel cubic phases with high purity, and are formed by ultrathin nano-sheet self-assembly. The microspheres comprise rich mesopores, and have a large specific surface area. The method has the advantages of simple operation, appropriate conditions and easy control.

The invention discloses a method for preparing monodisperse carbon microspheres by using cane sugar as a carbon source. According to the method, cane sugar is used as the silicon source, sodium polyacrylate is used as a dispersing agent, and after the hydrothermal reaction at the certain temperature, the monodisperse micron-sized carbon sphere is obtained. A one-step hydrothermal method is adopted in the method for preparing the monodisperse carbon microspheres, and sodium polyacrylate is used as a dispersing agent, and has an important effect on the particle diameter, the dispersity and the surface appearance of the carbon microspheres; the carbon microspheres are solid and have relatively rough surfaces, and can obtain lots of aperture passages through simple high temperature processing; the obtained carbon sphere particle diameter range is 1-6 microns, and the carbon sphere particle diameter can be adjusted controllably through experimental parameters such as cane sugar concentration, the reaction temperature and the reaction time; the obtained carbon sphere can be applied to the fields of liquid chromatograph stationary phases, super capacitors, protein separation, enrichment and removal of organic matter in water, and the like.

The invention brings forward a preparation method of mesoporous nickel cobaltate fiber. According to the preparation method, an organic solvent is added during the preparation process of a precursor; a mixed phase of a water phase and an organic phase is used as a solvent, soluble nickel salt and cobalt salt are used as raw materials, and oxalate is used as a precipitating agent; in a system of Ni<2+>-Co<2+>-NH3-NH4<+>-SG<n->-C2O4<2->-H20-C2H5OH, a fibrous precursor is prepared; and the fibrous precursor is subjected to thermal decomposition in the air atmosphere at 250-400 DEG C so as to obtain the mesoporous NiCo2O4 fiber. According to the invention, coprecipitation based on the Ni-Co ratio set in the raw materials is effectively realized. The prepared NiCo2O4 powder is a cubic phase, has high purity and large specific surface area, is fibrous and porous, and is applicable to be used as a catalyst or an alkaline solution oxygen-evolution/hydrogen-evolution electrode material or direct alcohol fuel cell anode catalyst. The method provided by the invention is simple to operate and easy to control, has advantages of mild condition and low cost, and is suitable for commercialized production.

The invention provides a rechargeable zinc-manganese battery and a preparation method thereof. A positive electrode adopts a linear alpha-MnO2 material to replace a traditional amorphous manganese dioxide material, and the linear alpha-MnO2 material has a uniform structure. The large tunnels and vacancies in MnO2 increase the contact between the active material and the electrode, reduce the internal resistance of the battery, and improve the diffusivity of protons. The larger aspect ratio of MnO2 can make the preferred orientation degree of the material higher, thus improving the rate performance of the battery. Stable structure, not easy to collapse, the activity can be maintained at a high level, the decay rate is slow, more conducive to the battery cycle performance. In accordance withthat present invention, the preparation method of the alpha-MnO2 material is simple and feasible, the experimental reproducibility is good, the raw materials used are cheap and easy to obtain, the linear alpha-MnO2 material has a uniform structure, large aspect ratio, and stable structure, and is not easy to collapse and slow in attenuation rate.

The invention relates to a preparation method of a graphite/Prussian blue composite material. The preparation method comprising that ferrous chloride and sodium ferrocyanide undergo a hydrothermal reaction in an aqueous solution of a surfactant based on a coprecipitation method to produce Prussian blue nanospheres, the Prussian blue nanospheres and graphite oxide are stirred, and the solution is quenched by liquid nitrogen, then is freeze-dried and finally is reduced through hydrazine hydrate. The invention discloses a use of the graphite/Prussian blue composite material as a sodium ion battery positive electrode material. The Prussian blue nanospheres have excellent electrochemical performances. Graphene roll coating further increases the conductivity of the Prussian blue nanospheres and improves the long cycle performance of the Prussian blue nanospheres. The capacity of a sodium ion battery positive electrode prepared from the graphite/Prussian blue composite material is not easy to decay, the magnification performance is good, and after cycle 500 times under current density of 150mAhg<-1>, the capacity is about 110mAhg<-1> and a capacity retention rate is 90.2%.

The invention provides a sintering ore burdening method. The method comprises the following steps of: calculating a liquid phase quantity and temperature relationship of a sintering burdening scheme by adopting thermodynamic calculation software Factsage, determining an undetermined scheme according to the liquid phase quantity and temperature relationship, then obtaining a melting shrinkage rate and temperature relationship of the undetermined scheme through a melting characteristic test experiment, and finally judging whether the undetermined scheme belongs to a reasonable scheme according to an initial melting temperature of the undetermined scheme and the fit degree of the liquid phase quantity and temperature relationship and the melting shrinkage rate and temperature relationship. The method of the invention greatly reduces the experiment workload and the labor intensity, overcomes the defect of burdening sintering ores simply by means of subjective experience, can intuitively and accurately reflect the liquid phase generating property of a sintering process, and has small experimental error and good experimental reproducibility compared with a traditional sintering cup experiment; and a sintering burdening scheme obtained by judging the data fit error is suitable for guiding the practical production.

The invention relates to a method for measuring a lamina decrement difference value of content of a paste-like ink volatile organic compound. The specific steps are as followings: firstly weighing the weight w of an empty glass sheet and recording; spreading an ink sample which is 1-2 times as large as the slicking amount uniformly on a membrane which covering the glass sheet and having a rectangular window by using a doctor blade so that an ink specimen lamina with the thickness of 0.2+/-0.01mm is left on a glass sheet through the window; and weighing the weight W2 of the glass sheet and recording; then baking the glass sheet for one hour in an air blast baking oven at the temperature of 110 DEG C+/- 2 DEG C; taking the glass sheet out and cooling to the room temperature, then weighing the weight W2 of the glass sheet and recording; calculating according to the formulas below: W1-Wempty=Wspecimen, W1-W2=Wvoc, and Wvoc/Wspecimen=Wvoc%; and respectively detecting and calculating the specimens twice and working out an average value. According to the method provided by the invention, a baking method is used for testing directly, the method is simple and feasible to operate and is safe and environmental friendly, the test error can be reduced well, the favorable test repeatability can be obtained, and the analyses accuracy is improved greatly.

The invention relates to a method for breeding cordyceps militaris by silkworm in an early transformation period. According to the method, the living silkworm in the early transformation period serves as a host, cordyceps militaris bacteria are inoculated by an injection method, and inoculation survival rate is greatly increased as the silkworm in the early transformation period is large in body. The concentration of inorganic salt in a strain culture medium is doubled before inoculation, injection is then performed, a more proper inorganic salt environment is provided for growth of the bacteria in silkworm pupas, spawn running time is shortened by 18%, and growth time is shortened by 15.6%. By the aid of the method, the rigidifying rate of the silkworm in the early transformation period reaches 94%-100%, and the fruiting rate of sporocarps reaches 90%-100%. The method for breeding the cordyceps militaris has the advantages of convenience in operation, low breeding rate, good experimental reproducibility and the like, is applicable to large-scale culture and has a wide application prospect.

The invention belongs to the field of analytical chemistry and relates to an extraction head detachable type solid phase micro extraction probe and a preparation method thereof. The preparation method comprises the following steps of: shearing a polydimethyl siloxane tube and a metal wire; coating a layer of high-temperature epoxy resin glue on the metal wire and sleeving the polydimethyl siloxane tube on the metal wire for fixedly bonding to obtain a self-made extraction head, wherein a sleeve is arranged at one end of the self-made extraction head, and a free metal wire is arranged at the other end of the self-made extraction head; then properly extruding at the position of an inner tube of a solid phase micro extraction probe suit, which is away from the tail end by 0.2-0.5cm so as to generate a dent, or bending the free metal wire part of the self-made extraction head by more than one bent; and inserting the metal wire into the inner tube. The probe is simple and convenient in theuse and preparation processes; the probe can be continuously used by extracting the extraction head and inserting a new self-made extraction head after being used; and the repeated selective examination times can reach 80-120 times. The cost of each probe is one thousand of that of the traditional commercial probe and has strong operability and reliability.

The invention belongs to the technical field of batteries, particularly to a preparation method of a long-acting metal lithium reference electrode for lithium ion and lithium metal batteries. The method comprises the following steps: soaking copper metal in an acid solution to remove a passivation layer on the surface of the copper metal; placing the copper metal without the passivation layer in an electrolytic tank to be electroplated with lithium metal; and coating the lithium-plated copper metal with an inorganic solid electrolyte layer through a physical or chemical pretreatment method. The reference electrode provided by the invention has good electrolyte corrosion resistance, can ensure long-time electrode potential stability, and provides a stable reference basis for monitoring potential changes of a positive electrode/a negative electrode respectively.

The invention relates to a quantum dot luminescent glass, and a preparation method and application thereof. Glass comprises 60-65% of SiO2, 15-25% of Al2O3, 0.1-5% of B2O3, 10-20% of Na2O, 0.1-5% of P2O5, 0.1-5% of MgO and 0.1-5% of SnO. A quantum dot comprises 5-15% of ZnO, 1-5% of CdS and 1-5% of Se. The preparation method comprises the following steps: preparing CdSxSe1x/ZnS powder from the quantum dot component; and uniformly mixing CdSxSe1x/ZnS powder with glass powder to obtain quantum dot luminescent glass powder, dissolving the quantum dot luminescent glass powder, casting to obtain aglass block, annealing, and cooling to room temperature to obtain the quantum dot luminescent glass.

The invention discloses a production method for synthesizing an environment-friendly magnesium isostearate detergent in the field of lubricating oil. The method comprises the following steps: (1) sequentially adding isostearic acid, dilute oil, dimethylbenzene, methanol, ammonia water and active-60 magnesium oxide into a 100mL stainless steel high-pressure kettle with a magnetic stirrer, sealing the high-pressure kettle, starting magnetic stirring, and performing a neutralizing reaction for 1-3h at 50-65 DEG C; (2) heating to 55-62 DEG C and pressing in a carbon dioxide gas to perform a carbonation reaction; and (3) after the reaction, centrifuging the reaction mixture and filtering to remove slag, and removing the solvent to obtain the oil-soluble magnesium isostearate detergent. The method disclosed by the invention has the beneficial effects that a detergent product with high base number over 350mg(KOH)/g is synthesized, and the synthesis method is easy to operate and has good experimental reproducibility.

The invention discloses a polyacid-imidazole member containing cadmium-based fluorescent probe compound, a preparation method therefor and an application of the polyacid-imidazole member containing cadmium-based fluorescent probe compound and belongs to the fields of synthesis and application fluorescent materials. The probe compound has a chemical formula of Cd2(C16H6O8)(C10H14N4)0.5(H2O)3.H2O and a molecular formula of C21H21Cd2N2O12, wherein C16H6O8 is deprotonated 2,3,3',5'-biphenyl tetraformic acid, and C10H14N4 is 1,4-diimidazolyl butane. The probe compound is prepared from an inorganiccadmium salt, the deprotonated 2,3,3',5'-biphenyl tetraformic acid and the 1,4-diimidazolyl butane, which serve as reactants, by a hydrothermal method, is a brand-new product and is simple in materialsynthesis process, high in yield and purity and good in stability; the production equipment is simple, and the raw materials are cheap and readily available; and the material has high detection and recognition capability to metal ions and organic solvents and can be extensively applied to detection, recognition, imaging and the like of specific ingredients in living bodies and water environments.

The invention provides a test method capable of effectively improving the mixing ratio of burning ash in cement raw materials. The method comprises the following steps of: analyzing original characteristics; performing washing pretreatment; firing ingredients to form clinker; and testing index and toxicity of the cement. The test method is designed completely aiming at a practical project, the raw materials are all the actual raw materials of a cement factory and the mixing ratio is also the actual production control ratio of the cement factory; the test method is well instructive to the project application; and on the premise of realizing stable operation of cement production and guaranteeing production quality, the test method greatly improves the mixing ratio of the burning ash in the cement raw materials. The whole test has the advantages of relatively a few involved large instruments, convenient operation, low cost and high test reproducibility.

The invention relates to a detection method for the residual quantity of chloramphenicol. The detection method includes the following steps of 1, sample pretreatment, wherein ethyl acetate is added into a sample, homogenizing and centrifugation are conducted, and then the mixture is evaporated to be almost dry; 2, purification of the sample, wherein normal hexane and an anhydrous sodium sulfate column are sequentially used for purifying the sample obtained in the step 1; 3, derivatization of the sample and a standard product, wherein acetic anhydride is adopted as a derivatization reagent, triethylamine is adopted as a catalyst, and the sample and the standard product are derived; 4, gas chromatography detection, wherein the sample solution and standard product solution obtained in the step 3 are injected into a gas chromatograph for detection. According to the detection method for the residual quantity of chloramphenicol, derivatization steps are simple, detection efficiency is high, the adopted derivatization reagent is low in sensitivity to the environment, the adopted catalyst is cheap, and harm to people and the environment is low.

The invention provides a preparation method of ultra-long highly-orderly TiO2 micro/nanoscale fiber. The preparation method includes following steps: (1), dissolving PEO used as a fiber forming formwork in a solvent, adding tetrabutyl titanate, stirring and standing to obtain a spinning solution, wherein molecular weight of PEO is 1000, 000-5000, 000; (2), subjecting the spinning solution to electrostatic spinning using a drum as a fiber collector to obtain highly-oriented Ti(OC4H9)4/PEO composite fiber; (3), heating and annealing the composite fiber through a program. The preparation method is simple to operate, low in equipment requirement and simple in preparation process, preparation of inorganic fiber which is arranged in a highly-orderly manner is enabled to be simple and easy to operate, and the preparation method is easy in mass production and high in experiment repeatability.

The invention provides a method for quickly quantifying traditional Chinese medicine active components based on a NMR (Nuclear Magnetic Resonance) technique. The method comprises the following steps: 1) dissolving a sample in a deuterium-substituting reagent, transferring into a nuclear magnetism tube and adding an internal standard substance into the nuclear magnetism tube; 2) sampling by adopting hydrogen resonant frequency in NMR; and 3) selecting a feature structure signal peak and an internal standard substance signal peak of a to-be-measured component and quantifying and calculating the content of the to-be-measured component by adopting an internal standard method. The method selects the NMR technique to detect the content of the traditional Chinese medicine active components, is capable of quickly quantitative analyzing the active components, such as, Chinese herb extracts, primary separating compounds or mixture thereof and natural sourced small molecule compounds, and is capable of giving the mole content. The method has the characteristics of simple operation, quick batch realization, high test reproducibility, direct and reliable test data, and the like; the method is especially suitable for the detection for trace sample; and a quick quantifying thought and a quick quantifying method are supplied for the research on the traditional Chinese medicine or compound effective material basis.

The invention relates to a rare earth catalyst and a preparation method thereof and a styrene syndiotactic polymerization method. The structural formula of the catalyst is shown in the description, wherein Ln is rare earth metal; R is alkyl or amido or halogen connected with the rare earth metal; B is alkyl with 1-10 carbon atoms or alkyl with 1-10 carbon atoms and several silicon atoms or alkyl with 1-10 carbon atoms and several halogen atoms; D is N or P or As; R' is hydrogen or methyl or ethyl or isopropyl or t-butyl; R'' is aryl or alkyl containing various substituent groups.

The invention discloses a simple preparation method for explosive solvate. The simple preparation method comprises the following key steps: under a normal temperature condition, placing explosive rawmaterials and a solvent in a sealed environment separately, slowly volatilizing the solvent through vacuuming, generating solvent steam of low pressure and low concentration, enabling the solvent steam to freely diffuse to the surface of explosive crystal, and inducing a gas-solid reaction, thereby obtaining the explosive solvate. The explosive solvate prepared by using the method is of a micro crystal cluster structure and has relatively low temperature, and a primary template can be provided for later explosive micro structure regulation and control. The method has the characteristics of being simple in process procedure, gentle in experiment condition, rapid and efficient in preparation, free of pollution, low in cost, and the like, and is particularly applicable to on-scale preparation.