1647results about How to "Short reaction cycle" patented technology

The present invention provides a preparation method of (S)-4-hydroxyl-2-oxo-1-pyrrolidine acetamide. The preparation method comprises: (S)-4-halogen-3-hydroxyl butyric ester as a raw material reacts under the conditions with polar solvent and alkalinity to prepare the crude product of (S)-4-hydroxyl-2-oxo-1-pyrrolidine acetamide; and the crude product is purified. The preparation method is characterized in that inorganic alkali is added for a plurality of times in the reaction process under the condition with alkalinity so as to control the pH value in the reaction to be less than or equal to 8.5. A large quantity of repeated tests are completed to determine that the optimum pH value of the reaction under the condition with alkalinity is less than or equal to 8.5, and the alkali is added in batches to strictly control the pH value of the whole reaction process, so that the alkali conditions required in the reaction can be satisfied and the reaction can be performed completely, and the target product (S)-oxiracetam is prevented from being damaged in the alkaline solution, thereby improving the yield rate of the target product (S)-oxiracetam and reducing the cost.

The invention discloses a method for synthesis of a cobalt nanoparticle and bamboo-like nitrogen doped carbon nanotube composite material. The method includes: dissolving a soluble cobalt salt and an amine polymer in a hydrophilic reagent according to a mole ratio of 1:(2-200), performing evaporation at 60DEG C, conducting grinding after cooling, performing calcination at 400-1400DEG C under nitrogen atmosphere, then treating the sample with acid, and carrying out washing, centrifugation and drying so as to obtain the cobalt nanoparticle and bamboo-like nitrogen doped carbon nanotube composite material. The obtained cobalt nanoparticles have small particle size and are employed to coat the head of a carbon nanotube evenly so as to combine tightly with the carbon nanotube. The composite material has application prospects in fuel cell anode materials, lithium ion battery cathode materials and the like. The method designed by the invention has the advantages of easily available raw materials, simple process and no pollution, short preparation period, mild reaction conditions, low cost, and mass synthesis capability, etc.

The invention relates to a tazobactam synthesis method which comprises the steps of: with 6-APA(Amino Penicillanic Acid) as raw material, preparing a key intermediate 6,6-dihydro penam sulphoxide acid diphenylcarbinol ester through successive reactions of esterification, oxidation, reduetive debromination and the like without separation; then, reacting with 2-triphenyl silicon-1,2,3-triazole; introducing a triazole ring; and finally obtaining the final product of tazobactam through potassium permanganate oxidation and metacresol deprotection. The tazobactam synthesis method is mainly characterized in that a phase transfer catalyst is introduced in the first step, therefore, the reaction rate and the product purity are improved; since an environment-friendly hydrogen peroxide-cobalt acetate catalytic oxidation system is adopted in the third step, the characteristics of good reaction selectivity, high yield, catalyst recyclability and the like are achieved; a method for synthesizing 2 alpha-methyl-2 beta-(1,2,3- triazole-1- radical) methyl penam-3 alpha-carboxylic acid diphenylcarbinol ester by using 2-triphenyl silicon-1,2,3-triazole is adopted in the fifth step, and the tazobactamsynthesis method is simple and convenient to operate, is safe and reliable, shortens the reaction route and improves the total yield. Compared with the traditional process, the tazobactam synthesis method greatly reduces the production cost and the environment pollution and has greater implementation value and economic benefits.

The invention discloses a preparation method of a three-dimensional layered structure Fe-doped Ni-MOF nano-array (Fe0.1-Ni-MOF/NF) which is grown in situ on foamed nickel and has high regular array. Nickel foam is used as a conductive substrate. The NiFe-LDH nano-array (NiFe-LDH/NF) firstly grows by a hydrothermal method, and then terephthalic acid is used as an organic ligand to convert a NiFe-LDH/NF precursor template to Fe0.1-Ni-MOF/NF by a solvothermal method, and the product is used as an electrocatalyst for water oxidation reaction. The electrocatalyst shows excellent catalytic activity(eta 100mA cm-2=263mV) in 1M KOH electrolyte, which is much better than undoped Ni-MOF/NF material (eta 100mA cm-2=298mV). The invention fully utilizes the doping introduction impurity level to regulate the electronic configuration and induce the synergy effect between metals, and the highly regularly arranged layered structure nano-array reduces the series resistance, exposes more active sites and promotes the diffusion of electrolytes and evolved gases. A novel energy-transduction material with high electrocatalytic activity, good cycle stability, durability and low cost is constructed.

This invention is azotize ferro-vanadium and method for making same. The composition of azotize ferro-vanadium is: vanadium 47-81%, nitrogen 8-16%, iron 4-44%, carbon<=1%, silicon<=1.50%, aluminium<=0.01%, manganese<=0.50%, sulfur<=0.05%, phosphor<=0.05%; the method includes following steps: mixing powderedvanadium compound, carbonaceous reducer and ferrous powder, then adding agglomerant, briquetting, putting them into metallurgical furnace with protective atmosphere when they have been dry to do carbon thermal reduction, nitridation and sintered reaction, the temperature of carbon thermal reduction part is: 900-1200DEG C, the temperature of nitridation part is: 1200DEG C-1350 DEG C, the temperature of sintered reaction part is: 1350DEG C-1490DEG C, the total reaction time is: 2-18 hours. This invention simplifies traditional technique, greatly shortens reaction period, reduces the equipment input and cost of production, the obtained products is of stable quality, high vanadium yield, large density, low fusing point in steel application.

The invention relates to a preparation method of a NiAl intermetallic base solid self-lubricating composite material containing Ti3SiC2 and C binary composite lubrication phase and wild phase TiC. The NiAl intermetallic base solid self-lubricating composite material is prepared from Ni powder, Al powder, Mo powder, Nb powder, Fe powder, B powder and Ti3SiC2 powder, wherein the molar ratio of Ni: Al: Mo: Nb: Fe: B=48: 50: 1: 1: 0.5: 0.02, and the addition quantity of the Ti3SiC2 powder is 5-20 weight percent of the total weight of the Ni powder, the Al powder, the Mo powder, the Nb powder, theFe powder and the B powder. The NiAl/ Ti3SiC2-C/TiC intermetallic base solid self-lubricating composite material synthesized by the method has novel component design (intermetallic matrix+ composite lubrication phase+ wild phase), high density, good tribological properties and stable technological parameters. The preparation process is fast and simple, and the method is easily operated and is suitable for preparing NiAl intermetallic base solid self-lubricating composite materials with high performance.

The invention relates to the field of chemical synthesis, in particular to a method for preparing cabazitaxel. Reaction steps are reduced, a protective group is removed in a mild mode, the reaction period is shortened, and the high-purity cabazitaxel is obtained. The whole preparation method has the advantages of a few reaction steps, light pollution and suitability for industrial production.

A V-N microalloying additive is prepared from vanadate or vanadium oxide, carbon reducing agent, and density intensifier through die pressing to become blocks, loading in high-temp furnace, introducing N2, and reduction reacting which nitrifying. It contains V (77-82%), nitrogen (11-16%) and C (2-7%).

The invention discloses a preparation method of a magnetic nanometer molecular imprinting composite material related to estrogen, comprising the following steps: dissolving bivalent iron salt and trivalent iron salt into water, performing ultrasonic dispersion, heating and regulating the system till being alkali, stirring the system, performing magnetic separation, washing the system till that pH is 6-8, and drying the system; adding ethanol solution, performing heating, stirring and dropping oleic acid, performing magnetic separation, washing the system till that pH is 7.0, and drying the system; adding a dispersant, a polymerization monomer, a functional monomer and a cross linker, and performing ultrasonic dispersion; adding an initiator, performing heating, stirring and magnetic separation, washing the system till that pH is 6-8, and drying the system; adding a composite reaction liquid of a template molecule and amino functional reagent, performing heating, stirring and magnetic separation, washing the system till that pH is 6-8, and drying the system to obtain a target product. The preparation method has the advantages of simple preparation process, controllable magnetic content, controllable functional group proportion and so on, and can arrive at a high enrichment factor when being applied in residual trace phenol environmental estrogens in enrichment drinking water.

The invention provides a method for preparing dopamine-modified hyaluronic acid micelle and belongs to the technical fields of polymer material and natural polymer. The method comprises the steps of introducing dopamine element on a hyaluronic acid main chain by amidation so as to provide certain amphipathy to the hyaluronic acid, so that micelle with the grain size of 100-700nm is formed in water solution by self-assembling. The hyaluronic acid micelle is excellent in biocompatibility, hydrophilicity and viscoelasticity, and can be applied to the fields such as biological materials and hydrophilic colloid. The adhesiveness of the dopamine provides excellent interface property, and the micelle can be applied to the fields such as emulsion, food, cosmetic and the like as emulsifier.

The invention discloses a method for preparing metal magnesium by using dolomite as a raw material, and aims to solve the problems of low reducing efficiency, high energy consumption, long production period and serious pollution existing in the conventional method for preparing the metal magnesium. The method comprises the steps: crushing of dolomites, vacuum low-temperature light calcining and recycling of carbon dioxide, cooling and heat recovery, ball-milling of mixed materials, briquetting of mixed materials, vacuum high-temperature hot reduction, separation of magnesium blocks, and utilization of slag, wherein in the vacuum low-temperature light calcining, the crushed dolomites undergo light calcining in a continuous type vacuum calcining furnace for 1 to 3 hours at the calcining temperature of between 500 and 1,000 DEG C and under the furnace pressure of 10,000 to 60,000Pa, MgCO3 and CaCO3 in the dolomites are decomposed in sequence, the reaction expression is: CaMg(CO3)2=CaCO3+MgO+CO2(gas) and CaCO3=CaO+CO2(gas), and the mixture of carbon dioxide and magnesium oxide and calcium oxide is obtained; and the carbon dioxide which flows in the furnace and heats the dolomites is recycled.

The invention relates to a preparation method of ultrahigh-viscosity sodium carboxymethyl cellulose, which comprises the following steps: by using refined cotton as the main raw material and an ethanol water solution/water mixed solution as a reaction medium, alkalifying, etherifying, washing, carrying out rake drying, baking, crushing and the like to obtain the ultrahigh-viscosity sodium carboxymethyl cellulose. In order to ensure the alkalifying effect, a certain amount of sheet alkali is added during alkalifying to enhance the utilization ratio of acid. The method provided by the invention has the advantages of simple production process, short reaction time, low equipment investment and low raw material consumption; and the sodium carboxymethyl cellulose produced by the method has high viscosity, wherein the viscosity of 1% Brookfield (3# rotor, under the condition of rotation speed 30R) is up to higher than 10000mPa.s.

The invention discloses a preparation method for a cellulose crystal susceptible to re-dispersion after drying, which comprises selection and using for cellulose crystal materials and non-ionic surface active agents; and a preparing and drying processing method for cellulose crystal suspending liquid materials, wherein the cellulose crystal materials comprise different types of cellulose crystals obtained by different cellulose sources and different processing methods; and the non-ionic surface active agents are APG, poly ethylene glycol, and polypropylene glycol. The preparation method comprises the following steps: mixing and stirring one of the non-ionic surface active agents and one of cellulose crystal suspending liquid to obtain the cellulose crystal suspending liquid materials; the cellulose crystal suspending liquid materials are subjected to drying processing by a fluid bed dryer or a spray dryer to obtain granulated, particulate, or powdered cellulose crystals which can disperse in an aqueous phase system quickly; and obtaining a particle size distribution, which can maintain original properties of the cellulose crystals, is similar to that of the original cellulose crystals after re-dispersing. Therefore, the cellulose crystals capable of re-dispersion provide convenience for the storage, the transportation, and the follow-up application.

The invention discloses a method for preparing spherical lithium titanate from inorganic titanium sources. The method comprises the following steps: pulping the titanium precipitate prepared from titanic acid or ilmenite and industrial titanic solution with water, adding a coordinating agent to the pulp according to the molar ratio of the coordinating agent to titanium being (1.0:1)-(20:1), adjusting the pH value to be 7-14 with alkali, then carrying out reaction in a stirred reactor at the temperature of 10-80 DEG C for 5-720min and filtering the reactant to obtain titanium solution; adding lithium sources to the solution according to the molar ratio of lithium to titanium being 4:5; and then carrying out spray drying on the mixed solution to obtain a lithium titanate precursor and calcining the precursor in the inert atmosphere at the temperature of 550-900 DEG C for 1-72 hours to obtain lithium titanate, the cathode material of lithium ion batteries. The method has the characteristics of wide raw material range, simple process flows, low energy consumption, low cost, good product particle size and morphology, high purity and excellent electrochemical property.

The invention relates to a method for preparing an iron modified SBA-15 mesoporous molecular sieve, which comprises the following steps of: 1) adding nonionic surfactant and ferric nitrate nonahydrate into solution prepared from hydrochloric acid and deionized water in a volume ratio of 1 to 10 with pH of about 1, and stirring the solution at the room temperature till the solution is clear and transparent; 2) adding tetraethoxysilane into the mixed solution obtained in the step 1), placing the mixed solution into an ultrasonic pool, acting ultrasonic wave on the mixed solution for 2 hours, adjusting the pH of the mixed solution to between 3 and 4, transferring the mixed solution to a reaction kettle, and hydro-thermally crystallizing the mixed solution for 24 hours at the temperature of 100 DEG C to form the iron modified SBA-15 mesoporous molecular sieve; and 3) filtering the reaction solution obtained in the step 2), repeatedly washing a filtered substance by using water and drying the filtered substance, and calcining the filtered substance for 6 hours at the temperature of 550 DEG C to obtain the SBA-15 mesoporous molecular sieve of which iron ions are high dispersed inside and outside a skeleton. The method reduces the reactive ageing time to 2 hours from 20 hours, does not need to use a mineralizing agent NH4F, greatly shortens the reaction period, and reduces the reaction cost.

The invention relates to an industrial synthesis method for producing absorbent resin. The method comprises the following steps: alkali liquor is used to neutralize acrylic acid; acrylamide is added into the reaction solution, is fully dissolved, is orderly added with starch and a catalyst for reaction at controlled temperature of between 30 and 40 DEG C for 30 to 60 minutes; a foam beater and a polymerizing agent are added into the mixture; the mixture is added into a polymerizing device for polymerization; and the polymerized semi-finished product is subjected to cooling, cutting, drying and crushing to obtain the finished product. The industrial synthesis method has the advantages of simple production process, short reaction period, less energy consumption, long product guarantee period, degradability, no pollution, low input cost and high profit value, and can produce the absorbent resin through self cross linking by utilizing heat released by chemical reaction without adding a cross-linking agent and heating on the basis of not introducing nitrogen at the prior normal pressure.

The preparation technique combined continual reaction rectification and liquid-liquid extraction for methylal comprises: one-time adding the catalyst of toluenesulfonic acid and formaldehyde into reaction kettle as well as methanol from rectification column; controlling the temperatures of kettle and top of reaction rectification device within 50~55Deg and 35~42Deg respectively; then, with glycerin or bicarbinolamine as extractant, taking liquid-liquid extraction to the distillate from tower top with 92% methylal and 6% methanol and 2% water to obtain the methylal on tower top; recovering the extractant and methanol-water mixture for cycle. This invention has yield more than 97% with short reaction period and fast speed.

The invention discloses a production method for manganous/magnesium silicate of chargeable magnesium battery positive pole material, which is the manganous/magnesium silicate of chargeable magnesium battery positive pole material using molten salts as reaction medium and having the characteristics of quickening up reaction speed, shortening reaction cycle, simplifying synthesis course, reducing synthesis cost, small synthesis particle size and symmetrical distribution of the particles. The material exhibits remarkable electrochemical charge and discharge effects, the steady discharge platform works up to 1.6V and 1.1V(vs.Mg/Mg<2+>); on the charge and discharge conditions of C/20 current density, the discharge capacitance can reach 289.3mAh*g<-1>(theoretical capacitance is 92%). In contrast to the relatively ideal positive pole material Mo3S4 of the current chargeable magnesium battery, the manganous/magnesium silicate positive pole material produced by the molten salt process has the advantages of simple production, large capacitance, high discharge voltage platform and the like.

The invention discloses a method for depolymerizing waste PET (polyethylene terephthalate). The method comprises: taking the waste PET as raw material and water as a supercritical medium, and depolymerizing the polyethylene terephthalate in the supercritical state to obtain depolymerization products of terephthalic acid and glycol, wherein the weight ration between the polyethylene terephthalate and the water is between 1:5 and 1:20, the depolymerizing temperature is between 375 and 450 DEG C, the pressure is between 22.12 and 50MPa, and the depolymerizing time is 5 to 60 minutes. The method has the advantages of short reaction period, simple process, high reaction efficiency, unnecessary catalyst and high monomer content of the product.

The invention relates to a rhodococcus ruber and a method for preparing 5-cyanovaleramide by utilizing the same. The strain needs oxygen, does not need power, spores and gram-positive bacteria, is already stored in the Common Microorganism Center of Chinese Microorganism Strain Storage Management Committee and has storage data of Jun. 4, 2009 and a preservation number of CGMCC No.3090. The method for preparing the 5-cyanovaleramide by utilizing the rhodococcus ruber comprises the following steps: (1) culturing seeds; (2) fermenting and culturing; (3) preparing a rhodococcus ruber suspension; (4) preparing a crude product of 5-cyanovaleramide; and (5) purifying the 5-cyanovaleramide. The invention provides a method for generating the 5-cyanovaleramide by selectively hydrolyzing adiponitrile in a rhodococcus ruber region, has high catalytic efficiency, high adiponitrile conversion rate up to 100 percent and 5-cyanovaleramide regioselectivity up to 100 percent, does not generate a side product of adipamide and simplifies the separation purification process of the 5-cyanovaleramide.

The invention discloses an ether type polycarboxylic acid slump retaining agent and a preparation method thereof. The slump retaining agent is prepared by the following steps of: adding methyl allyl polyethenoxy ether, sodium p-styrene sulfonate and an oxidant into a reaction kettle; adding water, mixing and stirring to obtain uniformly mixed solution; controlling the temperature of the obtained mixed solution at 30-60 DEG C; simultaneously dropwise adding solution A and solution B, wherein the solution A is obtained by dissolving acrylic ester and acrylic acid in water, the dropping time of the solution A is controlled to be 3-4 hours, the solution B is obtained by dissolving a reducing agent and a chain transfer in water and the dropping time of the solution B is controlled to be 3.5-4.5 hours; continuously stirring the obtained solution for 1-1.5 hours; adjusting the pH value of the solution to be 7; adding a proper amount of de-ionized water; and discharging to obtain the ether type polycarboxylic acid slump retaining agent. The prepared slump retaining agent is used in cement paste; the cement paste fluidity is not lost or increased within 2 hours; and the concrete slump loss is extremely low by applying the slump retaining agent to concrete.