34 results about "Reaction temperature" patented technology

The invention relates to a method for directly preparing propylene from crude methanol, wherein, in an integrated unit for preparing the methanol and preparing the propylene from the methanol, the crude methanol directly enters a multistage adiabatic fixed bed reactor loaded with an acid molecular sieve catalyst without rectification and purification to prepare low carbon olefin with the propyleneas a main component. In the method, steam and circulating hydrocarbon as diluent, and a mixture of the crude methanol and water is used for interstage cold shock to control reaction temperature of the reactor in each stage. The method helps obtain high propylene yield, and obviously reduce investment and energy consumption of the integrated unit for preparing the methanol and preparing the propylene from the methanol.

The invention relates to a catalyst for ternary copolymerization of norbornenes, tetrafluoroethylene and pentenes and a ternary copolymerization method. The catalyst is characterized in that the catalyst is prepared through the following method comprising the steps of: dissolving iron dichloride, a ligand and an alkyl metal compound in a solvent in a dry single-neck glass bottle in an inert gas atmosphere, sealing a bottle mouth through an emulsion pipe, keeping the constant temperature in a water bath at the temperature of 40-50 DEG C for 10-30min, and cooling to obtain an iron complex catalyst. Compared with the prior art, the catalyst provided by the invention is a novel iron complex catalyst which can produce catalytic activity in an nitrogen-protected system at a certain pressure and the temperature of 20-120 DEG C so as to catalyze the ternary copolymerization of the norbornenes with the tetrafluoroethylene and the pentenes, and a product after soaking in methanol is very easy to wash and separate. The catalyst has the characteristics of high copolymer yield, low reaction temperature, low price, easiness in obtainment, high catalytic efficiency and the like.

The invention relates to a low-density high-intensity ceramsite fracturing propping agent and a preparation method thereof. The low-density high-intensity ceramsite fracturing propping agent has a core material body which is composed of the following materials in percentage by weight: 30-40% of bauxite, 10-15% of talcum, 10-12 % of mullite, 12-15% of metakaolin, 6-15% of potassium feldspar, 3-6.5% of titanium dioxide, 1-3% of manganese powder, 3-4.5% of nano calcium carbonate, 2.5-3.5% of iron trioxide and 2.5-3.5% of magnesium orthosilicate; a gel breaker layer is arranged outside the core material body, and the gel breaker layer is sequentially coated with an external coating and a lubricant layer. When in preparation, various materials are firstly ball-milled, sieved and graded, and then matched in different ways; the potassium feldspar and the titanium dioxide both can reduce reaction temperature to a certain extent; the added manganese powder mainly plays a role in catalyzing; the nano calcium carbonate plays a role in reducing density of product; sintering temperature needed by the product is 1250 DEG C; the product is low in density, strong in anti-fracture capacity and high in sphericity; and meanwhile, the production technology is simple and easy to popularize and implement.

The invention relates to a preparation method of florfenicol intermediate, in particular to a preparation method of D-threo-2-(dichloromethyl)-4, 5-dihydro-5-(p-(methylsulfonyl) phenyl)-4-oxazole methanol, which comprises the detailed steps as follows: 100 portions of D-p-methylsulfino phenyl ethyl serinate (I) are dissolved in 500 to 700 portions of methanol; then 24 to 27 portions of potassium borohydride are added; the reaction temperature is between 30 and 50 DEG C and the reaction time is between 4 and 8 hours; 80 to 150 portions of methanol are recycled and 230 to 300 portions of glycerol are added; then acid is used for neutralizing the reaction solution to adjust the pH of the solution to be between 7 and 10; and 42 to 45 portions of dochloroacetonitril are added to generate the D-threo-2-(dichloromethyl)-4, 5-dihydro-5-(p-(methylsulfonyl) phenyl)-4-oxazole methanol (II). The preparation method has the characteristics of few technique steps, simple operation and low cost.

The invention discloses a method for producing isopropylamine, which belongs to the technical field of amine. To solve the problem that the prior isopropylamine industrial production device cannot effectively convert diisopropylamine into the isopropylamine, a reactor for an acetone hydroamination reaction performs the sectional control of the reaction temperature, the reaction temperature of a first section positioned at an inlet of the reactor is between 110 and 150 DEG C, and the reaction temperature of a downstream section is 5 to 30 DEG C higher than that of an upstream section which is adjacent to the downstream section. Along with the gradual reduction of the concentration of acetone along a bed, the reaction temperature is improved section by section, which is favorable for converting the diisopropylamine and isopropanol into the isopropylamine, thereby reducing the circulation of the diisopropylamine and the isopropanol, reducing energy consumption, and preventing the diisopropylamine from being gradually accumulated in a system so as not to need operating a diisopropylamine rectification system with difficult operation. The method is simple, feasible and easy to realize,and has considerable industrial application value and economic benefit.

The invention discloses a preparation method of 2-amino-5-chloropyridine, and belongs to the field of organic chemical synthesis. The method comprises the following steps of using 2-amino-pyridine as a raw material and N-fluoro-N-chlorobenzene sulfonamide as a chlorinating agent, in an organic solvent, using imidazole ionic liquid as a catalyst, and carrying out a reaction, wherein a reaction temperature is 0 to 40 DEG C, and a reaction time is 0.2h to 24h. The method provided by the invention is simple and convenient in preparation process, mild in reaction condition, low in cost and high in product yield.

The invention discloses parallel polymerization synthesis equipment which comprises an elevating mechanism provided with a transition saddle and an elevating pallet. An annular heating seat is arranged on the transition saddle, at least two heating kettles are embedded into the heating seat, and heat supply equipment of different heating kettles have different power and are separately arranged; the heating seat is provided with round holes over the heating kettles, and the round holes and the heating kettles form a flask seat. The upper part of the elevating pallet is connected with a stirring saddle, the lower part of which is provided with stirring axes that have the same quantity as the heating kettles and are connected with stirring paddles at the lower part, and the stirring paddles and the stirring axes are all positioned right above the corresponding heating kettles; and a stirring driving motor is arranged over the stirring saddle. The parallel polymerization synthesis equipment is applicable to stirring and mixing reactants or products with high or low viscosity, can provide multiple reaction temperature and stirring speed in a same reaction period, and is applicable to reaction containers of various types, thereby greatly saving the scientific research time of researchers, reducing labor intensity in scientific research, improving scientific research efficiency, and quickening the development of scientific research.

The invention discloses a method for preparing hydrogen by utilizing waste biomass, and the method comprises the following steps of: firstly, processing the waste biomass into semi-finished product fluid slurry; then, carrying out water vapor gasification treatment on the semi-finished product fluid slurry, thus obtaining crude oil; carrying out supercritical water gasification treatment on the crude oil, thus obtaining crude bio-gas; and finally, carrying out low-temperature transformation treatment on the crude bio-gas, thus obtaining transformed gas. The hydrogen is prepared by two-step gasification and low-temperature transformation, so that the biomass gasification efficiency is high, tar carbon deposit blockage can be avoided, continuous feeding is realized, and the prepared hydrogen is high in purity; furthermore, in the low-temperature transformation treatment, precious metals and rare-earth elements are added on the basis of a copper-zinc-aluminum catalyst, so that the reaction temperature is remarkably reduced, the activity and stability of the catalyst are improved, and the conversion rate of CO is high during the low-temperature transformation treatment.

A technology for reversion of FCC fraction of gasoline and simultaneous production of lower carbon alkene consists of preheating FCC fraction of gasoline to the reaction temperature, then entering the reactor filled with accelerating agent of modified zeolite molecular sieve to perform gasoline reversion reaction, cooling the reaction product to apply gas-liquid separation, in which the liquid product is modified gasoline and the lower carbon alkene product is obtained by separating gas product. The accelerating agent of modified zeolite molecular sieve is obtained by processing the zeolite molecular sieve at 600-850 DEG C with aqueous vapor for 1-24 hours. The invention has advantages that it can not only solve the problem of reduction of alkenes from FCC gasoline but also can substantially increase the product with a high added value including ethane and propylene, and the economic process technology is good.

The invention relates to a nickel-containing high-cobalt sulfide leaching technology. A leaching liquor rich in metal cobalt obtained through atmospheric pressure preheating and pressure leaching can directly enter a cobalt production system. The technology comprises the following technical steps of: (1) slurrying minerals in 10-20 g/l dilute acid solution, controlling the ratio of dilute acid volume to material mass at 6:1, and controlling slurrying temperature at 40-50 DEG C, slurrying time at 2-3 h and the concentration of slurrying end point acid at 5-15 g/l; (2) controlling the temperature of atmospheric pressure preheating at 80-85 DEG C; (3) controlling pressure leaching, controlling the ratio of dilute acid volume to material mass at 6:1, reaction temperature at 145-165 DEG C, and leaching partial pressure oxygen at 0.20-0.25 Mpa and reaction time at 6-8 h. In the invention, a nickel and cobalt sulfate solution containing more than 50 g/l cobalt is obtained, i.e. more than 98% of Ni and Co in the nickel-containing high-cobalt sulfide material is leached out to enter the solution.

The invention discloses a method for catalytic synthesis of dichloropropanol by hydrogen chloride-containing industrial waste gas and glycerol. The method synthesizes dichloropropanol by using hydrogen chloride-containing industrial waste gas and glycerol through a hydrochlorination reaction under the action of a catalyst; wherein the catalyst is zinc acetate or zinc adipate; the reaction temperature is 100-120 DEG C, and the reaction is performed for 72-96 hours under normal pressure. The invention adopts hydrogen chloride-containing industrial waste gas as a raw material, has the benefits of both economy and environmental protection.

The invention discloses a preparation process of a leak protection plugging agent along with drilling based on the control of monomer concentration. The preparation process comprises the following steps: (a) purifying AM (acrylamide) and AMPS (2-acrylamido-2-methyl propane sulfonic acid) for later use; (b) weighing AA (acrylic acid), hydrolyzing and transferring into a reactor in a super constant-temperature water bath; (c) adding a certain amount of cross-linking agent; (d) adding AM and AMPS solutions, and regulating the pH value of a reaction system to 7, wherein the monomer concentration is 14.3%-18.2% by weight; (e) introducing inert gas for deoxygenation, stirring and adding an initiator; and (f) regulating the temperature to reaction temperature, and performing polymerization reaction for a certain period of time to get a target product. According to the preparation process disclosed by the invention, the leak protection plugging agent along with drilling can be successfully prepared by controlling the monomer concentration in reaction process, the preparation process further has the advantages of high production efficiency, simple production process, simplicity in operation and capability of greatly reducing the production cost, various performances of the produced leak protection plugging agent along with drilling are far better than those of an existing product, and the leak protection plugging agent along with drilling is further conductive to field well leakage treatment.

The technical problem to be solved by the invention is to provide a preparation method for a catalyst for preparing chloroethylene via ethane oxychlorination. The catalyst contains rare-earth elements, alkali metal elements, iron element, tin element and titanium dioxide, and is applied to a fixed bed reactor; the preparation method for the catalyst is simple in process, low in reaction temperature, and reduced in energy consumption; air is used as a raw material gas, so that the cost is low; and the prepared catalyst has good catalytic activity while being applied to a reaction for preparing chloroethylene via ethane oxychlorination, the conversion rate of ethane is 80-100%, and the selectivity of chloroethylene is 40-68%.

The invention discloses a method for preparing coarse granularity chromium carbide powder capable of simplifying the process, saving the energy consumption, improving the rate of qualified products ina milling process and well meeting requirements of preparation of wear-resistant, corrosion-resistant, high-temperature oxidation resistant novel materials in industries such as hard-face materials,flux-cored wires, high temperature alloys and the like. The method comprises the following steps: burdening chromium sesquioxide powder and carbon, and adding an adhesive to be uniformly mixed; molding with a press after uniform mixing; placing the molded material block in a high-temperature vacuum induction heating furnace graphite crucible, vacuumizing, performing power-on heating and raising the temperature, and maintaining the vacuum degree to be within 200-400Pa; carrying out a vacuum carbonation reaction between the chromium sesquioxide powder and carbon to produce chromium carbide, andcontrolling the carbonation reaction temperature to be 1350-1550 DEG C, wherein the carbonation reaction time is 8-15 hours; enabling the vacuum degree to be less than 100Pa, filling the furnace withargon after the carbonation reaction is completed, controlling the pressure in the furnace to be 40-80kPa, and increasing the heating power to melt the chromium carbide sintered body so as to obtain achromium carbide ingot; crushing the chromium carbide ingot into particles with the granularity of less than 10mm by using a mechanical method, milling by an impact crusher, and passing through a 60-mesh sieve, thereby obtaining the coarse granularity chromium carbide powder.

The invention discloses a catalyst-based chlorinated neopentane preparation technology which is characterized in that a addition reaction is carried out on isoamylene and 36% of hydrochloric acid (in mass percent) under the condition of zinc chloride, the molar ratio of the zinc chloride to the isoamylene is 3:500-6:500, the molar ratio of the isoamylene to hydrochloric acid is 1:1.1-1:1.3, the reaction temperature is 5+/-1 DEG C, and the reaction time is 4-5 hours. The catalyst-based chlorinated neopentane preparation technology has the beneficial effects of having simple technology, being convenient to prepare, easy to realize and short in reaction time, having less addition side reaction, high product content and yield, effectively solving the problem that high content pentane chloride cannot be produced if phosphorous acid is not coproduced, and being considerable in economic benefit.

The invention relates to a preparation method of top-grade pure nickelous chloride, which comprises the following steps: (1) reaction between nickelous carbonate and hydrochloric acid: putting nickelous carbonate in a glass beaker, heating to 65 DEG C, slowly adding hydrochloric acid (the specific gravity is 1.18) while continuously stirring and controlling the reaction temperature at 75 DEG C, stopping adding the hydrochloric acid when the pH value is 5, standing for 20 minutes, and filtering to obtain a solution A; and (2) preparation of top-grade pure nickelous chloride by concentrating: concentrating the solution A obtained in the step (1) to 20 degrees Be while controlling the temperature at 240-260 DEG C, stopping concentrating, cooling, and carrying out suction filtration to precipitate a crystal, thereby obtaining the top-grade pure nickelous chloride. The preparation method has the advantages of simple processing steps, controllable operation steps, advanced technique and high production efficiency. The prepared product has the advantages of high purity and low impurity content, and satisfies the demands of high-end technology.

The invention discloses a method for controlling the terminal by using chlorine trifluoride to etch a polysilicon growth furnace, and at least a temperature detecting device is arranged inside the polysilicon growth furnace. The method comprises the following steps of: firstly, setting a reaction temperature and a warning temperature inside the polysilicon growth furnace, introducing chlorine trifluoride gas to the inside of the polysilicon growth furnace, and continuously introducing the gas to a pre-etching time; and secondly, monitoring the temperature detecting device inside the polysilicon growth furnace, and stopping introducing the gas after continuously passing the etching time when the temperature inside the polysilicon growth furnace increases from the warning temperature and falls back to the warning temperature. The method can be adopted to discover the reaction terminal of the chlorine trifluoride and the polysilicon, thereby avoiding waste of the chlorine trifluoride gas.

The invention discloses a preparation method of a Ni-doped stannic oxide formaldehyde sensitive ternary composite material based on a ZIF-8 metal organic framework template as well as a product and application of the Ni-doped stannic oxide formaldehyde sensitive ternary composite material. According to the method, the ZIF-8 MOF material is used as a crystallization template, thiourea is decomposedunder an ethylene glycol solvothermal condition to provide S2-, and SnS2 and NiS precursors are generated; the Ni-doped SnO2 formaldehyde sensitive ternary composite material based on the ZIF-8 metalorganic framework template is prepared by regulating and controlling conditions such as precursor roasting temperature and roasting time, ZIF-8 is used as a template, so that the specific surface area of the prepared composite material can be greatly increased, and meanwhile, Zn and Ni are doped, so that the response value and selectivity of SnO2 to formaldehyde gas are further improved; the solvothermal preparation method is simple, the reaction temperature is low, follow-up treatment is not needed, and the SnO2/NiO@ZIF-8 ternary composite material prepared by the method can be used for formaldehyde gas sensors and the like.

The invention discloses a preparation method of a dye. The dye is 3,3'-[(9,10-dihydro-9,10-dioxo-1,4-anthryl-di-yl)diimino]bis[N-cyclohexyl-2,4,6-trimethyl]benzenesulfonamide. The target product is prepared through a reaction of solvent blue 104 and chlorosulfonic acid as initial raw materials. Thionyl chloride adopted in the invention has little influence on the reaction and has large influence on the quality of the product; and the reaction temperature and the water washing temperature are controlled in the reaction in order to realize no stickiness or caking of the target product.

The invention relates to a method for preparing 2, 4-dinitrobromobenzene by bromobenzene, which comprises the following steps: adding metered bromobenzene and water into a reactor; heating to the temperature of 80 DEG C and beginning to drip mixed acid of nitric acid and sulphuric acid; controlling reaction temperature at 80 to 100 DEG C and reaction time for 1.5 to 2.5 hours; cooling, filtering,washing by water and drying the reactant to obtain a light yellow solid crude product; and recrystallizing the crude product by ethanol and drying the crude product to obtain the pure product, wherein the productive rate of the pure product is 91.0 to 97.0 percent and the purity is more than than 99 percent. The method has the advantages of simple operation, easy separation and purification for the products, high yield, low cost, little environment pollution, and the like.

The invention provides a spiro[cyclopropane-1, 2'-indene]-1', 3'-diketone derivative and a synthesis method thereof, and belongs to the technical field of organic synthesis of medical intermediates. The method comprises the following steps: adding a proper solvent and a proper alkali into a container filled with a substituted 2-ethylidene-1H-indene-1, 3 (2H)-diketone compound and a substituted sulfur ylide compound, stirring at a proper reaction temperature, filtering after the reaction is finished, adding water or a saturated salt aqueous solution into the filtrate, extracting with an organic solvent, carrying out drying, carrying out reduced pressure distillation concentration to remove the solvent, and carrying out column chromatography separation on the crude product to obtain the target product spiro[cyclopropane-1, 2'-indene]-1', 3'-diketone derivative.The method has the advantages of being efficient in reaction, convenient and rapid, wide in substrate adaptability, high in diastereoselectivity, high in yield and the like and has good industrial application prospects.

The invention relates to the technical field of gene engineering, in particular to a proline protease mutant and application thereof. The proline protein mutant screened by a directed evolution technology has an optimal reaction pH value of 4.0, an optimal reaction temperature of 55 DEG C, can keep 80% or above of the enzyme activity in the temperature range of 45 to 60 DEG C, and has remarkably-higher heat resistance than a wild type. The mutant can be widely applied to beer production, and can remarkably lower the turbidity of beer.