26 results about "Nitromethane" patented technology

The invention discloses a continuous kettle type nitromethane production process, and relates to the technical field of basic chemical raw material synthesis and flow chemical reaction process control, which comprises the following steps: quantitatively and continuously pumping a temperature-regulated sodium nitrite mixed solution into a raw material mixer in a closed-loop automatic control mode through a variable-frequency feeding pump matched with a mass flow meter; synchronously, quantitatively and continuously pumping dimethyl sulfate into the raw material mixer in a closed-loop automatic control manner by matching a feeding pump with a stop valve and a mass flow meter, and uniformly mixing the two raw materials in the raw material mixer according to the stoichiometric molar ratio of the dimethyl sulfate to the sodium nitrite, according to the tandem type segmented design, each reaction kettle can be subjected to customized temperature field control and heat transfer design specially aiming at the special thermodynamic and dynamic requirements of the reaction stage where the reaction kettle is located, the heat transfer efficiency of the whole system is greatly improved, and due to the fact that reaction heat is taken away timely and accurately, the heat transfer efficiency is greatly improved. And a by-product generation path induced by local abnormal high temperature is effectively restrained.

The invention discloses a phototherapy reagent and a preparation method and application thereof. The preparation method comprises the following steps: 1-[4-(diethylamino) phenyl]-ethane-1-ketone and 4-methoxybenzaldehyde are subjected to a condensation reaction in a NaOH ethanol solution, and a product and nitromethane are subjected to addition; performing condensation and addition on the other groups of raw materials by the same method; cyclizing the two addition products with ammonium acetate, and coordinating with boron trifluoride diethyl etherate to obtain NHM; carrying out substitution reaction on the NHM and sodium nitrite to obtain NOO; and oxidizing NOO by m-chloroperoxybenzoic acid to obtain NNOO. The reagent can target a tumor hypoxia microenvironment, hypoxia monitoring is achieved, NO is released through photostimulation for tumor gas therapy, meanwhile, the secondary amplification photo-thermal therapy effect is achieved, preparation is controllable, diagnosis and treatment are integrated, and the reagent is sensitive, safe and suitable for biomedical research and clinical diagnosis.

The present application provides a kind of nitromethane tail gas treatment method, comprising the following steps: sodium hydroxide or potassium hydroxide aqueous solution and low-grade fatty diol and organic base miscible to form mixed solution after preheating, then nitromethane tail gas is passed into mixed solution and reacts, reaction end product is separated and purified to obtain corresponding sodium nitrite or potassium nitrite product.The present application also provides a kind of nitromethane production method, including the sodium nitrite or hydrogen potassium obtained above as raw material to recycle production nitromethane.The method of the present application solves the problem of nitromethane tail gas treatment, also can turn waste into treasure, reduce production cost, conducive to nitromethane production and environmental protection.

The invention discloses a method for constructing a highly conjugated aromatic ring system from bio-based (Z)-3-hexene-2, 5-diketone, and the method comprises the following steps: preparing a 1, 3-dinitroalkane aromatic compound with high yield from a bio-based aldehyde substance in nitromethane through a nickel-based catalyst, and then carrying out ring opening on the 1, 3-dinitroalkane aromatic compound and electro-catalytic 2, 5-dimethylfuran to prepare the highly conjugated aromatic ring system from the bio-based (Z)-3-hexene-2, 5-diketone and the bio-based (Z)-3-hexene-2, 5-diketone. The high-conjugation biaromatic ring system is constructed through the reaction of 1, 5-diketone; the preparation method has the advantages that the yield is high, the greenization degree is high, and the obtained highly conjugated biaromatic ring system has high bio-based content (gt; 86%), and has a high application value.

The invention relates to the technical field of nitromethane leakage detection, in particular to a nitromethane leakage detection method and device. Comprising the following steps: SS01, presetting a nitromethane leakage detection device, moving the nitromethane leakage detection device to a detection area, starting a system by a microcontroller, resetting a rotating stand to enable a detection system to be aligned with a station, and establishing wireless data connection between a detection probe and the microcontroller; the flow dividing system extracts to-be-detected gas filtered by the filter element, the detection probe comprehensively detects and collects the gas in a composite motion mode, data are transmitted to the microcontroller in real time, and the cleaning brush ring synchronously cleans the detection probe. Through the innovative design of four-station circulating layout, linkage of the rotating stand and the detection system and gas circuit isolation of the flow dividing system, a cooperative and efficient detection mechanism is formed.

The invention discloses an oxidative coupling preparation method of a nitrogen / phosphine double-site conjugated polymer organic positive electrode material and application of the nitrogen / phosphine double-site conjugated polymer organic positive electrode material in an alkali metal-based battery. The nitrogen / phosphine double-site conjugated polymer with a permanent porous structure and a hierarchical network is prepared by enabling a triphenylamine derivative monomer and triphenylphosphine to react for 24-48 hours in an organic solvent (such as chloroform and nitromethane) under the protection of inert gas and the action of a catalyst (such as FeCl3 or AlCl3) through a Scholl oxidative coupling reaction and directly copolymerizing the triphenylamine derivative monomer and the triphenylphosphine in the organic solvent (such as chloroform and nitromethane) at the temperature of 0-30 DEG C, and the nitrogen / phosphine double-site conjugated polymer with the permanent porous structure and the hierarchical network is obtained. A typical embodiment of the present invention is named P (PZ2TPA-TPP). The polymer has high-density nitrogen and phosphorus active sites, triphenylamine and triphenylphosphine units are synchronously introduced into the structure, a difunctional site network for synergistically accelerating anion transmission is formed, and the technical bottlenecks of low ion transmission efficiency, poor rate capability, insufficient cycle stability and the like of a traditional organic positive electrode material are effectively improved. The material can be used for preparing a positive plate, and shows high working voltage (about 3.79 V), high specific capacity (-135mAh g <-1 >), excellent cycling stability (the voltage is not obviously attenuated after 200 times of cycling) and excellent rate capability (the voltage is still kept about 100mAh g <-1 > under 10Ag <-1 >) in a lithium dual-ion battery. After the lithium double-ion total battery is further assembled, under a high-load condition (gt; 2 mg cm <-2 >) shows long cycle life (600 times of cycle stability), high energy density and practical application potential, for example, the material can supply power to a smart phone in real time. The preparation process is simple and convenient, the yield is high (up to 88%), and the method is suitable for alkali metal-based batteries of lithium, sodium, potassium and the like, and has important scientific significance and industrial application value.

The invention relates to the technical field of tromethamine synthesis, in particular to a continuous flow synthesis process of tromethamine. Comprising the following steps: adding nitromethane and a solvent A into a container A to obtain a solution A; adding a depolymerizing agent, a solvent B and paraformaldehyde into a container B to obtain a solution B; the first feeding pump and the second feeding pump respectively convey the solution A and the solution B to a micro-channel reactor at the same time for condensation reaction to obtain condensation reaction liquid; transferring the condensation reaction solution to an acidification kettle, and adding a quenching solution for reaction to obtain a quenching reaction solution; diluting the quenching reaction solution, adding a decolorizing agent, and filtering to obtain a decolorizing reaction solution; adding the decolorization reaction liquid and a solvent C into a hydrogenation reaction system by using a circulating pump, and carrying out hydrogenation reaction under the action of hydrogen and a catalyst to obtain hydrogenation reaction liquid; concentrating the hydrogenation reaction liquid to remove the solvent to obtain a tromethamine crude product, and refining the tromethamine crude product to obtain a tromethamine finished product. The method has the effects of low safety risk, continuous and smooth continuous flow pipeline and high product yield and purity.

The application discloses a method for preparing trimethylolamine by a continuous flow method, and comprises the following steps: mixing polyformaldehyde and alkali to obtain a mixed solution 1; mixing a nitromethane solution and the mixed solution 1 to form a reaction solution, and then introducing the reaction solution into a micro-channel continuous flow reactor to obtain a mixed solution 2 after reaction; adjusting the flow rates of the mixed solution 2 and hydrogen, and then mixing the gas-liquid mixture into a gas-liquid mixer at the inlet of a micro-packed bed continuous flow reactor, passing through a catalyst bed layer of the micro-packed bed continuous flow reactor to react, and then adjusting the temperature through a reactor heat exchange cavity of the micro-packed bed continuous flow reactor to obtain a crude product after reaction, and then performing post-treatment and purification to obtain a trimethylolamine product; and the catalyst comprises a supported Pd catalyst, a supported Ni catalyst or a Raney nickel catalyst. The preparation method of the application enables the solid catalyst to fully contact with the mixed solution 2 and hydrogen, compared with a conventional intermittent hydrogenation preparation method, the reaction time is shortened, the product purity is high, the safety is high, and the method is beneficial to industrialized scale production.

This invention discloses a continuous flow synthesis method for nitromethane. The method includes mixing dimethyl sulfate, nitrite, a catalyst, and water to obtain a mixture; continuously feeding the mixture into a first reactor and reacting it at a first temperature to obtain a first reaction solution; continuously feeding the first reaction solution into a second reactor and reacting it at a second temperature to obtain a second reaction solution; continuously feeding the second reaction solution into a distillation column to obtain crude nitromethane, which is then purified by distillation to obtain the final nitromethane product. Both the first and second reactors are plug flow reactors, and the first temperature is lower than the second temperature. This method provides milder reaction conditions, easier process control, and by refining and precisely controlling the reaction temperatures of the two stages, it reduces the generation of byproducts and energy costs, avoids the safety hazards caused by violent foaming and material surges during the reaction, and significantly improves both process safety and efficiency.

This invention discloses a method for detecting disinfection byproducts in drinking water. By combining gas chromatography-triple quadrupole dynamic multiple reaction monitoring, ion pair information and standard curves containing disinfection byproduct standards are established. The extracted sample solution is tested under the same test conditions, enabling simultaneous extraction and quantitative and qualitative analysis of 34 disinfection byproducts in the sample. The byproducts detected simultaneously include five categories of substances: trihalomethanes, halonitromethanes, haloaldehydes, haloketones, and haloacetonitrs. This greatly increases the variety of disinfection byproducts that can be detected simultaneously and improves the detection efficiency.

This invention discloses a near-infrared photocatalytic coupling method for 2-benzene-1,2,3,4-tetrahydroisoquinoline compounds with nucleophiles. The method uses (MV)Bi₂I₈ type perovskite as a catalyst, wherein the organic portion of the catalyst, MV… 2+ The product is a methyl viologen cation. 2-Benzene-1,2,3,4-tetrahydroisoquinoline compounds are reacted with nucleophiles (dimethyl malonate, nitromethane, ethyl nitrosyl acetate) under light irradiation at room temperature or in air to undergo cross-dehydrogenation coupling reactions to obtain the corresponding product. This invention is simple to operate, operates under mild conditions, and uses readily available catalysts. It successfully achieves cross-dehydrogenation coupling between substrates using only near-infrared light, and yields high product yields.

This invention provides a method for synthesizing milobalin benzylsulfonic acid, comprising the following steps: a chiral enone undergoes a condensation reaction with cyanoacetate in the presence of ammonium acetate to obtain an unsaturated cyano ester; next, the unsaturated cyano ester undergoes a condensation reaction with nitromethane to obtain a nitro ester; the nitro ester is then deesterified at high temperature to obtain a chiral nitro nitrile, which is then reduced to a chiral amino nitrile; subsequently, the chiral amino nitrile is hydrolyzed to obtain the free base of milobalin; finally, the free base of milobalin is salted with benzylsulfonic acid to obtain milobalin benzylsulfonic acid. This invention stereospecifically constructs a chiral cyclobutane quaternary carbon center to obtain a chiral nitro ester with a single stereoconfiguration, avoiding the chiral isomer waste generated by chiral isomer resolution, eliminating the need for chiral column separation or chiral resolution, significantly reducing production costs, and simultaneously avoiding the environmental pollution caused by residual heavy metal titanium in the product and solid waste heavy metal titanium.

The invention discloses a synthetic method of 5-aminolevulinic acid and derivatives thereof, 5-aminolevulinic acid and derivatives thereof and application, and relates to the technical field of chemical synthesis, and the synthetic method comprises the following steps: mixing monoalkyl succinate, an inert solvent and an activating reagent, and carrying out acylation activating reaction to obtain a first intermediate; mixing the first intermediate, nitromethane, an alkaline agent, a molecular sieve and an organic solvent, and carrying out nitro condensation reaction to obtain a second intermediate; and mixing the second intermediate, a solvent and a catalyst, and carrying out catalytic hydrogenation reaction to obtain the 5-aminolevulinic acid and the derivative thereof. By adopting the steps, only three-step reaction is needed from the initial raw material to the target product, the reaction conditions are mild and efficient, the 5-aminolevulinic acid and the derivative thereof prepared by the process are white solids, the chemical purity of the 5-aminolevulinic acid and the derivative thereof can reach more than 96.0% and the yield can reach more than 70% through HPLC (High Performance Liquid Chromatography) analysis, and the requirements of industrial large-scale production are completely met.

The application provides a pyrazine compound and a preparation method and application thereof, a nitryl pyrazine compound and a preparation method and application thereof, and a preparation method of an upatin intermediate, and relates to the technical field of drug synthesis. The pyrazine compound with the structure shown in formula IV is subjected to an addition reaction with nitromethane to obtain a nitryl pyrazine compound with the structure shown in formula III, and then, under the condition of an alkaline reagent, an intramolecular cyclization-aromatization reaction is performed to obtain an upatin intermediate with the structure shown in formula II. Compared with the prior art, the application does not need to use expensive metal catalysts (such as a palladium catalyst) and other expensive silicon reagents, but only needs to use inexpensive and easily available formaldehyde aqueous solution and nitromethane, so that the production cost of the upatin intermediate is greatly reduced; and compared with the use of acetaldehyde gas, the application uses formaldehyde aqueous solution, and the operation is more simple, and the application is more conducive to industrialized production.

The invention belongs to the technical field of chemical solid waste resourceful treatment, and particularly relates to a treatment device and process for solid waste residues in nitromethane production.The treatment device comprises a treatment tank, a bottom supporting tank is fixedly mounted on the lower side of the treatment tank, and a base support is fixedly mounted on the lower end face of the bottom supporting tank; a circulating process water pipeline is fixedly mounted on one side face of the bottom supporting tank body and one side face of the treatment tank, an ultrasonic dissolving area is fixedly mounted on the lower end face of the mixing device, a built-in ceramic membrane filter is fixedly mounted on the lower end face of the ultrasonic dissolving area, and a spiral guide plate reaction channel is fixedly mounted on the lower end face of the built-in ceramic membrane filter. According to the invention, the processes of ultrasonic dissolution, membrane separation, photocatalytic degradation, flash evaporation crystallization, drying, mother liquor circulation and the like are vertically integrated in a single treatment tank, so that the energy consumption and loss of material transfer among traditional multiple devices are eliminated.

The invention belongs to the field of catalysis, and discloses a method for preparing surface methoxyl species by catalyzing dimethyl ether conversion based on an H-ZSM-5 molecular sieve. The method comprises the following steps: by taking an H-ZSM-5 molecular sieve as a catalyst, carrying out reaction on mixed gas of dimethyl ether and nitromethane at 90-120 DEG C under a mild condition, so that the dimethyl ether can be efficiently decomposed into surface methoxy species and methanol. The method disclosed by the invention has the remarkable advantages of simplicity and convenience in operation, mild reaction conditions and the like, provides an innovative solution for controllable preparation and industrial application of surface methoxy species, and has important scientific research value and wide industrial application prospect.

The present invention provides a nitromethane fluorescence determination device, and relates to the technical field of nitromethane fluorescence determination, the nitromethane fluorescence determination device comprises a detection assembly, a material control assembly and a hydraulic assembly, the detection assembly comprises a material box I and a material box II, the bottom of the material box I is provided with a batching assembly, the batching assembly comprises a batching barrel and a raw material barrel, the invention discloses a fluorescence determination method and device for nitromethane, the device comprises a dosing barrel, the bottom of the dosing barrel is provided with a mixing assembly, the mixing assembly comprises a mixing barrel and a detection cylinder, the mixing barrel is provided with a determination assembly, and the determination assembly comprises a fluorescence detector and a sensor. The problems of missed recording, wrong recording, disordered taking, disordered use and the like are greatly reduced, and the device is suitable for rapid routing inspection work of the land.

The invention discloses a green synthesis method for preparing oxime by catalyzing alcohol and nitromethane through metal salt, and belongs to the field of photoelectrocatalysis organic synthesis. In a single-chamber electrolytic cell, in the presence of a metal catalyst and a hydrogen atom transfer reagent, alcohol (I) and nitromethane (II) are used for preparing the oxime compound as shown in the formula (III) at high yield under the photoelectric synergistic effect. According to the invention, nitromethane is used as a nitric oxide free radical precursor, and the oxime compound is prepared through a coupling reaction between alcohol and nitromethane for the first time. The method is applicable to preparation of oxime compounds containing carbonyl and acid-sensitive groups, which cannot be realized by conventional methods. .

The application discloses a nitromethane continuous distillation device, and relates to the technical field of nitromethane separation.The application has the advantages that the distillation device body is provided with an outer cylinder and an inner cylinder connected in sequence from the outside to the inside at the rear end of the distillation device body, a jacket is connected to the outer wall of the outer cylinder, and a hollow roller shaft is rotatably connected to the inner wall of a through hole in the middle of the distillation device body.The device adopts a double heating mode, significantly improves the uniformity of material heating, continuously rotates an auger to push the axial transmission of the material, realizes continuous feeding, continuous distillation and continuous discharging, and the spiral blades rotate synchronously with the inner cylinder to continuously scrape off the impurities on the inner wall of the outer cylinder, so that the heat conduction surface is kept clean and uniform, and the product purity and production stability are improved.The application effectively solves the problems of low intermittent operation efficiency, uneven heating and inner wall scaling of the existing nitromethane distillation device, realizes the continuous production of nitromethane, and has important industrial application value.

The present invention provides a novel method for producing nitromethane. The method for producing nitromethane according to the present invention can provide nitromethane having minimized impurities and a high yield and purity, by controlling the reaction temperature upon carrying out the reaction process.

The present application relates to a kind of method for preparing trimethylolamine in continuous flow method, comprising the following steps: mixing paraformaldehyde and alkali solution, to obtain first mixed solution;The first mixed solution and nitromethane solution are as reaction liquid, the reaction liquid is passed into first continuous flow reactor at 0.1mL / min~1.5mL / min flow rate, reaction is ended to obtain second mixed solution, the reaction temperature in first continuous flow reactor is 20~30 ℃;Second continuous flow reactor is pressurized to 2MPa~6MPa, and the second mixed solution is passed into the second continuous flow reactor at 0.1mL / min~0.6mL / min flow rate, reaction is ended, to obtain the trimethylolamine, the reaction temperature in second continuous flow reactor is 40~80 ℃, the present application is easy to operate, synthesis is efficient, and high safety.

The invention provides a ZSM-22 molecular sieve preparation method, which comprises: mixing a silicon source, an aluminum source, an inorganic alkali source, a template agent, an etching agent and water to form a gel, and carrying out dynamic crystallization, separation, washing, drying and roasting to obtain a ZSM-22 molecular sieve, the etching agent is selected from at least one of isopropanol, 1, 6-hexanediol, lysine, tris (hydroxymethyl) nitromethane and 1, 2, 4-triazole. According to the method for preparing the ZSM-22 molecular sieve, the etching agent is added into the synthesized gel mother liquor, the etching effect is preposed to a molecular sieve precursor or crystal nucleus with the minimum size and is matched with growth, then the axial diameter ratio of the ZSM-22 molecular sieve is greatly reduced, meanwhile, crystallization of the molecular sieve is dynamically adjusted by utilizing the addition-bond breaking dynamic change process, and the yield of the ZSM-22 molecular sieve is improved. The internal structure of the crystal is optimized, and the catalytic performance of the ZSM-22 molecular sieve is greatly improved.

The present application relates to the technical field of aviation fuel, and discloses a high-stability jet aviation alcohol hydrogen fuel and a preparation method thereof, the fuel comprising bio aviation coal, a low-carbon alcohol mixture, adipate ester additives, nitromethane, carbonized poly[cyclotriphosphazene-co-(4,4'-sulfonated diphenol)] nanoparticles and polyisobutylene amine. In the system, rigid nanoparticles and flexible polymer long chains construct a composite steric network at the oil-alcohol interface, which inhibits the thermodynamic coalescence and oswald ripening of microemulsion droplets. The preparation method pumps the pre-cooled alcohol phase into the constant-temperature oil phase, uses the temperature difference thermal stress to cooperate with the flow field high shear force to accelerate the crushing of droplets and the remodeling of the phase interface, and is supplemented by online light transmittance monitoring to determine the microemulsification steady state end point. The present application improves the phase state continuity of the fuel system in a wide temperature range environment, and meets the kinetic pumping requirements of the aviation engine under extremely cold conditions.

The application discloses a kind of gel-like energetic material continuous pushing device and its related system, device and method, the gel-like energetic material can be stably filled in water gap for a long time without shell and connect gap positive and negative electrode.Other ingredients do not contain explosive in dangerous goods item, common formula is the mixture containing nitromethane, aluminum powder, metal oxide, friction sensitivity and impact sensitivity are zero after test of initiating explosive, safety is extremely high.And formula component is not soluble or very difficult to dissolve in water, not fail, not decompose under long-time soaking in water, still can be normally initiated under the action of pulse current.Gel-like energetic material is filled in water gap and can generate fixed amplitude, impulse and energy shock wave under the driving of specific parameter pulse source, with excellent repeatability.Compared with original parameter, water gap discharge greatly improves the amplitude, impulse and energy of shock wave, with great engineering application prospect.

The invention relates to the technical field of nitromethane storage, in particular to a nitromethane storage device. Comprising a rotating frame, the rotating frame is rotationally sleeved with a transmission gear ring, a distance adjusting piece is arranged at the axis position of the rotating frame, the rotating frame and the transmission gear ring are driven by a first motor, the distance adjusting piece is connected with two expanding and supporting rings, and a set of storage modules are arranged on the rotating frame and comprise mounting frames slidably connected to the rotating frame; two connecting rods are hinged to the bottom face of each mounting frame, the other ends of the two connecting rods are hinged to the two expanding and supporting rings correspondingly, rotating cylinders are rotationally connected to the mounting frames, the rotating cylinders are driven through transmission gear rings, storage tanks are clamped in the rotating cylinders, and first measurement and control modules for monitoring the temperature and pressure of inner cavities of the storage tanks are arranged on the storage tanks; and a protective cavity is arranged between the rotary cylinder and the storage tank. According to the invention, an automatic safety prevention and control closed loop which takes the microcontroller as a core and is linked with the double measurement and control modules, the gas tank, the adsorption liquid storage tank, the rotating stand and the spraying system is constructed, and the passive situation of manual disposal is avoided.

A separation and purification method of 2-nitroethanol, including: (a) reacting paraformaldehyde with nitromethane in the presence of a base to obtain a mixture of 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III); and (b) selecting an extraction solvent in which 2-nitroethanol (I), 2-nitro-1,3-propanediol (II) and tris(hydroxymethyl) nitromethane (III) are different in solubility; adding the extraction solvent to the mixture followed by extraction, separation, and vacuum concentration to obtain the 2-nitroethanol (I).