22 results about "Nitroguanidine" patented technology

The invention discloses a fermentation process for shortening a fermentation period and efficiently synthesizing Ectoine. The fermentation process comprises the following steps: screening and activating high-yield strains, preparing a fermentation culture medium, performing fermentation culture, performing sectional dissolved oxygen regulation and control, performing double-stage pH dynamic regulation and control, performing carbon-nitrogen ratio dynamic regulation based on metabolic flow analysis, performing osmotic pressure gradient induction in the later stage of fermentation, and extracting and purifying a product. According to the fermentation process for shortening the fermentation period and efficiently synthesizing the Ectoin, the expression quantity of key enzymes for synthesizing the Ectoin is increased by 80% or above compared with that of an original strain through the Halomonassp.ECT-09 strain bred through ultraviolet-nitrosoguanidine compound mutation, the basic yield reaches 35 g / L, a foundation is laid for high yield, and the method is suitable for industrial production. A glucose-trehalose mixed carbon source and a yeast extract-ammonium nitrate mixed nitrogen source are adopted, and an L-aspartic acid-L-asparagine mixed precursor is added, so that the metabolic pathway is shortened, and the loss of an intermediate product is reduced.

The invention discloses a method for determining clothianidin and metabolite residues of clothianidin in soil. The method comprises the following steps: step 1, preparing a clothianidin standard stock solution and a standard stock solution of metabolites (Z)-1-methylene-2-nitroguanidine and (2-chlorothiazol-5-y1) metyl)-3-metyl guanidine, and preparing the clothianidin standard stock solution and the standard stock solution of the metabolites (Z)-1-methylene-2-nitroguanidine and (2-chlorothiazol-5-y1) metyl-3-metyl guanidine; 2, preparing a solvent mixed standard working solution according to the standard stock solution in the step 1; 3, the solvent mixed standard working solution is added into the soil blank extracting solution, and a matrix mixed standard working solution is prepared; and 4, weighing a soil sample to be detected, carrying out pretreatment, and detecting by adopting a liquid chromatography-tandem mass spectrometry method. According to the technical scheme provided by the invention, the residual quantity of the clothianidin and the metabolites (Z)-1-methyl-2-nitroguanine and the residual quantity of the 1-((2-chlorothiazol-5-y1)-3-methylguanine of the clothianidin in the soil can be rapidly, simply, conveniently and accurately measured.

A grinding device for nitroguanidine production belongs to the field of devices for nitroguanidine production and comprises a bottom plate assembly, a containing unit, a grinding unit, a protection unit and a filtering unit, the containing unit is clamped at the upper end of the bottom plate assembly, the bottom plate assembly is fixedly connected with the grinding unit, the grinding unit is used in cooperation with the containing unit, and the filtering unit is used in cooperation with the grinding unit. The protection unit is fixedly connected with the bottom plate assembly, and the bottom plate assembly is fixedly connected with the filtering unit. The problems that in the background technology, an existing grinding device is simple in structure and poor in protection performance, nitroguanidine is not stable in chemical property, the danger of explosion is generated due to the fact that the nitroguanidine is prone to being affected by the temperature generated by friction during grinding, and dust generated during grinding can harm operators can be solved.

The invention discloses a method for realizing continuous synthesis and crystallization control of nitroguanidine by using a continuous flow multi-stage stirring reactor. The method comprises the following steps: weighing perfluorinated sulfonic acid resin, placing the perfluorinated sulfonic acid resin in a catalyst cage, and mounting the catalyst cage in the continuous flow multi-stage stirring reactor; setting the temperature of a reaction section to be 20-50 DEG C and the temperature of a crystallization section to be-20-10 DEG C; introducing concentrated sulfuric acid in advance to fill an internal channel of the continuous flow multi-stage stirring reactor; guanidine nitrate and concentrated sulfuric acid are premixed and then introduced into the reactor, and the retention time of a reaction section is 0.5-10 min; water is introduced into the crystallization section, and the standing time in the crystallization section is 1-30 min; and collecting a reaction product solution, washing with cold water, and filtering. The continuous synthesis of the nitroguanidine prepared by the sulfuric acid method is realized, the mass and heat transfer efficiency is greatly improved, the reaction time is greatly shortened, the product yield is greatly improved, and the maximum yield of the nitroguanidine is 98%.

The utility model relates to the technical field of synthesis of pesticide intermediates, and provides supergravity hydrolysis equipment for continuously preparing nitroguanidine, which comprises a supporting seat, supergravity equipment mounted at the top end of the supporting seat, a water inlet pump mounted at the top end of the supporting seat, and a frozen brine adjusting valve mounted at the top end of the supergravity equipment. A screw conveyor and a joint control mechanism are mounted at the bottom end of the supporting seat, and the joint control mechanism is arranged at the top end of the supporting seat and comprises a peristaltic pump; continuous production of nitroguanidine is achieved through an automatic control system, frequent manual operation is not needed, the production efficiency is greatly improved, accurate control is achieved, the system can accurately control the mixing proportion of nitroguanidine sulfate and primary water and the hydrolysis and crystallization temperature, the stability and consistency of product quality are ensured, and the production efficiency is improved. Energy conservation and emission reduction are achieved, and the mass transfer and heat transfer processes are enhanced through the application of the supergravity technology, so that the hydrolysis reaction is more efficient.

The invention discloses a methyl nitroguanidine wastewater ultralow-temperature MVR coupling reverse Carnot cycle zero-discharge treatment method, and relates to the technical field of methyl nitroguanidine wastewater treatment.The methyl nitroguanidine wastewater ultralow-temperature MVR coupling reverse Carnot cycle zero-discharge treatment method comprises the following steps that firstly, after methyl nitroguanidine wastewater enters a regulating reservoir to be homogenized and homogenized, floating oil is removed through an oil removal device, suspended matter is removed through a multi-medium filter, and a mixed solution is obtained; volatile organic compounds are removed by the air stripping device, and the organic compounds are degraded by the ozone catalytic oxidation-biological aerated filter; according to the ultralow-temperature MVR coupled reverse Carnot cycle zero-emission treatment method for the methyl nitroguanidine wastewater, organic matters and salts in the methyl nitroguanidine wastewater are thoroughly separated through a coupling process of ultralow-temperature MVR evaporation concentration and reverse Carnot cycle DTB crystallization, the targets of complete resource utilization and zero emission of the wastewater are achieved, no secondary pollution is generated in the whole treatment process, and the method is suitable for industrial production. The treatment effect is stable and reliable.

The invention discloses a method for realizing one-step continuous synthesis and crystallization control of nitroguanidine by acoustic resonance enhancement, which comprises the following steps of: 1, purging the interior of a whole reactor by using inert gas, and introducing concentrated nitric acid and the inert gas in advance; 2, starting an acoustic resonance reaction platform, and adjusting the resonance frequency and the acceleration of the acoustic resonance reaction platform; 3, guanidine nitrate and nitric acid are premixed and then introduced into the continuous reactor, and meanwhile inert gas is controlled to be introduced into the continuous reactor; and 4, collecting a reaction product, washing with cold water, and filtering. According to the method, the mass transfer and heat transfer efficiency is greatly improved, the reaction time is greatly shortened, the product yield is greatly improved, and the highest yield of nitroguanidine is 98%; by adjusting the resonant frequency and the acceleration, the granularity of the product can be accurately controlled, and the granularity requirement of the industry is met.

The invention relates to a preparation method of high-yield oxadiazine. Efficient synthesis is realized through cyclic utilization of concentrated mother liquor and collaborative optimization of key reaction parameters. Specifically, methyl nitroguanidine and paraformaldehyde serve as raw materials and react at the temperature of 70-95 DEG C under the catalysis of sulfuric acid, reaction filtrate is collected to serve as mother liquor to be treated into clear liquid water and concentrated mother liquor, the concentrated mother liquor and the clear liquid water in a certain proportion are mechanically applied to replace a pure water solvent, filtrate generated through mechanical application is collected to be continuously treated and mechanically applied, and mother liquor recycling is achieved. According to the method, the product yield is up to 93%, the purity is greater than or equal to 99%, the reaction time can be greatly shortened, the mother liquor is recycled to reduce the generation of waste liquid by 60% or above, and the use of high-risk reagents such as dimethyl sulfate is avoided. The method is suitable for large-scale production of thiamethoxam insecticide intermediates, has significant cost-reducing and synergistic potential, and provides a high-benefit solution for the green pesticide industry.

The invention relates to the technical field of preparation of fine chemical intermediates, in particular to a method for preparing nitroguanidine by a continuous static tubular reaction process, which comprises the following steps: pumping a sulfuric acid solution in a batching tank into a static tubular reactor; the guanidine nitrate in the feeding hopper is pushed to a static tubular reactor through a solid feeder installed at an output port of the feeding hopper, and the mass ratio of the sulfuric acid solution to the guanidine nitrate is controlled to be 1.0: (1.0-5.0); uniformly mixing a sulfuric acid solution and guanidine nitrate through a high-shear pump, and conveying the mixture to a reaction section of the static tubular reactor for reaction; conveying a reaction product into a hydrolysis kettle, and sequentially carrying out hydrolysis and preliminary cooling treatment; and conveying the initial product into a crystallization mechanism for cooling crystallization, and carrying out filtering centrifugal treatment and drying treatment to obtain a target nitroguanidine product. According to the method, high-efficiency, safe and continuous nitroguanidine production is realized, and the purity and quality of the target product nitroguanidine are also effectively improved.

The invention discloses a nitroguanidine spherical crystal and a preparation method thereof.The preparation method comprises the following steps that under the stirring condition, an additive is added into a nitroguanidine saturated water solution, the temperature is kept at 55-70 DEG C for 30-60 min, then cooling crystallization is conducted, and the nitroguanidine spherical crystal is obtained; the additive is a polyacrylic acid polymer and / or sodium carboxymethyl cellulose. According to the preparation method, the additive and cooling crystallization are matched to obtain the nitroguanidine spherical crystal, and the spherical crystal product is good in degree of sphericity, uniform in particle and good in flowability; the crystallization process only relates to a single water solvent, mother liquor can be recycled, the method is green and environment-friendly, the process is simple, and industrial large-scale production and application are facilitated.

The utility model discloses a continuous shearing device for superfine nitroguanidine, and relates to the technical field of chemical equipment, the device comprises a stirring batching tank, a first material conveying pipeline, a material control valve, a material flow detector, a material discharge pipeline, a shearing mechanism and a control device; the shearing mechanism comprises a first-stage spiral stirring shearing machine, a second-stage spiral stirring shearing machine, a third-stage spiral stirring shearing machine, a first three-way valve, a second three-way valve and a third three-way valve; each of the first-stage spiral stirring shearing machine, the second-stage spiral stirring shearing machine and the third-stage spiral stirring shearing machine comprises a spiral stirring blade, a stirring shaft, a driving mechanism and a stirring tank; a second outlet end of the first three-way valve is connected with an input end of the material discharge pipeline; a second outlet end of the second three-way valve is connected with an input end of the material discharge pipeline; the control device comprises a frequency converter and a control mechanism. By means of the arrangement, the shearing efficiency is high, the reaction process is easy to control, continuous feeding and discharging can be achieved, and meanwhile the product particle size can be selected in multiple modes.

The invention relates to the field of adhesive films, in particular to an adhesive film easy to disassemble, a preparation method of the adhesive film easy to disassemble, a photovoltaic module and a disassembling method of a retired photovoltaic module. The easy-to-disassemble photovoltaic module adhesive film provided by the invention is prepared from the following raw materials: resin, a cross-linking agent TB, a cross-linking agent TA, an assistant cross-linking agent, a coupling agent and a foaming agent which are matched according to a certain proportion, wherein the foaming agent is at least one of a foaming agent ADC, a foaming agent H, nitroguanidine, a foaming agent RA and a foaming agent THT; the cross-linking agent TB is tert-butyl peroxide carbonic acid-2-ethyl hexyl ester; the cross-linking agent TA is peroxide (2-ethylhexyl) tert-amyl carbonate. The easy-to-disassemble adhesive film disclosed by the invention can be used for controlling failure after the photovoltaic module is decommissioned, so that the stripping difficulty of module glass and a battery piece is reduced, and the recovery efficiency is improved.

The application discloses a kind of nitro guanidine continuity preparation device and process, the bottom end inner wall of the pretreatment mechanism is connected with waste outlet, and first solenoid valve is arranged on waste outlet, and the bottom end of pretreatment mechanism is provided with mixing mechanism, and the bottom end outer wall of mixing mechanism is fixed with underframe;The mixing mechanism includes mixing bin, and the inner wall of one side of mixing bin is closely connected with second conveying pipe, and the top inner wall of second conveying pipe is connected with powder storage bin by first conveying pipe, and one end of second conveying pipe is closely connected with air blower, and the inner wall of mixing bin is provided with baffle above second conveying pipe, and frequency adjusting mechanism is simultaneously provided on second conveying pipe and first conveying pipe;The top inner wall center position of the mixing bin is provided with movable connecting piece, and the nitro guanidine continuity preparation device and process disclosed in the application can better realize the continuity preparation of nitro guanidine and effectively improve the preparation efficiency.

The present application relates to a kind of low-temperature preparation methods of phosphating solution for improving the corrosion resistance of steel surface phosphating film, specifically is the deionized water is cooled to 10-15 DEG C by water bath;Phosphoric acid, phosphate, nitrate, nitroguanidine and organic acid are sequentially dissolved in deionized water in order, then cooled to 1-5 DEG C, and maintain more than 20 min;Phosphating solution is heated to the operating temperature required by phosphating process.The present application method does not need to change the specific composition of phosphating solution, also does not need to adjust the temperature, time and other process conditions of phosphating process, only needs to ensure specific low-temperature conditions and the adding order of chemical reagent when preparing phosphating solution, can form thicker corrosion-resistant film layer on the surface of steel parts, and while greatly improving the stability of plating solution, also can maintain higher plating speed, thereby effectively control production cost and production efficiency.

The invention discloses a preparation method and application of a core-shell nitroguanidine propellant based on a coaxial electrostatic spraying technology. The preparation method comprises the following steps: dissolving nitroguanidine in a polar solvent to form a core layer solution; dissolving an insensitive high polymer material or a high-energy binder in a polar solvent to form a shell solution; a solution (an inner needle conveys a core layer solution and an outer needle conveys a shell layer solution) is sucked into an injector with a coaxial needle head, is fixed on an electrostatic sprayer and is received by an aluminum foil baffle, a positive electrode is connected to the needle head of the injector, a negative electrode is connected to the aluminum foil baffle, parameters are adjusted, and the solution forms stable spray with a taper angle of 20-60 degrees at a nozzle of the needle head; and atomizing in a high-voltage electrostatic field to obtain the nitroguanidine propellant with the core-shell structure. According to the nitroguanidine propellant with the core-shell structure, a core layer is high-energy nitroguanidine, a shell layer is an insensitive polymer or an energetic binder, and collaborative optimization of sensitivity reduction and energy release can be achieved; the shell layer can form a microporous structure by controlling the volatilization rate of the solvent, so that the combustion efficiency of the propellant powder is improved.

This invention discloses an iron-carbon micro-electrolysis filler for the degradation of nitroguanidine wastewater and its preparation method. It is prepared using red mud as the iron source, waste oil as the carbon source, and potassium hydroxide as the pore-forming agent. This invention utilizes strong acid to etch the red mud, extracting iron from it. Adjusting the pH of the leachate yields high-purity Fe(OH)3, which is then decomposed into Fe2O3 at high temperature and subsequently carbothermally reduced to zero-valent iron. This avoids the silicon and aluminum in the red mud coating the zero-valent iron, thus preventing it from affecting the micro-electrolysis effect. The zero-valent iron has good contact with the carbon material, effectively forming a galvanic cell. Using liquid waste oil and organic flocculants as the carbon material and reducing agent sources increases the contact between the carbon material and iron oxide, improving the reduction efficiency. KOH etching of the carbon material forms channels, preparing a porous composite material that enhances the adsorption and enrichment of pollutants. Compared with existing red mud-based iron-carbon micro-electrolysis materials, this method is simpler, lower in cost, and easier to scale up.

The invention relates to the technical field of chemical engineering, in particular to a method for synthesizing aminonitroguanidine, which comprises the following steps: S1, adding recycled hydroxylamine into an operation cylinder, adding nitroguanidine, uniformly stirring, adding hydroxylamine, and controlling the adding time of hydroxylamine to be 5-6 hours; s2, heating the stirred raw materials to 60 DEG C for reaction, keeping the temperature and refluxing for 6 hours, cooling to 20 DEG C after the reaction is completed, and then filtering and washing to obtain an amino nitroguanidine crude product; and S3, adding the crude aminonitroguanidine product into the pulping tank, adding clear water, uniformly stirring, and centrifuging in a centrifugal machine to obtain a finished aminonitroguanidine product. According to the preparation method, the nitroguanidine falls into each position of the operation cylinder, so that the subsequent stirring speed is increased, the problem that the nitroguanidine can only be stacked at one position when being put in the past is solved, meanwhile, the content of the aminonitroguanidine is increased to 99%, the yield of the aminonitroguanidine is increased to 90%, and the preparation method is safe, environmentally friendly and suitable for industrial production.

The invention discloses a selective desulfurizer and application thereof, the total mass of the selective desulfurizer is 100%, and the selective desulfurizer comprises: 5-35 wt% of s-triazine and derivatives thereof; 0.1 to 5 weight percent of nitroguanidine and a water-soluble organic alkali compound; and the balance of water. Wherein the content of nitroguanidine is greater than 0, and the content of the water-soluble organic alkali compound is greater than 0. The desulfurizer can efficiently reduce the content of low-concentration sulfur in fuel gas, has high selectivity under the condition that the desulfurizer contains acid gas carbon dioxide, and reduces the content of hydrogen sulfide in the desulfurized gas to 2 mg / Nm < 3 > or below.

The present invention discloses a continuous nitroguanidine production system and process, comprising a concentrated nitric acid storage tank, a solid feeder, a mixing kettle, a transfer kettle, a microchannel reaction assembly, a dilute nitric acid storage tank, a dilution crystallization kettle, a wastewater receiving tank, a washing kettle, and a smoke absorption device; the concentrated nitric acid storage tank and the solid feeder are both connected to the mixing kettle, the discharge port of the mixing kettle is connected to the feed port of the transfer kettle, the transfer kettle is connected to the dilution crystallization kettle via the microchannel reaction assembly, the feed port and water inlet of the dilution crystallization kettle are respectively connected to the dilute nitric acid storage tank and the wastewater receiving tank, the discharge port of the dilution crystallization kettle is connected to an industrial centrifuge, and the filtrate outlet of the industrial centrifuge is connected to the waste acid receiving tank. The present invention provides a continuous nitroguanidine production system capable of preparing 25% aqueous nitroguanidine, which uses 50% dilute nitric acid for crystallization, undergoes multiple water washing treatments and centrifugal dehydration to obtain high-purity nitroguanidine and byproducts, and the byproducts are reused as raw materials to achieve zero waste liquid, no waste gas, and no solid waste.

The present invention relates to the technical field of insecticides, and specifically discloses a synthesis process of clothianidin. The specific process includes the following steps: Synthesis: Add water into a reaction kettle, then put nitroguanidine and monomethylamine solution, and slowly raise the temperature of the reaction kettle to 40-43 °C and keep it warm for 1.5-2 h. After the heat preservation is completed, when the reaction solution is sampled and analyzed without nitroguanidine, continue the heat preservation reaction for 0.5 h, and then make the clothianidin filter cake through neutralization, filtration, recrystallization, centrifugation, drying, substitution, filtration, desolvation, crystallization, centrifugation and drying and packaging of the materials. The present invention obtains methylguanidine by the processes of synthesis, neutralization, filtration, recrystallization, centrifugation and drying of water, synthesis mother liquor, nitroguanidine and monomethylamine solution, and then uses carbon tetrachloride, methylguanidine, potassium carbonate, tetrabutylammonium bromide and dichloromethylthiophene as solvents for substitution reaction. After the reaction, clothianidin is prepared through filtration, desolvation, crystallization, centrifugation and drying processes, thus opening up a new synthesis method.

The present invention discloses a process and device for continuously preparing ultrafine nitroguanidine. By adopting the supergravity technology, ultrafine nitroguanidine is prepared in one step during the acid solution precipitation crystallization process of nitroguanidine. An impact flow - rotating packing bed is used as the crystallization device. Using nitroguanidine acid solution and water as raw materials, through primary mixing and explosive nucleation, the crystal nuclei of nitroguanidine are formed and grow rapidly, shear - controlled forming is carried out for crystal form transformation and growth control, crystal form optimization and regrowth are carried out for crystal form improvement and further growth to increase the yield, and through a post - treatment process, ultrafine nitroguanidine is obtained. Ultrafine nitroguanidine with a Fisher average particle size of 2 - 6 μm and uniform particle size is continuously prepared with a small volume, short residence time, and wide operation range. The present invention solves the problems of long process flow, high energy consumption, and unstable quality in the industrial production of nitroguanidine. At the same time, it improves the disadvantages of poor flowability and poor mechanical properties of nitroguanidine, and is a low - risk and high - efficiency production method, expanding the application of supergravity technology in the control of energetic material crystals.

This invention discloses a highly insulating and low-hygroscopic thermal aerosol fire extinguishing agent and its preparation method, relating to the field of lithium-ion battery fire extinguishing agent technology. The key technical points include a redox system based on strontium nitrate and nitroguanidine, combined with a specific proportion of ammonium polyphosphate-melamine cyanurate-nano silica composite flame retardant, and the introduction of an additive. This additive is prepared by loading a mixture of methyltrimethoxysilane and octyltriethoxysilane onto a tin-doped mesoporous silica carrier. The effect is that when the fire extinguishing agent is released, the silane in the additive rapidly forms a highly insulating and hydrophobic siloxane network covering layer under the catalysis of tin ions. Simultaneously, the synergistic effect of the formulation and carrier structure endows the product with low hygroscopicity, ensuring stable performance in humid environments.