59results about "Hydrazoic-acids/azides/halogen-azides" patented technology

In one aspect, the invention provides a novel quaternary hydrogen storage composition having a hydrogenated state and a dehydrogenated state. Further, the present invention provides methods of storing hydrogen in a hydrogen storage composition, and methods of releasing hydrogen by reacting a nitride composition and a hydride composition.

The invention provides a preparation method of sodium azide. The preparation method comprises the steps of adding sulfuric acid to a solution consisting of an ethanol, a sodium nitrite, introducing the produced ethyl nitrite gas into a mixture consisting of a hydrazine hydrate, a sodium hydroxide, a catalyst, and an ethanol, and after the gas is introduced, carrying out a reaction for 1.5 to 2.5h at a temperature of 18 to 25 DEG C. The preparation method provided by the invention which adopts one step to prepare the sodium azide has the advantages of simple production process and easy operation. Since just one step is adopted, the intermediate product is not wasted, the product yield is greatly improved, the yield is more than 90%, the product qualification rate is great, and the purity is more than 99%.

The invention discloses a making method of sodium azide, which comprises the following steps: dripping sulfuric acid in the solution with alcohol, sodium nitrite and water; aerating ethyl nitrite gas into solution with hydrazine hydrate, sodium hydroxide, tetrabutylammonium bromide and alcohol; generating sodium azide; evaporating solvent; crystallizing; separating solid from liquid to obtain the product.

The invention discloses a microfluidics-based initiating explosive synthesis system and a method thereof. The microfluidics-based initiating explosive synthesis system comprises a main control computer and an initiating explosive synthesis unit; the initiating explosive synthesis unit comprises a set of reaction syringes, a micromixer, a liquid loading syringe, a T-shaped connector, a water bath heating unit and two injection pumps. The two injection pumps are both connected to the main control computer, wherein the outlet of one injection pump is connected with the liquid loading syringe, and the outlet of the other injection pump is connected with the set of reaction syringes; the outlet of the set of reaction syringes is connected with the micromixer; the micromixer and the outlet of the liquid loading syringe are connected with two mutually perpendicular outlets of the T-shaped connector respectively; a third outlet of the T-shaped connector is connected with a polyfluortetraethylene pipe arranged in the water bath heating unit. A liquid outputted from the set of reaction syringes is delivered through the micromixer, and is mixed with a liquid outputted from the liquid loading syringe in the T-shaped connector, and then the mixture is delivered into the polyfluortetraethylene pipe arranged in the water bath heating unit through the third outlet of the T-shaped connector. The microfluidics-based initiating explosive synthesis system and the method are high-efficient, safe and environment-friendly.

The invention provides a method for continuously preparing sodium azide. According to the method, the sodium azide is prepared through gas-liquid tower type continuous reaction and liquid-liquid continuous reaction, wherein ammonia gas and air serve as initial raw materials; and propanol, isopropanol, butanol, isobutanol, pentanol or isopentanol serve as carrier raw materials. Compared with the existing process, the method has the advantages that a large amount of inorganic salt waste water is avoided; all the harmful gases in a continuous system are recycled, so that danger is avoided; and the produced product has stable quality and is popularized in industry easily and widely.

The invention discloses a method and a device for synthesizing copper azide, in order to solve the problem of high danger in synthesis of copper azide and provide a new technology and a new technique for preparation of a novel green initiating explosive. A reaction device comprises an azoimide generation device, an azidation device and a tail gas absorption device. The method and the device for synthesizing the copper azide initiating explosive have the following remarkable advantages: (1) since explosion happens very easily once azoimide gas is in contact with grease, water and the like, and the whole device is all formed by means of connecting glassware through ground openings without rubber tubes and grease type substances such as vaseline, the safety of reaction is guaranteed fundamentally; (2) the azoimide gas is fed in from the lower part and discharged out from the upper part, thereby fully reacting with porous copper; (3) an anti-explosion ball is smart is structure design and samples can be conveniently placed in and taken out; (4) the gas absorption device with an anti-back-suction ball is capable of effectively preventing the azoimide gas from escaping.

The invention belongs to the field of organic chemical industry, and particularly relates to a sodium azide synthesis process, wherein sodium azide is prepared by using a micro-channel reactor systemand / or a tubular reactor system as a reaction device, using nitrite, hydrazine hydrate and sodium hydroxide as main raw materials and using an alcohol as a solvent through a continuous production process. Compared with the traditional kettle type reaction, the synthesis process of the present invention has advantages of low danger during the production, high safety factor, high product conversionrate, high product purity, low by-products and no waste salt generation. According to the present invention, corresponding alcohols, water, centrifugation mother liquors and the like generated by thereaction can be recovered and applied so as to reduce the production cost and reduce the environmental pressure, such that the economic benefits and the environmental benefits are improved.

The invention discloses application of fluorosulfonyl compound I to preparation of FSO2N3. According to application of the fluorosulfonyl compound I to preparation of the FSO2N3, the fluorosulfonyl compound I comprises a positive ion and a negative ion, the positive ion is presented as a formula A: please see the specification for the formula, wherein R1, R2, R3 and R4 are individually hydrogen orC1-C6 alkyl group, or the R3 and the R4 and a carbon atom between the R3 and the R4 commonly form unsaturation C5-C8 cyclo-hydrocarbyl. The required FSO2N3 can be safely, simply, conveniently and quickly prepared in high yield by adopting the fluorosulfonyl compound; and the prepared FSO2N3 can be directly used in subsequent reactions without treatment.

The invention relates to a preparation method of a high-density metal azide with arbitrarily regulated filling density, and belongs to the field of initiating explosive devices. The preparation methodmixes hollow microspheres with different diameters constructed by nanoporous metal / metal oxide and fills a restraint shell with the hollow microspheres to prepare hollow microspheres constructed by the nanoporous metal / metal oxide with a little filling density in the restraint shell, and then places the restraint shell filled with the hollow microspheres constructed by the nanoporous metal / metaloxide in a reactor to be subjected to gas-solid in-situ chemical reaction with hydrazoic acid gas to prepare the metal azide with high filling density. The preparation method of the invention can prepare the high-density metal azide having a filling density of 50%-92% of theoretical density in the restraint shell. The prepared high-density metal azide (for example, the copper azide dose is more than or equal to 0.4 mg) in a single restraint shell can detonate HNS-IV, CL-20, PETN, RDX and other explosives with a filling density being 75%-92% of the theoretical density and a diameter being morethan or equal to 0.5 mm or ignite B / KNO3 and other ignition powder.

The invention discloses an aqueous-phase synthetic method of sodium azide with n-butyl alcohol being circularly recycled, wherein the method includes following steps: (1) mixing butyl nitrite, sodium hydroxide, hydrazine hydrate, a catalyst and water to form a reaction system; (2) after the reaction finished, recycling the n-butyl alcohol and water; and (3) filtering a reaction solution to obtain a sodium azide (white solid) and circularly recycling the recycled n-butyl alcohol. In the method, by means of the butyl nitrite for synthesizing the sodium azide, so that compared with a synthesis route from ethyl nitrite, the synthetic method is free of high-pressure operations and the risk of leakage of gas. Meanwhile, the reaction can be carried out in the aqueous phase and just needs to added with the catalyst in a micro amount (especially, herein the catalyst may be composited of tributylamine and methanol), so that the synthetic method is environmental-protective. The method is high in yield of product, is low in the content of free alkali and is high in product purity. Meanwhile, the reaction achieves the recycle of a by-product n-butyl alcohol for synthesizing the butyl nitrite, by means of the technical scheme, the environmental pollution is reduced while the economic benefit is increased.

The invention discloses a high-performance copper azide composite initiating explosive and a preparation method thereof, and belongs to the crossing field of nano-chemistry and energetic materials. Firstly, a novel copper-sulfur cluster-based porous coordination polymer (Cu12bpy for short) is prepared, and the chemical formula of the compound is [Cu12(StBu)9(CF3COO)3(bpy)4]n. Then, Cu12bpy is usedas a precursor to prepare a copper azide-heteroatom co-doped porous carbon material (CA-HPCH for short); and the CA-HPCH has a high copper azide content (89.43%), excellent ignition capacity (H50>=60cm) and low electrostatic sensitivity (E50=1.1 mJ), and is superior to common copper azide in performance. The micro initiating device made of CA-HPCH has short ignition time (7.0[mu]s) and low ignition energy (0.106 mJ), the performance of the composite initiating explosive exceeds that of most reported initiating explosives, and a basis is provided for further designing and synthesizing a high-performance initiating explosive.

The invention discloses a method for preparing nickel hydrazine azide. The method comprises: taking soluble nickel salts as base solution; using acetic acid to adjust the pH of the formed base solution; using graphite as modified additives of medicaments; adding sodium nitride solution and hydrazine hydrate solution to the base solution dropwise to perform chemical combination; preserving heat, cooling, leaching, washing, dehydrating and drying; and obtaining a finished product of nickel hydrazine azide. The method is simple in pH control, and buffer solution consisting of weak acid and weak-acid salts ensures stable pH, longer effectiveness and the unicity of medicament composition, and significantly improves explosion initiation capacity, so the buffer solution is more suitable to be used as a primary explosive. By adopting nickel acetate as raw material, a small quantity of nickel hydrazine nitrate substances which are formed by use of nitrates and result in worse or unstable pharmaceutical performance can be avoided. Dropping and time difference ensure the complete reaction of sodium nitride and high yield of nickel hydrazine azide.

The present invention relates to a method, a reagent and an apparatus for determining a substrate concentration based on an amount of hydrogen peroxide generated from a substrate. In the present invention, a suppressing agent for suppressing a reaction between the hydrogen peroxide and an inhibitor is added. As the suppressing agent, an azide compound such as sodium azide or a nitrite compound such as sodium nitrite is used. In the invention, a supporting electrolyte, such as sodium chloride or potassium chloride may be further added.

The invention relates to the technical field of nitrogen-rich material preparation, and provides a high-pressure preparation method of sodium pentazole. The method comprises the following steps: filling a diamond anvil cell sample cavity with sodium azide, and pressurizing sodium azide in the sample cavity to obtain sodium pentazole; wherein the pressure of the pressurization is 21.6 GPa or more.According to the method provided by the invention, sodium pentazole can be obtained through simple one-step pressurizing treatment without heating or adding any pressure transmission medium, other impurities are not introduced in the whole process, the synthesis cost is saved, the environment is not polluted, and the method is simple, safe and reliable.

The invention proposes a trinitride and a synthesis method thereof, and application thereof as a heat-resisting initiating explosive. The chemical name of the trinitride is azide cadmium, the molecular formula is Cd(N3)2, the trinitride reacts through a cadmium nitrate solution and a sodium azide solution under the conditions of required reaction temperature, material ratio, charging sequence, reaction time and pH value of a reaction solution, so as to obtain the azide cadmium. The performance of the azide cadmium is subjected to comprehensive assessment by a test. The impact sensitivity of carbonic anhydrase (CA) is equivalent to that of lead azide while the friction sensitivity and the static-electric sensitivity are more insensitive than those of the lead azide; the decomposition peak temperature of the CA is higher than that of the lead azide, and achieves 334-370 DEG C; the explosion temperature can be up to 417-426 DEG C; the initiating power of the CA is much stronger than that of the lead azide. Thus, the CA can be applied to heat-resisting detonators and various miniature detonators instead of the lead azide.

The invention discloses a preparation method of copper azide / cuprous azide packaged by a conductive metal organic framework. According to the method, a conductive copper-containing metal organic framework material is adopted as a precursor, and azido of the precursor is completed through a liquid-solid electrochemical azido reaction. According to the invention, the copper azide / cuprous azide nanocrystals are highly and uniformly embedded in the conductive frame, so that agglomeration of copper azide / cuprous azide can be effectively avoided, static electricity generated by friction, displacement and the like can be reduced, the conductive frame can promote effective transfer of charges, accumulation of static charges is avoided, and the static safety performance is improved. Besides, the liquid-solid electrochemical azide reaction has the advantages of safety, high efficiency, short reaction time, high operability and the like, and the preparation process is compatible with the MEMS process, so that the application of the copper azide / cuprous azide material in micro devices is facilitated.

The invention provides a foam graphene-based metal azide compound and a preparation method thereof. Soluble metal salt, nano metal powder or nano metal oxide is used as a raw material, graphene is used as a conductive carbon material carrier, and the foam graphene-based metal azide compound is prepared. The azide is a metal azide initiating explosive material based on foamed graphene, which is prepared by uniformly dispersing nano metal / metal oxide in a graphene oxide solution and carrying out high-temperature hydrothermal reduction reaction, freeze drying and in-situ azide reaction. Comparedwith the traditional azide, the foam graphene-based azide initiating explosive has the advantages that the particle size can reach hundreds of nanometers, the electrostatic sensitivity of the foam graphene-based azide initiating explosive can be greatly reduced due to the existence of the graphene conductive material, and the safety of the foam graphene-based azide initiating explosive is greatlyimproved.

The invention relates to a preparation method for high-density copper azide with a constrained shell, and belongs to the field of initiating explosive devices. Nanoporous copper or nanoporous copper oxide fills the constraining shell and then is stored, and then the high-density copper azide is prepared by a gas-solid in-situ chemical reaction with hydrazoic acid gas before use; and risks of production, transportation and post-explosive pressing of the traditional primary explosives are avoided during the operation. The prepared copper azide with the constrained shell has high loading density,no dangers during the loading process, safe transportation and storage, and strong detonation power. The explosive quantity of single-shot copper azide in the constrained shell belongs to the submilligram class, and the preparation process is green and pollution-free. The high-density copper azide of which the loading density is 1.4 to 3.2g / cm<3> can be prepared by the method disclosed by the invention, and the prepared high-density copper azide in the constraining shell can initiate explosives such as HNS-IV, CL-20, PETN and RDX of which the loading density is 75% to 92% of the theoretical density and the diameters are not smaller than 0.5mm and ignite igniters of B / KNO3 and the like when the explosive quantity of the high-density copper azide is not smaller than 0.4mg.

The invention relates to the technical field of confinement nanometer compound materials, particularly to a NaN3@BNNTs confinement nanometer compound material and a preparation method thereof. According to the NaN3@BNNTs confinement nanometer compound material, sodium azide is confined inside boron nitride nanotubes, and through weak interaction between the sodium azide and the boron nitride nanotubes, the sodium azide can exist stably, so that the problem of safe storage of the sodium azide can be solved.

The invention discloses a silver azide initiating explosive film and a preparation method thereof. According to the method, het silver azide initiating explosive film is integrated on the surface of a conductive substrate in situ by adopting a two-step electrochemical method. The preparation method specifically comprises the following steps: firstly, preparing a porous silver film by adopting an electrochemical cathode deposition method, and then taking the porous silver film as a precursor, and obtaining the porous silver azide primary explosive film by adopting an electrochemical anode azidation method. Compared with a traditional silver azide preparation method, the method has the advantages that use of high-risk chemical reagents is avoided, and the preparation process is simple, efficient, safe and controllable; and the in-situ growth mode does not need an additional charging process, is highly compatible with the MEMS process, and has a good application prospect in the field of micro-explosion systems.

The invention discloses a synthesis method of sodium azide. According to the synthesis method, sodium nitrite and isoamyl alcohol are taken as the initial raw materials; sodium nitrite and isoamyl carry out reactions, the reaction product is isoamyl nitrite, isoamyl nitrite is dropwise added into alkaline hydrazine hydrate to carry out reactions, and the reaction product is sodium azide crystal. In the provided synthesis method, liquid-liquid homogenous reactions are carried out, the process is easy to control, the operation is stable and safe, the yield is improved by 5% or more, the comprehensive cost is low, and the synthesis method can be applied to industrial massive production.

The invention discloses a method for preparing low-sensitivity copper azide by compounding rGO and copper nano-wires. The method comprises the following steps: preparing copper nano-wires by using a liquid phase reduction method, adding graphene oxide in the copper nano-wire synthesis process, preparing an electrophoretic solution from the prepared copper nano-wire / reduced graphene oxide compositematerial by using catechuic acid as a reducing agent through a hydrothermal method, carrying out an electrophoretic deposition experiment by using graphite as an anode and using a silicon wafer as acathode to deposit the surface of the silicon wafer, and carrying out azidation to prepare the low-sensitivity copper azide prepared from the composite rGO and the copper nano-wires. According to theinvention, with the preparation method, the influence of external force on the reaction product can be effectively reduced so as to improve the safety and the reliability; sodium azide and nitric acidare used as the reactants, the adopted device is simple, and the azidation efficiency is high; and the accumulation of electrostatic charges on the composite material is reduced through the carbon material, so that the electrostatic sensitivity of the copper azide is reduced while the excellent detonation performance of the copper azide is not affected.

A method for generation of material in a liquid phase comprising a step of subjecting the liquid phase to a nanosecond-pulsed discharge plasma.

The invention discloses a method for preparing low-sensitivity copper azide by compounding carbon nano-tubes and copper nano-wires. The method comprises the following steps: preparing copper nano-wires by utilizing a liquid phase reduction method, mixing the copper nano-wires and single-walled carbon nano-tubes, depositing the prepared composite material on an electric-conducting substrate by utilizing an electrochemical deposition method, and preparing the copper azide / carbon nano-tube composite energetic material through a gas-solid phase azide reaction. According to the preparation method provided by the invention, the influence of external force on the reaction product can be effectively reduced so as to improve the safety and the reliability; sodium azide and stearic acid are used asthe reactants, the adopted device is simple, and the azidation efficiency is high; and the accumulation of electrostatic charges on the composite material is reduced through the carbon material, so that the electrostatic sensitivity of the copper azide is reduced while the excellent detonation performance of the copper azide is not affected.

The present invention discloses a process for the on-demand production of small quantities of lead azide. First, a metered quantity of sodium azide solution and a metered quantity of a solution of a lead salt sufficient to react with the sodium azide are introduced into a T-mixer or Y-mixer. Then, the sodium azide and lead salt solutions are conveyed into a static mixer and the azide and lead compounds are permitted to react together, forming insoluble crystals of lead azide as a slurry in an aqueous medium. The lead azide crystals are then separated from the aqueous medium. The process is carried out within an explosion-proof chamber.

The invention belongs to the technical field of environment-friendly waste gas treatment, and particularly discloses a nitromethane waste gas recycling treatment method. According to a technical scheme in the invention, the method comprises the following steps: (1) washing the nitromethane waste gas through multi-stage alkali liquor in sequence; and (2) introducing tail gas washed by the multi-stage alkali liquor into absorption liquid of a sodium hydroxide or potassium hydroxide organic solvent containing hydrazine hydrate for reaction absorption. The invention also provides a method for preparing sodium azide or potassium azide and a medical intermediate methylmercaptotetrazole by using the nitromethane tail gas. The method is different from an existing method which only uses alkali liquor for absorption treatment; and according to the method, the waste gas is purified through multi-stage alkali liquor washing, then methyl nitrite causing excessive emission of nitric oxide is subjected to reaction absorption, efficient co-production can be achieved while the waste gas is treated, the waste is turned into the wealth, and problems in treatment of nitrogen oxides in continuous large-scale production of nitromethane are solved.

The invention discloses a continuous production method of sodium azide. According to the method, a packed tower is used as a reactor such as a fixed bed, so that gas and liquid completely come into contact with each other to finish synthetic reaction within a certain time to realize continuous production, and the synthesis yield is further improved; process conditions are simple, few chemical equipment is used, a flow is short, and the method is applied to industrial production; therefore, the method has huge market space.