CN109206284A - The method for preparing super-hydrophobic oxidant based on lotus leaf effect - Google Patents

The method for preparing super-hydrophobic oxidant based on lotus leaf effect Download PDF

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CN109206284A
CN109206284A CN201811130851.2A CN201811130851A CN109206284A CN 109206284 A CN109206284 A CN 109206284A CN 201811130851 A CN201811130851 A CN 201811130851A CN 109206284 A CN109206284 A CN 109206284A
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hydrophobic
super
oxidizing agent
acetate
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CN109206284B (en
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郭长平
许鹏飞
王敦举
王瑞浩
冀威
田璐
杨光成
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Southwest University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
    • C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
    • C06B23/009—Wetting agents, hydrophobing agents, dehydrating agents, antistatic additives, viscosity improvers, antiagglomerating agents, grinding agents and other additives for working up
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
    • C06B31/28—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B43/00—Compositions characterised by explosive or thermic constituents not provided for in groups C06B25/00 - C06B41/00
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
    • C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
    • C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
    • C06B45/32—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a kind of methods for preparing super-hydrophobic oxidant based on lotus leaf effect, comprising: low-surface-energy material is added in solvent, oxidizing agent pellets, stirring, filtering, drying is then added；Oxidizing agent pellets after low-surface-energy material is modified are added in metal salt solution, filter after it is sufficiently reacted, is dry, obtaining super-hydrophobic oxidizing agent pellets.The present invention is surface-treated oxidant easy to moisture absorption using bionic super-hydrophobic principle, it is substantially reduced its hydroscopicity, especially under the conditions of temperature is 60 DEG C, relative humidity is 80% and the testing time is 400 hours, the hydroscopicity of ADN reduces 53% or so, it can place in air 6 months and agglomeration still do not occur, used covering material is while realizing oxidant anti-moisture absorption energy, metal salt therein can significantly reduce the thermal decomposition temperature of oxidant, this is very significant to application of the oxidant in high burn rate solid propellant.

Description

The method for preparing super-hydrophobic oxidant based on lotus leaf effect
Technical field
It is specially a kind of super thin based on lotus leaf effect preparation the invention belongs to the anti-moisture absorption technology of inorganic oxidizer easy to moisture absorption The method of water oxygen agent.
Background technique
Aeronautics and space technology is most active, most influential science and technology in human knowledge and nature remodeling process, It is the important symbol of human civilization high development.Composite solidpropellant is most common energy and material in aerospace, master Wanting ingredient is oxidant and fuel agent.Currently, common oxidant is ammonia perchlorate (AP), diamide ammonium (ADN) and nitric acid Ammonium (AN) etc., these oxidants provide oxygen during propellant combustion, and for it, smoothly burning provides guarantee, but they have one A common disadvantage: the easily hygroscopicity during preparation, production, storage, propellant casting etc., and then influence its usability Can, therefore need to be modified these oxidants before application to reduce its hygroscopicity.
Moisture-absorption modified technology is realized by coating mostly is prevented to oxidant easy to moisture absorption both at home and abroad at present, husky identical use Polysilane is that coupling agent is modified AP, and the functional group on the functional group in the coupling agent and the surface AP acts on, and is formed firm Chemical bond, AP particle surface formed one layer of separation layer prevent its coalesced by moisture absorption (energetic material, 1995,3 (2): 26-30).Nitrocotton (NC) is coated on AP particle surface using solvent evaporated method by Deng Guodong etc., and soilless sticking phenomenon, makes in 30 days (explosive wastewater journal, 2009,32 (1): 9-12) are greatly reduced in its hygroscopicity.Pei Hao etc. is contained and can be increased with the deterrent containing energy and low sensitivity Agent is moulded as covering material, surface is carried out to ultrafine ammonium perchlorate using solvent evaporated method, solution suspension method and distillation under vacuum The influence of method for coating and covering dosage to covered effect and performance is investigated in coating modification, achieves preferable effect (south Capital Polytechnics, 2013, master thesis).Liu Kejian etc. obstructs principle according to crystal brige, utilizes inertia nano inorganic oxide It is mutually compound for carrier and function additive, it is prepared for being prepared for the functional modifier for preventing ultra-fine agglomeration by formulation optimization The ultra-fine AP powder of anti-caking, under conventional hermetic condition of storage, can store more than June (Institutes Of Technology Of Nanjing, 2009, it is large Bachelorship paper).Wu Hao etc. coats its surface using polystyrene and ten difluoro heptyl propyl trimethoxy silicanes, reduces The hygroscopicity (energetic material, 2014,22 (4): 482-486) of AP.It is compound that Yang Fan etc. uses sol-gal process to be prepared for ADN/AP Two kinds of compound particles of particle and ADN/ carbon nanotube, the results showed that, the hygroscopicity of ADN/AP compound particle has bright compared with former ADN Aobvious to reduce, the hygroscopicity of the especially ADN/AP compound particle of ethanol/dichloromethane system preparation reduces nearly 10 than former ADN Again (Institutes Of HulunBuir's journal, 2008,14 (4): 67-71).German Ulrich etc. carries out ADN using cellulose acetate-butyrate Microcapsule coated improves the stability etc. of product, then uses amino in particle surface cladding coating of wax shape object additionally by elder generation Resin cladding, hygroscopicity obtained a degree of improvement (Propellants, Explosives, Pyrotechnics, 2000, 25(2):81-85).Liu Jinhe etc. uses vacuum gas-phase cladding process, by dodecyl benzene sulfonic acid decorations, stearic acid decorations and octadecylamine Nitrate etc. is coated on nitric acid ammonia surface, and analyzes the reason of additive reduces nitric acid money hygroscopicity and caking capacity, obtains The adding order of temperature of plate and compound additive is to influence two principal elements of resistive connection block effect.
Although currently, carried out preventing moisture-absorption modified processing in the prior art to oxidant easy to moisture absorption using a variety of methods, But the effect obtained is satisfactory not to the utmost, and the surface for being primarily due to these oxidants can be too high, easily the water in absorption air Steam, while must take into account energy and security performance etc. as energetic material therefore cannot say that clad is done too thick.Therefore it needs It is moisture-absorption modified prevent to these oxidants to seek significantly more efficient technology.Super-hydrophobic technology is to simulate lotus over the past decade Foliar surface structure and a kind of bionics techniques to grow up in waterproof, are catchmented, automatically cleaning, the side such as water-oil separating and steamer drag reduction There are extensive research and application prospect in face, but is rarely reported in the anti-moisture absorption of energetic material.The present invention utilizes super-hydrophobic principle The efficient anti-moisture absorption energy of tri- kinds of oxidants of AP, ADN and AN is realized, provides a kind of new think of to prepare composite modified propellant Road.
Summary of the invention
It is excellent it is an object of the invention to solve at least the above problems and/or defect, and provide at least to will be described later Point.
In order to realize these purposes and other advantages according to the present invention, provide a kind of super thin based on lotus leaf effect preparation The method of water oxygen agent, comprising the following steps:
Step 1: low-surface-energy material is added in solvent, oxidizing agent pellets, stirring, filtering, drying is then added；
Step 2: the oxidizing agent pellets after low-surface-energy material is modified are added in metal salt solution, it is sufficiently anti-to it Should after filter, dry, obtain super-hydrophobic oxidizing agent pellets.
Preferably, the low-surface-energy material is ten~25 alkanoic acids, ten~25 alkanoic acid potassium, ten~bis- 15 alkanoic acid sodium, vinyltrimethoxysilane, three ethoxy silane of vinyl, 3- aminopropyl triethoxysilane, propyl three Ethoxysilane, gamma-aminopropyl-triethoxy-silane, perfluoropolyether, perfluorocarboxylic acid, one of or it is a variety of.
Preferably, the dosage of the low-surface-energy material is the 0.01%-10% of oxidizing agent pellets total amount.
Preferably, the solvent in the step 1 is ethyl alcohol, n-butanol, isopropanol, ethyl acetate, butyl acetate, second Isoamyl valerate, acetic acid, propionic acid, methylene chloride, chloroform, carbon tetrachloride, dichloroethanes, ether, petroleum ether, normal butane, ring One of hexane is a variety of.
Preferably, it is 0.1%~50% that the mass concentration of the feed liquid formed in solvent, which is added, in the low-surface-energy material.
Preferably, the oxidant is ammonia perchlorate, diamide ammonium, any one in ammonium nitrate.
Preferably, the stirring is any one in mechanical stirring, magnetic agitation or ultrasonic agitation；The step 1 It is air drying, vacuum drying, any one in freeze-drying with the drying in step 2；Surpass obtained in the step 2 The size of hydrophobic oxidizing agent pellets is 10nm~2mm.
Preferably, the mass concentration of the metal salt solution is 0.5~5%；Solute in the metal salt solution is Copper nitrate, copper chloride, copper sulphate, copper acetate, ferric nitrate, iron chloride, ferric sulfate, ferric acetate, ferrous nitrate, frerrous chloride, sulphur Sour ferrous iron, ferrous acetate, cobalt nitrate, cobalt chloride, cobaltous sulfate, cobalt acetate, copper nitrate, copper chloride, copper sulphate, copper acetate, nitric acid Manganese, manganese chloride, manganese sulfate, manganese acetate, zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, nickel nitrate, nickel chloride, nickel sulfate, acetic acid One of nickel, silver nitrate, silver chlorate, silver acetate are a variety of；Solvent in the metal salt solution is ethyl alcohol, n-butanol, different One of propyl alcohol, ethyl acetate, butyl acetate, isoamyl acetate, methylene chloride, chloroform, carbon tetrachloride, dichloroethanes Or it is a variety of.
Preferably, the low-surface-energy material the preparation method comprises the following steps: by nano-attapulgite according to solid-to-liquid ratio 1:12~ 15 are added to the water, and dispersing agent is added, and stirring obtains nano-attapulgite dispersion liquid, then carry out to attapulgite suspension high Impulse electric field processing is pressed, is added after being disposed into attapulgite suspension and is equivalent to the hard of attapulgite quality 12~15% Resin acid sodium and 3~5% sodium lauroyl sarcosine are stirred to react 30~60min at 70~80 DEG C, filter, and wash, dry, Dry product is configured to the suspension that concentration is 10~15wt%；It is by 30~60 parts of suspensions and 5~10 parts of weight ratios 2:2:1 vinyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane and octadecanoid acid are added in sealing container, and sealing is set Irradiation stir process is carried out in the electron accelerator of 2.5MeV, 40mA, is filtered, and drying, nano grinder crushes, and obtains low table It face can material；The radiation dose rate of the irradiation is 100~200kGy/h, and irradiation dose is 200~1000kGy, mixing speed For 100~150r/min；The dispersing agent accounts for nano-attapulgite quality 1~3%；The dispersing agent is 1- ethyl -3- methyl Imidazoleacetic acid salt.
It preferably, further include that the super-hydrophobic oxidizing agent pellets that will be obtained are reprocessed after the step 2, process Are as follows: super-hydrophobic oxidizing agent pellets are sent into atmos low-temperature plasma device, super-hydrophobic oxidizing agent pellets is made to be in atmosphere 20~60mm at the jet exit of isothermal plasma is forced down, according to the gas of 8~12L/h in atmos low-temperature plasma device Flow is passed through gas medium, applies operating voltage, forms plasma jet, controls the spray of atmos low-temperature plasma device The movement speed of exit wound of bullet makes plasma jet injection on super-hydrophobic oxidizing agent pellets, to super-hydrophobic oxygen in 5~10mm/s Catalyst particles carry out 30~60min of processing；The operating voltage using high-voltage ac power provide, the operating voltage be 50~ The alternating voltage of 100kV, frequency are 100~300kHz；The gas medium be rare gas/oxygen, oxygen, nitrogen, ammonia, CF4、CCl4、SF6One or more of mixing.
The present invention is include at least the following beneficial effects:
The present invention is surface-treated oxidant easy to moisture absorption using bionic super-hydrophobic principle, drops its hydroscopicity obviously Low, especially under the conditions of temperature is 60 DEG C, relative humidity is 80% and the testing time is 400 hours, the hydroscopicity of ADN is reduced 53% or so (being tested using using GJB770A-97), can be placed in air 6 months and agglomeration still do not occur；Value It obtains it is noted that used covering material is while realizing oxidant anti-moisture absorption energy, metal salt therein can significantly drop The thermal decomposition temperature of hypoxemia agent, this is very significant to application of the oxidant in high burn rate solid propellant.The present invention is real Show the efficient anti-moisture absorption energy of tri- kinds of oxidants of AP, ADN and AN, provides a kind of new think of to prepare composite modified propellant Road.Its remarkable advantage: (1) it is easy to operate, high-efficient and at local, it can be with mass production；(2) experiment condition is mild, product Quality is higher；(3) non-energetic material ratio used in is small, does not interfere with the oxidation effectiveness of oxidant.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention:
Fig. 1 is the scanning electron microscope (SEM) photograph of super-hydrophobic oxidizing agent pellets prepared by the embodiment of the present invention 1.
Specific embodiment:
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text Word can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more The presence or addition of a other elements or combinations thereof.
Embodiment 1:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
It is configured to the solution that mass concentration is 2% in ethyl acetate Step 1: 1g tetradecanoic acid is dissolved in, 50g is added Ammonium perchlorate solid particle, filtration drying is stand-by after stirring 30 minutes；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g copper chloride is dissolved to, it is dry that step 1 is added Solid after dry stirs 20 minutes, and filtration drying obtains super-hydrophobic oxidizing agent pellets.
Embodiment 2:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
It is configured to the solution that mass concentration is 3% in ethyl acetate Step 1: 1g Heptadecanoic acide is dissolved in, 50g is added Ammonium perchlorate solid particle, filtration drying is stand-by after stirring 30 minutes；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g silver nitrate is dissolved to, it is dry that step 1 is added Solid after dry stirs 20 minutes, and filtration drying obtains super-hydrophobic oxidizing agent pellets.
Embodiment 3:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
The solution that mass concentration is 1% is configured in dichloroethanes Step 1: three ethoxy silane of 1g vinyl is dissolved in, 50g diamide ammonium solid particle is added, filtration drying obtains finished product after ten minutes for stirring；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g ferric nitrate is dissolved to, it is dry that step 1 is added Solid after dry stirs 20 minutes, and filtration drying obtains super-hydrophobic oxidizing agent pellets.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 15%.
Embodiment 4:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
It is configured to the solution that mass concentration is 0.1% in ethyl alcohol Step 1: 0.1g perfluoropolyether is dissolved in, 50g is added Diamide ammonium solid particle, filtration drying is stand-by after stirring 30 minutes；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g nickel nitrate is dissolved to, above-mentioned drying is added Solid afterwards stirs 20 minutes, and filtration drying obtains super-hydrophobic oxidizing agent pellets.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 15.5%.
Embodiment 5:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
It is configured to the solution that mass concentration is 0.1% in ethyl alcohol Step 1: 0.1g octadecanoid acid is dissolved in, 50g is added Ammonium nitrate solid particle, filtration drying is stand-by after stirring 30 minutes；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g nickel nitrate is dissolved to, above-mentioned drying is added Solid afterwards stirs 20 minutes, and filtration drying obtains super-hydrophobic oxidizing agent pellets.
Embodiment 6:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
It is configured to the feed liquid that mass concentration is 1% in butyl acetate Step 1: 1g low-surface-energy material is added to, is added 50g diamide ammonium solid particle, filtration drying obtains finished product after ten minutes for stirring；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g ferric nitrate is dissolved to, it is dry that step 1 is added Solid after dry stirs 20 minutes, and filtration drying obtains finished product；
The low-surface-energy material the preparation method comprises the following steps: nano-attapulgite is added to the water according to solid-to-liquid ratio 1:12, add Enter dispersing agent, stir, obtain nano-attapulgite dispersion liquid, then attapulgite suspension is carried out at high-pressure pulse electric The moon of the odium stearate and 5% that are equivalent to attapulgite quality 12% is added in reason into attapulgite suspension after being disposed Osmanthus acylsarcosine sodium is stirred to react 60min at 80 DEG C, filters, and washs, and dry, dry product, which is configured to concentration, is The suspension of 15wt%；It is 2:2:1 vinyltrimethoxysilane, γ-aminopropyl three by 60 parts of suspensions and 10 parts of weight ratios Ethoxysilane and octadecanoid acid are added in sealing container, and sealing is placed in the electron accelerator of 2.5MeV, 40mA and is irradiated Stir process filters, and drying, nano grinder crushes, and obtains low-surface-energy material；The radiation dose rate of the irradiation is 200kGy/h, irradiation dose 1000kGy, mixing speed 150r/min；The dispersing agent accounts for nano-attapulgite quality 3%；The dispersing agent is 1- ethyl-3-methylimidazole acetate.Being passed through using low-surface-energy material prepared by the present invention will be recessed Convex stick soil is modified as hydrophobic structure, and with vinyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane and octadecanoid acid etc. In conjunction with can be further improved the hydrophobic performance of diamide ammonium crystal.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 12.2%.
Embodiment 7:
A method of super-hydrophobic oxidant is prepared based on lotus leaf effect, comprising the following steps:
It is configured to the feed liquid that mass concentration is 1% in butyl acetate Step 1: 1g low-surface-energy material is added to, is added 50g diamide ammonium solid particle, filtration drying obtains finished product after ten minutes for stirring；
It is configured to the solution that concentration is 1% in ethyl acetate Step 2: 0.5g ferric nitrate is dissolved to, it is dry that step 1 is added Solid after dry stirs 20 minutes, and filtration drying obtains finished product；
The low-surface-energy material the preparation method comprises the following steps: nano-attapulgite is added to the water according to solid-to-liquid ratio 1:14, add Enter dispersing agent, stir, obtain nano-attapulgite dispersion liquid, then attapulgite suspension is carried out at high-pressure pulse electric The moon of the odium stearate and 3% that are equivalent to attapulgite quality 12% is added in reason into attapulgite suspension after being disposed Osmanthus acylsarcosine sodium is stirred to react 60min at 70 DEG C, filters, and washs, and dry, dry product, which is configured to concentration, is The suspension of 12wt%；It is 2:2:1 vinyltrimethoxysilane, γ-aminopropyl three by 60 parts of suspensions and 10 parts of weight ratios Ethoxysilane and octadecanoid acid are added in sealing container, and sealing is placed in the electron accelerator of 2.5MeV, 40mA and is irradiated Stir process filters, and drying, nano grinder crushes, and obtains low-surface-energy material；The radiation dose rate of the irradiation is 200kGy/h, irradiation dose 1000kGy, mixing speed 150r/min；The dispersing agent accounts for nano-attapulgite quality 3%；The dispersing agent is 1- ethyl-3-methylimidazole acetate.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 12.3%.
Embodiment 8:
It further include that the super-hydrophobic oxidizing agent pellets that will be obtained are reprocessed after the step 2, process are as follows: will be super thin Water oxygen catalyst particles be sent into atmos low-temperature plasma device in, make super-hydrophobic oxidizing agent pellets be in atmos low-temperature etc. from 60mm at the jet exit of daughter is passed through gas medium according to the throughput of 12L/h in atmos low-temperature plasma device, Apply operating voltage, form plasma jet, controls the movement speed of the jet exit of atmos low-temperature plasma device In 10mm/s, makes plasma jet injection on super-hydrophobic oxidizing agent pellets, super-hydrophobic oxidizing agent pellets are handled 60min；The operating voltage is provided using high-voltage ac power, and the operating voltage is the alternating voltage of 100kV, and frequency is 300kHz；The gas medium is nitrogen.By atmos low-temperature plasma processing technique, material matrix can not influenced Under the premise of performance, the hydrophobic performance of material is further increased.
Remaining technological parameter and process with it is identical in embodiment 3.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 13%.
Embodiment 9:
It further include that the super-hydrophobic oxidizing agent pellets that will be obtained are reprocessed after the step 2, process are as follows: will be super thin Water oxygen catalyst particles be sent into atmos low-temperature plasma device in, make super-hydrophobic oxidizing agent pellets be in atmos low-temperature etc. from 30mm at the jet exit of daughter is passed through gas medium according to the throughput of 10L/h in atmos low-temperature plasma device, Apply operating voltage, form plasma jet, controls the movement speed of the jet exit of atmos low-temperature plasma device In 5mm/s, makes plasma jet injection on super-hydrophobic oxidizing agent pellets, super-hydrophobic oxidizing agent pellets are handled 60min；The operating voltage is provided using high-voltage ac power, and the operating voltage is the alternating voltage of 85kV, and frequency is 250kHz；The gas medium is CCl4。
Remaining technological parameter and process with it is identical in embodiment 3.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 12.8%.
Embodiment 10:
It further include that the super-hydrophobic oxidizing agent pellets that will be obtained are reprocessed after the step 2, process are as follows: will be super thin Water oxygen catalyst particles be sent into atmos low-temperature plasma device in, make super-hydrophobic oxidizing agent pellets be in atmos low-temperature etc. from 30mm at the jet exit of daughter is passed through gas medium according to the throughput of 10L/h in atmos low-temperature plasma device, Apply operating voltage, form plasma jet, controls the movement speed of the jet exit of atmos low-temperature plasma device In 5mm/s, makes plasma jet injection on super-hydrophobic oxidizing agent pellets, super-hydrophobic oxidizing agent pellets are handled 60min；The operating voltage is provided using high-voltage ac power, and the operating voltage is the alternating voltage of 85kV, and frequency is 250kHz；The gas medium is CCl4。
Remaining technological parameter and process with it is identical in embodiment 6.
Hygroscopicity test is carried out to the super-hydrophobic spherical diamide ammonium of untreated diamide ammonium crystal and preparation (to adopt With GJB770A-97 standard), the hydroscopicity of untreated diamide ammonium crystal is 68%；The super-hydrophobic oxygen that the embodiment obtains The hydroscopicity of catalyst particles is 10.2%.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and legend shown and described herein.

Claims (10)

1. a kind of method for preparing super-hydrophobic oxidant based on lotus leaf effect, which comprises the following steps:
Step 1: low-surface-energy material is added in solvent, oxidizing agent pellets, stirring, filtering, drying is then added；
Step 2: the oxidizing agent pellets after low-surface-energy material is modified are added in metal salt solution, after it is sufficiently reacted Filtering, drying, obtain super-hydrophobic oxidizing agent pellets.
2. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the low table Face energy material is ten~25 alkanoic acids, ten~25 alkanoic acid potassium, ten~25 alkanoic acid sodium, vinyl trimethoxy Base silane, three ethoxy silane of vinyl, 3- aminopropyl triethoxysilane, propyl-triethoxysilicane, three ethoxy of γ-aminopropyl One of base silane, perfluoropolyether, perfluorocarboxylic acid are a variety of.
3. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the low table The dosage of face energy material is the 0.01%-10% of oxidizing agent pellets total amount.
4. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the step Solvent in one is ethyl alcohol, n-butanol, isopropanol, ethyl acetate, butyl acetate, isoamyl acetate, acetic acid, propionic acid, dichloromethane One of alkane, chloroform, carbon tetrachloride, dichloroethanes, ether, petroleum ether, normal butane, hexamethylene are a variety of.
5. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the low table The mass concentration that the feed liquid formed in solvent is added in face energy material is 0.1%~50%.
6. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the oxidation Agent is ammonia perchlorate, diamide ammonium, any one in ammonium nitrate.
7. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the stirring For any one in mechanical stirring, magnetic agitation or ultrasonic agitation；Drying in the step 1 and step 2 is dry for room temperature It is dry, vacuum drying, freeze-drying in any one；The size of super-hydrophobic oxidizing agent pellets obtained in the step 2 is 10nm~2mm.
8. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the metal The mass concentration of salting liquid is 0.5~5%；Solute in the metal salt solution is copper nitrate, copper chloride, copper sulphate, acetic acid Copper, ferric nitrate, iron chloride, ferric sulfate, ferric acetate, ferrous nitrate, frerrous chloride, ferrous sulfate, ferrous acetate, cobalt nitrate, chlorine Change cobalt, cobaltous sulfate, cobalt acetate, copper nitrate, copper chloride, copper sulphate, copper acetate, manganese nitrate, manganese chloride, manganese sulfate, manganese acetate, nitre Sour zinc, zinc chloride, zinc sulfate, zinc acetate, nickel nitrate, nickel chloride, nickel sulfate, nickel acetate, silver nitrate, silver chlorate, in silver acetate It is one or more；Solvent in the metal salt solution is ethyl alcohol, n-butanol, isopropanol, ethyl acetate, butyl acetate, second One of isoamyl valerate, methylene chloride, chloroform, carbon tetrachloride, dichloroethanes are a variety of.
9. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the low table Face can material the preparation method comprises the following steps: nano-attapulgite is added to the water according to solid-to-liquid ratio 1:12~15, dispersing agent is added, stirs It mixes, obtains nano-attapulgite dispersion liquid, high-pressure pulse electric processing then is carried out to attapulgite suspension, after being disposed The lauroyl flesh of the odium stearate and 3~5% that are equivalent to attapulgite quality 12~15% is added into attapulgite suspension Propylhomoserin sodium is stirred to react 30~60min at 70~80 DEG C, filters, and washs, and dry, dry product, which is configured to concentration, is The suspension of 10~15wt%；Be 2:2:1 vinyltrimethoxysilane by 30~60 parts of suspensions and 5~10 parts of weight ratios, Gamma-aminopropyl-triethoxy-silane and octadecanoid acid are added in sealing container, sealing, and the electronics for being placed in 2.5MeV, 40mA accelerates Irradiation stir process is carried out in device, is filtered, and drying, nano grinder crushes, and obtains low-surface-energy material；The irradiation of the irradiation Dosage rate is 100~200kGy/h, and irradiation dose is 200~1000kGy, and mixing speed is 100~150r/min；The dispersion Agent accounts for nano-attapulgite quality 1~3%；The dispersing agent is 1- ethyl-3-methylimidazole acetate.
10. the method for preparing super-hydrophobic oxidant based on lotus leaf effect as described in claim 1, which is characterized in that the step It further include that the super-hydrophobic oxidizing agent pellets that will be obtained are reprocessed after rapid two, process are as follows: send super-hydrophobic oxidizing agent pellets Enter in atmos low-temperature plasma device, super-hydrophobic oxidizing agent pellets is made to be in the jet exit of atmos low-temperature plasma Locate 20~60mm, the throughput in atmos low-temperature plasma device according to 8~12L/h is passed through gas medium, applies work Make voltage, form plasma jet, control the movement speed of the jet exit of atmos low-temperature plasma device 5~ 10mm/s makes plasma jet injection on super-hydrophobic oxidizing agent pellets, to super-hydrophobic oxidizing agent pellets carry out processing 30~ 60min；The operating voltage is provided using high-voltage ac power, and the operating voltage is the alternating voltage of 50~100kV, frequency For 100~300kHz；The gas medium is rare gas/oxygen, oxygen, nitrogen, ammonia, CF4、CCl4、SF6One of Or a variety of mixing.
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CN113415809A (en) * 2021-06-10 2021-09-21 湖北航天化学技术研究所 Spherical ADN particle, preparation method and application thereof
CN113634469A (en) * 2021-07-21 2021-11-12 江苏大学 CuO/SiO2Preparation method and application of desert beetle-like bionic membrane material
CN115806458A (en) * 2022-12-06 2023-03-17 西安近代化学研究所 Modified nitrocotton coating material, preparation method and application thereof
CN116947576A (en) * 2022-04-20 2023-10-27 北京理工大学 Simple preparation method of polyhedral oligomeric silsesquioxane coated dinitramide ammonium

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CN103880569A (en) * 2014-03-24 2014-06-25 西安近代化学研究所 Surface modification and coating method for ammonium dinitramide
CN106976881A (en) * 2017-04-26 2017-07-25 清华大学深圳研究生院 A kind of method of modifying of activated carbon and application

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CN110963872A (en) * 2019-11-15 2020-04-07 上海航天化工应用研究所 Modified oxidant for high-burning-speed solid propellant and preparation method thereof
CN113415809A (en) * 2021-06-10 2021-09-21 湖北航天化学技术研究所 Spherical ADN particle, preparation method and application thereof
CN113634469A (en) * 2021-07-21 2021-11-12 江苏大学 CuO/SiO2Preparation method and application of desert beetle-like bionic membrane material
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CN115806458A (en) * 2022-12-06 2023-03-17 西安近代化学研究所 Modified nitrocotton coating material, preparation method and application thereof
CN115806458B (en) * 2022-12-06 2024-03-29 西安近代化学研究所 Modified nitrocotton coating material, preparation method and application thereof

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