CN102581272A - Method for preparing nanometer aluminum composite powder coated with nitro-cotton - Google Patents
Method for preparing nanometer aluminum composite powder coated with nitro-cotton Download PDFInfo
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- CN102581272A CN102581272A CN2012100252658A CN201210025265A CN102581272A CN 102581272 A CN102581272 A CN 102581272A CN 2012100252658 A CN2012100252658 A CN 2012100252658A CN 201210025265 A CN201210025265 A CN 201210025265A CN 102581272 A CN102581272 A CN 102581272A
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Abstract
The invention discloses a method for preparing nanometer aluminum composite powder coated with nitro-cotton. The method includes the steps of: dispersing nanometer aluminum powder into absolute ethyl alcohol; adding silane coupling agent with the weight accounting for 5-10% of that of the nanometer aluminum powder to obtain nanometer aluminum powder treated by the silane coupling agent; dissolving the nitro-cotton and plasticizer into ethyl acetate or acetone; dispersing the nanometer aluminum powder treated by the silane coupling agent into cyclohexane to form cyclohexane dispersing agent; adding nitro-cotton liquor into the cyclohexane dispersing agent and evenly mixing the nitro-cotton liquor; and performing filtering and vacuum drying to obtain the nanometer aluminum composite powder coated with the nitro-cotton, wherein the weight of the nitro-cotton is 0.04-0.15 time that of the aluminum powder, and the weight of the plasticizer accounts for 3-10% of that of the nitro-cotton. The nanometer aluminum powder is firstly treated by the silane coupling agent and then coated with the nitro-cotton, the surface of the nanometer aluminum powder is effectively coated with the nitro-cotton, the activity of the nanometer aluminum powder can be kept, and the oxidation resistance of the nanometer aluminum powder is improved.
Description
Technical field
The present invention relates to a kind of preparation method of coated with Nitrocellulose nano aluminum composite granule, this composite granule can be used as modified double base propellant (CMDB) and nitrate ester plasticized polyether propellant (NEPE) is used efficient metal fuel, belongs to the nano material preparation technical field.
Background technology
Aluminium powder is one of modern solid rocket propellant additive commonly used.Adding aluminium powder is to increase energy, the most effective and the most with practical value method of inhibition rocket engine rough burning.Aluminium powder is because high, the high enthalpy of combustion of density and quite remarkable to the specific impulse effect that improves solid propellant, adds to draw materials abundantly, and cost is lower, is therefore extensively adopted.Yet; The ignition delay time of common aluminium powder and micron order aluminium powder is long, efficiency of combustion is lower; And in the propellant combustion process, be prone to reunite and form big dripping with fixed attention, thereby cause the two phase flow of jet pipe to lose and form defectives such as plumage cigarette discharge surperficial generation of propellant combustion.
Nanometer aluminium powder plays an important role in energetic material fields such as propellant, explosive and thermite because its excellent heat discharges and the low-temperature oxidation ability.But the nano aluminum particle has special volume and skin effect, makes it be in the height state of activation, and is very responsive to environment of living in; Easily and gas, fluid molecule generation reciprocation in the environment; Make to be exposed to the very easily oxidation of airborne nano aluminum particle surface, even spontaneous combustion in air, thereby cause the decline of nano aluminum particle stability and lose its activity; Bring very big difficulty for storage and use, make its application in solid propellant receive very big restriction.
Coat layer protecting film on the surface of nano aluminum particle and form nano level nucleocapsid structure, particle surface character is changed, isolate the aluminium nano particle of activity and contacting of surrounding environment, thereby the activated aluminum of protection kernel is not by further oxidation.It is a kind of effective ways that improve nanometer Al mealiness ability that the surface coats, and it not only can effectively solve reunites and problem of oxidation, but also can effectively improve the efficiency of combustion of aluminium powder, and selects for use special coating can also give the Al powder new function.
Nitrocotton is claimed nitrocellulose again; It is important component and additive in CMDB propellant and the NEPE propellant; Adopt nitrocotton that nanometer aluminium powder is carried out the surface and coat processing, can prevent that not only its oxidation from also can effectively improve the dispersiveness of nanometer aluminium powder in propellant.[Applied Surface Science such as Young-Soon Kwon; 2007; The nanometer aluminium powder that 273 (12): 5558-5564] will adopt the discharge-induced explosion method to make joins rapidly in the ethanolic solution of NC; About 2 h of mechanical agitation under 30 ° of C, residual solvent at room temperature carries out vacuum drying treatment, has made the nanometer aluminium powder by coated with Nitrocellulose.But because the nitrocotton molecule is rigidity, and has only the effect of molecular separating force between nitrocotton and the nanometer aluminium powder, therefore; Adopt this method directly nanometer aluminium powder to be added in the solution of nitrocotton; Can cause the nanometer aluminium powder surface to coat not exclusively, oxidation resistance is poor, is prone to form big defectives such as reunion.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can form fine and close protective layer, improve the preparation method of coated with Nitrocellulose nanometer aluminium powder of dispersiveness and the oxidation resistance of nanometer aluminium powder, for application in double-basis and the modified double base propellant provides technical foundation on the nanometer aluminium powder surface.
Implementation procedure of the present invention is following:
A kind of preparation method of coated with Nitrocellulose nano aluminum composite granule may further comprise the steps:
(1) under nitrogen protection, nanometer aluminium powder is dispersed in the absolute ethyl alcohol;
(2) silane coupler with nanometer aluminium powder quality 5 ~ 10 % adds in step (1) solution, the dry nanometer aluminium powder that gets the silane coupler processing of dispersed with stirring final vacuum;
(3) aluminium powder quality 0.04-0.15 nitrocotton doubly and the plasticizer that accounts for nitrocotton quality 3 ~ 10 % are dissolved in ethyl acetate or the acetone;
(4) nanometer aluminium powder of step (2) silane coupler being handled is scattered in and forms the cyclohexane dispersion liquid in the cyclohexane;
(5) stir down, the nitrocellulose solution of step (3) is added to mix in the cyclohexane dispersion liquid;
(6) the nano aluminum composite granule that filter, vacuum drying gets coated with Nitrocellulose.
Said nanometer aluminium powder average grain diameter is 40 ~ 60 nm.
Step (5) reaction temperature is controlled at 40 ~ 45 ° of C.
Said silane coupler is KH-550 (gamma-aminopropyl-triethoxy-silane), KH-560 (γ-glycidyl ether oxygen propyl trimethoxy silicane), KH-570 (γ-(methacryloxypropyl) propyl trimethoxy silicane), KH-580 (γ-mercaptopropyl trimethoxysilane), silane coupling A-171 (vinyltrimethoxy silane) silane coupling A-151 (VTES), silane coupler CG-103 (MTMS) etc., preferably gamma-aminopropyl-triethoxy-silane.
Said plasticizer is diethyl phthalate (DEP) or dibutyl phthalate (DBP).
Advantage of the present invention and good effect: (1) is because nitrocotton is important component and additive in CMDB propellant and the NEPE propellant; Therefore; Nanometer aluminium powder after the employing coated with Nitrocellulose is handled is when keeping the nanometer aluminium powder reactivity; Have good compatibility with propellant component again, and can prevent to reunite; (2) nanometer aluminium powder is handled with silane coupler earlier, adopts coated with Nitrocellulose then, has realized the effective coating of nitrocotton on the nanometer aluminium powder surface, can keep the activity of nanometer aluminium powder, improves its antioxygenic property; (3) preparation method of the present invention is simple, and is easy to operate, and manufacturing cycle is short, easy control of reaction conditions.
Description of drawings
Fig. 1 is the SEM photo of the product of the embodiment of the invention 1,2 and 3 preparations;
Fig. 2 is the XRD spectra of the product of the embodiment of the invention 1,2 and 3 preparations;
Fig. 3 be the embodiment of the invention 1,2 and 3 the preparation product at air at room temperature following time of condition-mass change curve.
The specific embodiment
Embodiment 1
Taking by weighing 4.0 g average grain diameters is the nanometer aluminium powder of 50 nm, adds in the 100 mL absolute ethyl alcohols, and ultrasonic dispersion 30 min are uniformly dispersed nanometer aluminium powder in absolute ethyl alcohol; Take by weighing 0.2 g silane resin acceptor kh-550; Join in the absolute ethyl alcohol suspension of the nanometer aluminium powder after ultrasonic dispersion; Continue ultrasonic dispersion 10 min, in the water bath with thermostatic control of 60 ° of C, stir 2 h, leave standstill with glue head dropper and remove supernatant liquor; Dry 8 h make the nanometer aluminium powder after coupling agent treatment in the vacuum drying oven of 60 ° of C; Take by weighing 5.0 g nitrocottons and 0.5 g diethyl phthalate (DEP) is dissolved in the 1000 mL ethyl acetate, and be aided with the ultrasonic wave dissolving, be configured to 5.0 gL
-1Nitrocellulose solution; Take by weighing the nanometer aluminium powder of 2.0 g after coupling agent treatment, add in the 100 mL cyclohexanes, ultrasonic dispersion 30 min form homodisperse cyclohexane suspension; Continuing under the stirring action, the rate of addition of above-mentioned 19.0 mL nitrocellulose solutions with 1 ~ 2 droplet/second added in the cyclohexane suspension, dropwising continued and stir 12 h, fluid temperature is controlled in 40 ~ 45 ° of C scopes in the whole process; After stirring end, solution left standstill is made its Separation of Solid and Liquid, filter and also in the vacuum drying oven of 60 ° of C, take out the nano aluminum composite granule that is coated with Nitrocellulose behind dry 12 h.Fig. 1 a is the SEM photo of product.Photo shows that nitrocotton can effectively be coated on the nanometer aluminium powder surface, compares with the raw material nano aluminium powder, and the aluminium powder particle diameter obviously increases, and is dispersed better.Can find out in the XRD spectra of Fig. 2 a that the characteristic peak of this composite granule and the characteristic peak of aluminium match, and only have a small amount of non crystalline structure.The result of Fig. 3 a shows that the nano aluminum composite granule of this method preparation has good antioxygenic property in air.
Taking by weighing 4.0 g average grain diameters is the nanometer aluminium powder of 50 nm, adds in the 100 mL absolute ethyl alcohols, and ultrasonic dispersion 30 min are uniformly dispersed nanometer aluminium powder in absolute ethyl alcohol; Take by weighing 0.32 g silane coupler KH-560; Join in the absolute ethyl alcohol suspension of the nanometer aluminium powder after ultrasonic dispersion; Continue ultrasonic dispersion 10 min, in the water bath with thermostatic control of 60 ° of C, stir 2 h, leave standstill with glue head dropper and remove supernatant liquor; Dry 8 h make the nanometer aluminium powder after coupling agent treatment in the vacuum drying oven of 60 ° of C; Take by weighing 5.0 g nitrocottons and 0.4 g dibutyl phthalate (DEP) is dissolved in the 1000 mL ethyl acetate, and be aided with the ultrasonic wave dissolving, be configured to 5.0 gL
-1Nitrocellulose solution; Take by weighing the nanometer aluminium powder of 2.0 g after coupling agent treatment, add in the 100 mL cyclohexanes, ultrasonic dispersion 30 min form homodisperse cyclohexane suspension; Continuing under the stirring action, the rate of addition of above-mentioned 37 mL nitrocellulose solutions with 1 ~ 2 droplet/second added in the cyclohexane suspension, dropwising continued and stir 12 h, fluid temperature is controlled in 40 ~ 45 ° of C scopes in the whole process; After stirring end, solution left standstill is made its Separation of Solid and Liquid, filter and also in the vacuum drying oven of 60 ° of C, take out the nano aluminum composite granule that is coated with Nitrocellulose behind dry 12 h.Fig. 2 b is the SEM photo of product.From Fig. 1 b, can find out, between the nanometer aluminium powder after the coated with Nitrocellulose, bonding effect take place, nitrocotton coats fully on the nanometer aluminium powder surface.Can find out in the XRD spectra of Fig. 2 b that the characteristic peak of this composite granule and the characteristic peak of aluminium match, and only have a small amount of non crystalline structure.The result of Fig. 3 b shows that the nano aluminum composite granule of this method preparation has good antioxygenic property in air.
Embodiment 3
Taking by weighing 4.0 g average grain diameters is the nanometer aluminium powder of 50 nm, adds in the 100 mL absolute ethyl alcohols, and ultrasonic dispersion 30 min are uniformly dispersed nanometer aluminium powder in absolute ethyl alcohol; Take by weighing 0.24 g silane coupler CG-103; Join in the absolute ethyl alcohol suspension of the nanometer aluminium powder after ultrasonic dispersion; Continue ultrasonic dispersion 10 min, in the water bath with thermostatic control of 60 ° of C, stir 2 h, leave standstill with glue head dropper and remove supernatant liquor; Dry 8 h make the nanometer aluminium powder after coupling agent treatment in the vacuum drying oven of 60 ° of C; Take by weighing 5.0 g nitrocottons and 0.3g dibutyl phthalate (DBP) is dissolved in the 1000 mL acetone, and be aided with the ultrasonic wave dissolving, be configured to 5.0 gL
-1Nitrocellulose solution; Take by weighing the nanometer aluminium powder of 2.0 g after coupling agent treatment, add in the 100 mL cyclohexanes, ultrasonic dispersion 30 min form homodisperse cyclohexane suspension; Continuing under the stirring action, the rate of addition of above-mentioned 40 mL nitrocellulose solutions with 1 ~ 2 droplet/second added in the cyclohexane suspension, dropwising continued and stir 12 h, fluid temperature is controlled in 40 ~ 45 ° of C scopes in the whole process; After stirring end, solution left standstill is made its Separation of Solid and Liquid, filter and also in the vacuum drying oven of 60 ° of C, take out the nano aluminum composite granule that is coated with Nitrocellulose behind dry 12 h.Fig. 1 c is the SEM photo of product.As can be seen from the figure, the nanometer aluminium powder particle of coated with Nitrocellulose is spherical in shape, evenly, good dispersiveness is arranged all.Can find out in the XRD spectra of Fig. 2 c that the characteristic peak of this composite granule and the characteristic peak of aluminium match, and have non crystalline structure hardly.The result of Fig. 3 c shows that the nano aluminum composite granule of this method preparation has good antioxygenic property in air.
Claims (6)
1. the preparation method of a coated with Nitrocellulose nano aluminum composite granule is characterized in that may further comprise the steps:
(1) under nitrogen protection, nanometer aluminium powder is dispersed in the absolute ethyl alcohol;
(2) silane coupler with nanometer aluminium powder quality 5 ~ 10 % adds in step (1) solution, the dry nanometer aluminium powder that gets the silane coupler processing of dispersed with stirring final vacuum;
(3) aluminium powder quality 0.04-0.15 nitrocotton doubly and the plasticizer that accounts for nitrocotton quality 3 ~ 10 % are dissolved in ethyl acetate or the acetone;
(4) nanometer aluminium powder of step (2) silane coupler being handled is scattered in and forms the cyclohexane dispersion liquid in the cyclohexane;
(5) stir down, the nitrocellulose solution of step (3) is added to mix in the cyclohexane dispersion liquid;
(6) the nano aluminum composite granule that filter, vacuum drying gets coated with Nitrocellulose.
2. the preparation method of coated with Nitrocellulose nano aluminum composite granule according to claim 1 is characterized in that: said nanometer aluminium powder average grain diameter is 40 ~ 60 nm.
3. the preparation method of coated with Nitrocellulose nano aluminum composite granule according to claim 1 is characterized in that: step (5) reaction temperature is controlled at 40 ~ 45 ° of C.
4. the preparation method of coated with Nitrocellulose nano aluminum composite granule according to claim 1 is characterized in that: said silane coupler is KH-550, KH-560, KH-570, KH-580, A-150, A-171, A-151, CG-103.
5. the preparation method of coated with Nitrocellulose nano aluminum composite granule according to claim 4 is characterized in that: said silane coupler is KH-550.
6. the preparation method of coated with Nitrocellulose nano aluminum composite granule according to claim 1 is characterized in that: said plasticizer is selected from diethyl phthalate, dibutyl phthalate.
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| CN103752820A (en) * | 2014-02-19 | 2014-04-30 | 南京林业大学 | Method for preparing modified nanometer cobalt powder |
| CN104043826A (en) * | 2014-07-02 | 2014-09-17 | 广东新劲刚新材料科技股份有限公司 | Aluminum powder surface hydration processing method and application of aluminum powder in preparing Al@Ag nuclear shell composite particle conductive and electromagnetic shielding filler |
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| CN104043826A (en) * | 2014-07-02 | 2014-09-17 | 广东新劲刚新材料科技股份有限公司 | Aluminum powder surface hydration processing method and application of aluminum powder in preparing Al@Ag nuclear shell composite particle conductive and electromagnetic shielding filler |
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| CN106964771B (en) * | 2017-05-16 | 2018-09-14 | 合肥学院 | A kind of characterizing method of the control method of superfine Mg powder oxygen content, oxidation resistance |
| CN106964771A (en) * | 2017-05-16 | 2017-07-21 | 合肥学院 | A kind of control method of superfine Mg powder oxygen content, the characterizing method of oxidation resistance |
| CN107812938A (en) * | 2017-12-04 | 2018-03-20 | 中国工程物理研究院化工材料研究所 | A kind of pre- method of agglomeration of the micro-meter scale of nanometer aluminium powder |
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| CN109128147A (en) * | 2018-07-13 | 2019-01-04 | 南京理工大学 | A kind of surface coating method of ball aluminum powder |
| CN109824464A (en) * | 2019-02-25 | 2019-05-31 | 谭亚 | A kind of preparation method of dispersing type resistance to oxidation boron magnesium composite granule |
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| CN112643025A (en) * | 2020-11-20 | 2021-04-13 | 南京理工大学 | Preparation method of high-reactivity nano aluminum/copper oxide microspheres |
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