CN108163839A - A kind of method that carbon nanotube coats three aluminum hydrides - Google Patents
A kind of method that carbon nanotube coats three aluminum hydrides Download PDFInfo
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- CN108163839A CN108163839A CN201810031352.1A CN201810031352A CN108163839A CN 108163839 A CN108163839 A CN 108163839A CN 201810031352 A CN201810031352 A CN 201810031352A CN 108163839 A CN108163839 A CN 108163839A
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- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
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Abstract
A kind of method that carbon nanotube coats three aluminum hydrides, includes the following steps：1) three aluminum hydrides and organic amine are formed into complex, by amine exchange reaction, prepares three hydrogenation aluminum solutions；2) in certain density salpeter solution, carbon nanotube is carried out to prescind processing；3) carbon nanotube after prescinding with three hydrogenation aluminum solutions is mixed, under catalyst action, three aluminum hydrides is precipitated in carbon nanotube, three aluminum hydrides of carbon nanotube cladding are obtained after filtration drying.The present invention, which solves current three aluminum hydride, can not be covered by the problems in nano level carbon nanotube, solid propellant fuel, catalyst, hydrogen storage material and fuel cell etc. can be efficiently applied to, while also the preparation for three aluminum hydride of nanoscale provides a kind of technological approaches.
Description
Technical field
The invention belongs to the methods of technical field of material, more particularly to a kind of three aluminum hydrides of carbon nanotube cladding.
Background technology
Three aluminum hydrides have many advantages, such as that the combustion heat is high, flame temperature is low, good into gas relative to aluminium powder, and granularity is generally several
Hundred microns, it is considered as the high-energy fuel for most having development potentiality, great expectations is sent in solid propellant field.
But three aluminum hydrides are made of the element of two kinds of strong reducing properties, and redox reaction and hydrolysis easily occurs,
With relatively low chemical stability and thermal stability, with energetic binder there are great incompatibility in solid propellant,
Solid propellant security performance is caused drastically to decline.
Three aluminum hydrides are coated using carbon nanotube (diameter several nanometers to several tens of nanometers), nano level three aluminum hydride after cladding
The efficiency of combustion of solid propellant can not only be increased with carbon nanotube, improve its energy characteristics, while realize three aluminum hydrides
With the physical isolation of energetic binder, compatibility is improved, has ensured security performance.In addition, nano level three hydrogenation after cladding
Aluminium also has preferable application prospect in fields such as hydrogen storage material, fuel cell, catalyst.
Invention content
The present invention is intended to provide a kind of method that carbon nanotube coats three aluminum hydrides.
The technical scheme is that a kind of method that carbon nanotube coats three aluminum hydrides, includes the following steps：
Step a)：The preparation of three hydrogenation aluminum solutions, specifically includes step a1) and a2)；
a1)：Under protective gas protection, organic amine is added in into three aluminum hydrides, the amount of the organic amine substance is three
0.5 times -15 times of aluminum hydride, add toluene solvant, and the amount of the toluene solvant of addition is 1 times -20 of organic amine by volume
Times, it then heats 25 DEG C -65 DEG C, be refluxed 3h-20h, suction filtration removes insoluble matter, obtains filtrate；
a2)：To step a1) in add in triethylamine in obtained filtrate, the volume of the triethylamine is the 1-10 of organic amine
Times, add toluene solvant (because in step a1) and have been added to toluene solvant, if step a1) in the toluene that adds in foot
It is more than enough, in this step can no longer plus toluene solvant, but step a1) heating process in have toluene solvant evaporation, if step
Rapid a1) in add in toluene be not enough, toluene solvant, the volume of the toluene solvant of addition can be added in this step
It is that organic amine is more than 0 times to 10 times), under protective gas protection, 25 DEG C -65 DEG C are refluxed 1h-15h to get to three
Aluminum solutions are hydrogenated, shown in reaction equation such as formula (1) and formula (2)：
Further, above-mentioned steps a1) in protective gas be nitrogen, argon gas, the mixing of one or more of helium.
Further, above-mentioned steps a1) in organic amine include trimethylamine, N, N- dimethyl amines, N, N- diethyl first
It is one or more in amine and N-Methyl pyrrolidone.
Further, above-mentioned steps a1) in the amount of organic amine substance that adds in be 0.5 times -15 times of three aluminum hydrides, add in
The volume of toluene solvant be 1 times -20 times of organic amine.
Further, above-mentioned steps a2) in add in the volume of triethylamine be 1-10 times of organic amine.
Further, above-mentioned steps a2) addition organic amine after, be refluxed before, further include add in toluene it is molten
The step of agent, the amount of the toluene solvant of addition are more than 0 times to 10 times for organic amine by volume.
Step b)：Carbon nanotube prescinds processing
Salpeter solution is added in into carbon nanotube, the sonic oscillation time is not less than 5min, and 80 DEG C -160 DEG C are refluxed 1h-
15h, filtering, while adopt and solid product is washed with deionized, heating solid product is to get the carbon nanotube to after prescinding.
Further, a concentration of 0.5mol/L-10mol/L of above-mentioned salpeter solution, the quality of salpeter solution is carbon nanometer
50 times or more of pipe.
Further, above-mentioned washing solid matter with deionized water quality is 50 times or more of carbon nanotube, heats solid
The temperature of product is 40 DEG C -150 DEG C, and the time is not less than 2h.
Step c)：Carbon nanotube coats the processing of three aluminum hydrides
Carbon nanotube after prescinding obtained by step b) is added in into step a2) obtained by three hydrogenation aluminum solutions in, mixing is stirred
More than 10min is mixed, three hydrogenation aluminum solutions is made to be full of carbon nanotube, are then slowly added into a small amount of lithium aluminium hydride reduction (as catalyst),
Protective gas protection is lower to heat, and is refluxed, the reaction equation such as formula (3) that three hydrogenation aluminum solutions in carbon nanotube occur
Shown, filtering, solid product heats in a vacuum, obtains three aluminum hydride products of carbon nanotube cladding.
Further, above-mentioned addition step a2) obtained by three hydrogenation aluminum solutions in the quality for prescinding rear carbon nanotube be
Step a2) obtained by 0.1 times -10 times of three aluminum hydrides.
Further, the lower heating temperature heated of above-mentioned protective gas protection is 25 DEG C -65 DEG C, the time being refluxed
For 1h-15h.
Further, the temperature that above-mentioned solid product heats in a vacuum in the range of 20 DEG C -60 DEG C, the time be not less than
1h。
The present invention by the three hydrogenation preparations of aluminum solutions, carbon nanotube prescind processing and carbon nanotube coats three aluminum hydrides
Processing and etc. realize carbon nanotube coat three aluminum hydride techniques, solid propellant fuel, catalyst, storage can be efficiently applied to
Hydrogen material and fuel cell etc., while also the preparation for three aluminum hydride of nanoscale provides a kind of technological approaches.The present invention is raw
Production method is simple, production cost is low and safe and reliable.
Description of the drawings
From the detailed description below in conjunction with the accompanying drawings to the embodiment of the present invention, these and/or other aspects of the invention and
Advantage will become clearer and be easier to understand, wherein：
Attached drawing 1 coats the transmission electron microscope figure of three aluminum hydride products for the carbon nanotube that the embodiment of the present invention 1 obtains,
Wherein Fig. 1 (a) is the transmission electron microscope figure of 20nm scales；Fig. 1 (b) is the transmission electron microscope figure of 20nm scales.
Fig. 2 is the thermogram that the carbon nanotube that the embodiment of the present invention 1 obtains coats three aluminum hydride products.
Specific embodiment
In order to which those skilled in the art is made to more fully understand the present invention, with reference to the accompanying drawings and detailed description to this hair
It is bright to be described in further detail.Here it is to be noted that it in the accompanying drawings, identical reference numeral imparting is substantially had
The component part of same or like structure and function, and will omit about their repeated description.
1 carbon nanotube of embodiment coats the technique of three aluminum hydrides, includes the following steps：
Step 1：Under nitrogen protection, the N of 30mL, N- dimethyl amine solution are added in into tri- aluminum hydrides of 0.3g, then is added
Enter 90mL toluene solvants, 40 DEG C of heating is refluxed 5h, and suction filtration removes insoluble matter, 60mL triethylamines is added in into filtrate, then add
Enter 30mL toluene solvants, under nitrogen protection, 40 DEG C are refluxed 5h, obtain three hydrogenation aluminum solutions.
Step 2：The salpeter solution of a concentration of 2mol/L of 100mL, sonic oscillation time are added in into 0.2g carbon nanotubes
20min, 140 DEG C are refluxed 2h, filtering, while using 150mL deionized waters washing solid product, by solid product at 65 DEG C
Lower dry 3h is to get the carbon nanotube to after prescinding.
Step 3：Carbon nanotube coats the processing of three aluminum hydrides
Carbon nanotube after step 2 is prescinded is added in three hydrogenation aluminum solutions of step 1, and 30min is mixed, makes three hydrogen
Change aluminum solutions full of carbon nanotube, be then slowly added into 0.05g lithium aluminium hydride reduction catalyst, heat 40 DEG C under nitrogen protection, return
Stream stirring 5h, filtering, solid product heating in vacuum 5h at 40 DEG C obtain the three aluminum hydride products that carbon nanotube coats.
2 carbon nanotube of embodiment coats the technique of three aluminum hydrides, includes the following steps：
Step 1：Under nitrogen protection, the N-Methyl pyrrolidone solution of 40mL is added in into tri- aluminum hydrides of 0.5g, then is added
Entering 130mL toluene solvants, 45 DEG C of heating is refluxed 5h, and suction filtration removes insoluble matter, and 80mL triethylamines are added in into filtrate, then
50mL toluene solvants are added in, under nitrogen protection, 45 DEG C are refluxed 5h, obtain three hydrogenation aluminum solutions.
Step 2：The salpeter solution of a concentration of 3mol/L of addition 130mL into 0.35g carbon nanotubes, sonic oscillation 30min,
100 DEG C are refluxed 3h, filtering, while using 200mL deionized waters washing solid product, and solid product is dry at 65 DEG C
4h is to get the carbon nanotube to after prescinding.
Step 3：Carbon nanotube coats the processing of three aluminum hydrides
Carbon nanotube after step 2 is prescinded is added in three hydrogenation aluminum solutions of step 1, and 30min is mixed, makes three hydrogen
Change aluminum solutions full of carbon nanotube, be then slowly added into 0.1g lithium aluminium hydride reduction catalyst, heat 35 DEG C under nitrogen protection, reflux
10h, filtering are stirred, solid product heating in vacuum 8h at 45 DEG C obtains the three aluminum hydride products that carbon nanotube coats.
Fig. 1 is the transmission electron microscope figure that carbon nanotube of the embodiment of the present invention coats three aluminum hydride products, and Fig. 2 is this hair
Bright embodiment carbon nanotube coats the thermogram of three aluminum hydride products.As seen from Figure 1, three aluminum hydrides are successfully loaded
In carbon nanotube；As seen from Figure 2, carbon nanotube coats the typical weightlessness for having three aluminum hydrides in three aluminum hydride products and puts
Thermal spike, no other impurity peaks；Therefore, the product of three aluminum hydrides of carbon nanotube cladding has obtained.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.In the case of without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes will be apparent from for the those of ordinary skill in art field.Therefore, protection scope of the present invention should
This is subject to the protection scope in claims.
Claims (11)
1. a kind of method that carbon nanotube coats three aluminum hydrides, which is characterized in that include the following steps：
a1)：Under protective gas protection, organic amine is added in into three aluminum hydrides, adds toluene solvant, heats 25 DEG C -65
DEG C, be refluxed 3h-20h, suction filtration removes insoluble matter, obtains filtrate；
a2)：To step a1) obtained by filtrate in add in triethylamine, protective gas protection under, 25 DEG C -65 DEG C are refluxed
1h-15h obtains three hydrogenation aluminum solutions；
b)：Salpeter solution is added in into carbon nanotube, carries out sonic oscillation, the time is not less than 5min, then is returned at 80 DEG C -160 DEG C
Then stream stirring 1h-15h, filtering are washed with deionized solid product, heat solid product later, the carbon after being prescinded
Nanotube；
c)：Carbon nanotube after prescinding obtained by step b) is added in into step a2) obtained by three hydrogenation aluminum solutions in, be mixed
More than 10min makes three hydrogenation aluminum solutions be then slowly added into a small amount of lithium aluminium hydride reduction, protective gas protection full of carbon nanotube
Lower heating, is refluxed, and filtering, solid product heats in a vacuum, obtains three aluminum hydride products of carbon nanotube cladding.
2. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that the step a1) in
Protective gas be nitrogen, argon gas, the mixing of one or more of helium.
3. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that the step a1) in
Organic amine include trimethylamine, N, N- dimethyl amines, N, one kind or more in N- diethyl methyl amines and N-Methyl pyrrolidone
Kind.
4. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that the step a1) in
The amount of the organic amine of addition is calculated as 0.5 times -15 times of three aluminum hydrides by the amount of substance, and the amount of the toluene solvant of addition is by volume
1 times -20 times for organic amine.
5. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that the step a2) in
The amount for adding in triethylamine is 1-10 times of organic amine by volume.
6. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that the step a2) in
Addition organic amine after, be refluxed before, further include add in toluene solvant the step of, the amount of the toluene solvant of addition presses body
Product be calculated as organic amine be more than 0 times to 10 times.
7. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that add in the step b)
A concentration of 0.5mol/L-10mol/L of the salpeter solution entered, the quality of salpeter solution are 50 times or more of carbon nanotube.
8. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that washed in the step b)
It washs with 50 times or more of the amount of deionized water by mass for carbon nanotube；The heating temperature of solid product is heated at 40 DEG C -150
In the range of DEG C, heating time is not less than 2h.
9. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that add in the step c)
It is step a2 to enter the amount of the carbon nanotube after prescinding in three hydrogenation aluminum solutions by quality) in 0.1-10 times of three aluminum hydrides.
10. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that in the step c)
The heating temperature heated under protective gas protection is 25 DEG C -65 DEG C, and the time being refluxed is 1h-15h.
11. the method that carbon nanotube according to claim 1 coats three aluminum hydrides, which is characterized in that in the step c)
The temperature that heats in a vacuum of solid product in the range of 20 DEG C -60 DEG C, the time is not less than 1h.
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| CN201810031352.1A CN108163839B (en) | 2018-01-12 | 2018-01-12 | Method for coating aluminum trihydride on carbon nano tube |
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| CN201810031352.1A CN108163839B (en) | 2018-01-12 | 2018-01-12 | Method for coating aluminum trihydride on carbon nano tube |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019507A (en) * | 2018-09-03 | 2018-12-18 | 黎明化工研究设计院有限责任公司 | A method of improving three aluminium hydride thermostabilisations |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8153554B2 (en) * | 2006-11-15 | 2012-04-10 | University Of South Carolina | Reversible hydrogen storage materials |
| CN106006556A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Regeneration method of aluminum trihydride |
| CN106410210A (en) * | 2016-10-31 | 2017-02-15 | 复旦大学 | Preparation method of metal hydride/nano carbon composite materials |
-
2018
- 2018-01-12 CN CN201810031352.1A patent/CN108163839B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8153554B2 (en) * | 2006-11-15 | 2012-04-10 | University Of South Carolina | Reversible hydrogen storage materials |
| CN106006556A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Regeneration method of aluminum trihydride |
| CN106410210A (en) * | 2016-10-31 | 2017-02-15 | 复旦大学 | Preparation method of metal hydride/nano carbon composite materials |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019507A (en) * | 2018-09-03 | 2018-12-18 | 黎明化工研究设计院有限责任公司 | A method of improving three aluminium hydride thermostabilisations |
| CN109019507B (en) * | 2018-09-03 | 2021-11-05 | 黎明化工研究设计院有限责任公司 | Method for improving thermal stability of aluminum trihydride |
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