CN107597062A - A kind of preparation method of galapectite multistage hydridization gas adsorption material - Google Patents
A kind of preparation method of galapectite multistage hydridization gas adsorption material Download PDFInfo
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- CN107597062A CN107597062A CN201711067411.2A CN201711067411A CN107597062A CN 107597062 A CN107597062 A CN 107597062A CN 201711067411 A CN201711067411 A CN 201711067411A CN 107597062 A CN107597062 A CN 107597062A
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Abstract
A kind of preparation method of galapectite multistage hydridization gas adsorption material disclosed in this invention, carbon hydridization halloysite nanotubes shape material is obtained using sucrose and natural galapectite are compound, and introduce precious metal palladium and three-component compound system is obtained to its further modification, regulate and control to obtain carbon-coating-palladium-galapectite multistage hydridization tubular composite material by combination process.The sandwich type composite at room temperature, 2.65MPa hydrogen adsorption capacity be up to 0.6wt%~0.8wt%.The raw material that this method prepares material are cheap and easy to get, and preparation method is simply efficient, and gas absorption performance is good and stability is good, are good hydrogen adsorption and tail gas adsorption processing material.
Description
Technical field
The invention belongs to field of material technology, designs a kind of preparation method of galapectite multistage hydridization gas adsorption material.
Background technology
Endlessly motor-vehicle tail-gas causes serious influence, motor vehicle exhaust emission production to the health of environment and the mankind
Raw NOx、COx、CHxDeng gas, the environmental contaminants more than 80% of its discharge are accounted for, it, which endangers, is mainly manifested in haze weather frequency
Hair, human respiratory system's disease etc..Therefore treating tail gas is environmental problem important in automobile industry.Simultaneously hydrogen energy source by
In its good sustainability, recyclability and its abundant energy supply the features such as, it is considered to be fossil fuel it is good
Substitute, and it provides possibility for the production of the zero-emission vehicles.But the utilization of hydrogen energy source is faced with production, fortune
It is defeated, storage the problems such as.
The physical absorption of solid material is received significant attention due to it to the flexibility of adsorbed gas release.Especially porous ore deposit
Thing service life length, has relatively high specific surface area, and high adsorption/desorption is compared under room temperature condition because its cost is low
Performance and paid special attention to.Natural galapectite is a kind of aqueous lamellar aluminosilicate in kaolin series, hollow tubular structure,
Formed by the lamella curling of many sub-millimeter dimensions.Nanotube is also due to its size, architectural characteristic bring potential application
Value is also by widely studied.Natural halloysite nanotubes have special physics, chemical property, such as higher specific surface area,
High porosity, and good cation exchange capacity (CEC).In view of the high porosity of galapectite, high-specific surface area, good adsorptivity
Can be with the advantageous property of natural minerals, it is considered as fabulous sorbing material.However, this absorption class material can not be abundant
The problems such as effective solution absorbs tail gas, hydrogen is fixed in absorption, the key of improving performance are to change material porosity characteristic and lead to
Suitable metal-modified is crossed, the absorption property of material is improved by its mechanism.Metal Palladium is the hydrogen-absorbing material found earliest,
Hydrogen-absorbing ability is extremely strong, while is also widely used in the fields such as tail gas catalyzed processing.
A kind of preparation method of galapectite multistage hydridization gas adsorption material disclosed in this invention, will using synthesis technique
There is the palladium metal granular absorption of high activity in galapectite surface to tail gas and hydrogen etc., and coat carbon-coating and further fix palladium
Grain finally obtains carbon-coating-palladium-galapectite multistage hydridization tubular composite material to construct three-component compound system.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of stable, more with higher specific surface area, chemical property
The preparation method of the level gas adsorption material that composite construction is clear and absorption property is good, the material is available for tail gas adsorption processing
With the field such as hydrogen adsorption.
In order to solve the above-mentioned technical problem, the preparation side of galapectite multistage hydridization gas adsorption material provided by the invention
Method, using galapectite as primary raw material, using sucrose as carbon source, palladium is chosen as the expensive gold of high activity for carrying gas sorption ability
Category, using following steps：
(1) 85mg palladium bichloride and 0.15g polyvinylpyrrolidone are weighed, is dissolved in 50ml methanol solutions；
(2) 2~3h is heated at reflux in 65~75 DEG C of constant temperature, obtains deep brown solution (PVP-PdCl2Solution)；
(3) 1g galapectite is added to 50ml PVP-PdCl2Used in solution after stirring -12~24h of staticaccelerator adsorption
Deionized water and ethanol cleaning, are subsequently placed at 100ml concentration to be reduced in 0.0375mol/L hydrazine hydrate alkaline solutions, wash, do
It is dry to obtain dark gray powder；
(4) it is 1 3g sucrose to be dissolved in into deionized water and ethanol volume ratio:By 1g after formation uniform solution in 1 mixed liquor
Black powder adds in above-mentioned (3), ultrasonic disperse 30min, and the stainless steel that polytetrafluoroethyllining lining is transferred to after 2~3h of stirring is anti-
Answer in kettle, in 170~190 DEG C of constant temperature 24h, then use absolute ethyl alcohol and deionized water rinsing, be dried for standby；
(5) gained brown-black powder is placed in vertical-type quartz pipe, with 5 DEG C/min heating rate liter under nitrogen atmosphere
Temperature is cooled to room temperature to 600 DEG C of calcining 3h under nitrogen atmosphere.
Using the preparation method of the galapectite multistage hydridization gas adsorption material of above-mentioned technical proposal, palladium particle is scattered, solid
Due between carbon-coating and galapectite, 0.7~2 μm of pipe average length, 30~75nm of external diameter, internal diameter 10~30nm, 5~10nm are thick
Carbon-coating is clear in structure visible.Hydrogen adsorption capacity of the multistage hydridization tubular material at room temperature, under the conditions of 2.65MPa is up to
0.6wt%~0.8wt%, there is higher gas sorption ability, durability is good, has important exploitation and application prospect.
Brief description of the drawings
Fig. 1 is the present invention with the transmission electron microscope shape appearance figure of multistage hybrid material made from embodiment 1.
Can significantly be observed from Fig. 1 has obvious line of demarcation between carbon-coating and galapectite, and carbon layers having thicknesses are about 5~
10nm, outside dimension is between 30~75nm.Palladium particle integrated distribution is tightly coated by carbon-coating in galapectite surface, is fixed.
Embodiment
The following examples are of the invention only for further illustrating, rather than the limitation present invention.The present invention can be by invention
Any mode described in content is implemented, and the invention will be further described with reference to the accompanying drawings and detailed description.
Embodiment 1：
85mg palladium bichloride and 0.15g polyvinylpyrrolidone are weighed, is dissolved in 50ml methanol solutions, Ran Hou
68 DEG C of constant temperature are heated at reflux 3h, obtain deep brown solution (PVP-PdCl2Solution).1g galapectite is added into the above-mentioned PVP- of 50ml
PdCl2Respectively rinsed three times with ethanol and deionized water after stirring-staticaccelerator adsorption 12h in solution, it is dense to be subsequently placed at 100ml
Spend to be reduced in 0.0375mol/L hydrazine hydrate alkaline solutions, then it is scrubbed, be dried to obtain dark gray powder.3g sucrose is dissolved in
Deionized water and ethanol volume ratio are 1:The above-mentioned black powders of 1g are added after uniform solution is formed in 1 mixed liquor, ultrasound point
30min is dissipated, brown suspension is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining after stirring 2h, using solvent heat
Method, in 170 DEG C of constant temperature 24h, then use absolute ethyl alcohol and deionized water rinsing, be dried for standby.Gained brown-black powder is put
In vertical-type quartz pipe, 600 DEG C of calcining 3h are warming up to 5 DEG C/min heating rate under nitrogen atmosphere, and in nitrogen atmosphere
Under be cooled to room temperature.Final product is obtained, hydrogen absorption capacity reaches 0.63wt% under room temperature condition.
Embodiment 2：
85mg palladium bichloride and 0.15g polyvinylpyrrolidone are weighed, is dissolved in 50ml methanol solutions, Ran Hou
75 DEG C of constant temperature are heated at reflux 2h, obtain deep brown solution (PVP-PdCl2Solution).1g galapectite is added into the above-mentioned PVP- of 50ml
PdCl2Respectively rinsed three times with ethanol and deionized water after stirring-staticaccelerator adsorption 18h in solution, it is dense to be subsequently placed at 100ml
Spend to be reduced in 0.0375mol/L hydrazine hydrate alkaline solutions, then it is scrubbed, be dried to obtain dark gray powder.3g sucrose is dissolved in
Deionized water and ethanol volume ratio are 1:The above-mentioned black powders of 1g are added after uniform solution is formed in 1 mixed liquor, ultrasound point
30min is dissipated, brown suspension is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining after stirring 3h, using solvent heat
Method, in 180 DEG C of constant temperature 24h, then use absolute ethyl alcohol and deionized water rinsing, be dried for standby.Gained brown-black powder is put
In vertical-type quartz pipe, 600 DEG C of calcining 3h are warming up to 5 DEG C/min heating rate under nitrogen atmosphere, and in nitrogen atmosphere
Under be cooled to room temperature.Final product is obtained, hydrogen absorption capacity reaches 0.68wt% under room temperature condition.
Claims (2)
- A kind of 1. galapectite multistage hydridization gas adsorption material, it is characterised in that：Using natural galapectite as raw material, with reference to noble metal Deposition, carbon-coating cladding process obtain 0.7~2 μm of average length, 30~75nm of external diameter, the carbon of internal diameter 10~30nm, 5~10nm thickness Rotating fields are clear and multistage hydridization tubular construction of the platinum grain interlayer between galapectite-carbon-coating.Adopt and be prepared by the following steps：(1) palladium bichloride is dissolved in the methanol solution containing polyvinylpyrrolidone, the 2~3h that then flowed back at 65~75 DEG C is obtained To stable auburn PVP-PdCl2Solution.(2) natural galapectite is impregnated in PVP-PdCl2Stirring -12~24h of staticaccelerator adsorption, is subsequently placed at hydrazine hydrate alkali in solution Reduced in property solution, wash, be dried to obtain dark gray powder.(3) above-mentioned powder is scattered in certain density sucrose alcohol solution, ultrasonic disperse 30min, shifted after stirring 2~3h Into the stainless steel cauldron of polytetrafluoroethyllining lining, in 170~190 DEG C of constant temperature 24h, then absolute ethyl alcohol and deionization are used Water is rinsed, is dried for standby.(4) powder is placed in vertical-type quartz pipe, and 600 DEG C of calcining 3h are warming up to 5 DEG C/min heating rate under nitrogen atmosphere, And it is cooled to room temperature under nitrogen atmosphere.
- 2. the preparation method of galapectite multistage hydridization gas adsorption material according to claim 1, it is characterised in that：(1) PVP-PdCl is first made2Galapectite surface is adsorbed in, then carries out the particulate load type that reduction obtains palladium modification galapectite Tubular composite material；(2) it is carbon source to recycle sucrose alcohol solution, and carbon-coating clad structure is obtained using solvent thermal process.By nitrogen atmosphere quilt Carbon-coating-palladium-galapectite multistage hydridization tubular composite material is obtained after burning.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109317138A (en) * | 2018-09-17 | 2019-02-12 | 合肥工业大学 | It is a kind of using galapectite/carbon as low-temperature SCR catalyst of carrier and preparation method thereof |
| CN110193361A (en) * | 2019-07-01 | 2019-09-03 | 中国工程物理研究院机械制造工艺研究所 | A kind of preparation method that Irreversible hydrogen-absorbing is composite porous and its product |
| CN111285349A (en) * | 2018-12-10 | 2020-06-16 | 河南工程学院 | Highly graphitized boron-doped carbon nanocapsule and preparation method thereof |
| CN112604654A (en) * | 2020-11-09 | 2021-04-06 | 中国科学院广州地球化学研究所 | Halloysite-based porous carbon composite material for adsorbing organic gas and preparation method thereof |
-
2017
- 2017-11-03 CN CN201711067411.2A patent/CN107597062A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| JIAOJIN ET AL.: ""Carbon hybridized halloysite nanotubes for high-performance hydrogen storage capacities"", 《SICENTIFIC REPORTS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109317138A (en) * | 2018-09-17 | 2019-02-12 | 合肥工业大学 | It is a kind of using galapectite/carbon as low-temperature SCR catalyst of carrier and preparation method thereof |
| CN111285349A (en) * | 2018-12-10 | 2020-06-16 | 河南工程学院 | Highly graphitized boron-doped carbon nanocapsule and preparation method thereof |
| CN111285349B (en) * | 2018-12-10 | 2022-05-27 | 河南工程学院 | Highly graphitized boron-doped carbon nanocapsule and preparation method thereof |
| CN110193361A (en) * | 2019-07-01 | 2019-09-03 | 中国工程物理研究院机械制造工艺研究所 | A kind of preparation method that Irreversible hydrogen-absorbing is composite porous and its product |
| CN112604654A (en) * | 2020-11-09 | 2021-04-06 | 中国科学院广州地球化学研究所 | Halloysite-based porous carbon composite material for adsorbing organic gas and preparation method thereof |
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Application publication date: 20180119 |