CN107601581A - A kind of double pore dimension structure nano crystalline substance cobalt acetate powders and preparation method thereof - Google Patents
A kind of double pore dimension structure nano crystalline substance cobalt acetate powders and preparation method thereof Download PDFInfo
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Abstract
A kind of double pore dimension structure nano crystalline substance cobalt acetate powders and preparation method thereof, belong to field of material technology, the crystallite dimension of powder is 50~100nm, and crystal grain accumulates Special composition structure, the meso-hole structure of macrovoid and 2~40nm with 150~500nm, form double pore dimension structures；Preparation method is：(1) cobalt nitrate aqueous solution is made in cobalt nitrate and water；(2) absolute ethyl alcohol, butyl titanate and complexing agent are stirred mixing, solution A is made；(3) add glacial acetic acid and B solution is made；(4) cobalt nitrate aqueous solution is instilled and cobalt titanate colloidal sol is formed in B solution；(5) stirring in water bath is to obtaining gel；(6) in 550~750 DEG C of roastings after drying.The product of the present invention has the advantages that specific surface area is big, and gas diffusion transports easy progress and high specific surface area effective rate of utilization；Method is simple to operate, and synthesis temperature is low, low without complex device, cost.
Description
Technical field
The invention belongs to porous material technical field, more particularly to a kind of double pore dimension structure nano crystalline substance cobalt acetate powders
And preparation method thereof.
Background technology
The cobalt titanate of perovskite structure is a kind of new inorganic functional material, in gas sensing, gasoline desulfurization catalyst, wet
Quick detection and photocatalytic degradation etc. suffer from very extensive application.Nanocrystalline barium titanate cobalt has larger ratio surface because of it
Product and skin effect, small-size effect and quantum size effect etc., there is more excellent table than common cobalt titanate during application
It is existing.Preparing the method for cobalt titanate nano material at present includes liquid phase method, vapor phase method and solid phase method, cobalt titanate prepared by these methods
Nano material is light concentration gas poor sensitivity, low, the operating temperature model of selectivity using existing subject matter in terms of air-sensitive
It is longer to enclose narrow and response recovery time.
Double yardstick pore structure nanocrystalline barium titanate cobalt powder bodies can both retain the high-specific surface area and active sites of original nano material
The advantages that point is more, while also there is the classification pore canal system being mutually communicated, there is provided more gas transport spaces and selectivity
Adsorb duct, its adsorbance to object gas can be effectively increased, so as to improve its sensitivity and it is selective while contract
The response of short corresponding gas sensor, recovery time；The preparation method on porous cobalt acetate powder material has template at present
With fused salt assisted self assembling method.Template is single as main body configuration, pore structure using template；Fused salt assisted self assembling method preparation technology
Complexity, production cost is high, is unfavorable for industrialization.On double yardstick pore structure nanocrystalline barium titanate cobalt powder body materials and its preparation side
Method, have not yet to see relevant report.
The content of the invention
The purpose of the present invention aims to provide a kind of double pore dimension structure nano crystalline substance cobalt acetate powders and preparation method thereof, leads to
Cross sol-gal process and be made double pore dimension structures, this pair of pore dimension structure can dramatically increase material effectively using area and
To the adsorbance of object gas, so as to improve corresponding gas sensing performance.
The crystallite dimension of double pore dimension structure nano crystalline substance cobalt acetate powders of the invention is 50~100nm, and crystal grain accumulates structure
Into space structure, the space structure has 150~500nm macrovoid, while macroporous hole wall is mesoporous with 2~40nm
Structure, form double pore dimension structures.
The specific surface area of above-mentioned double pore dimension structure nano crystalline substance cobalt acetate powders is 90.3~102.5m2/g。
Weight content >=98.1% of cobalt titanate in above-mentioned double pore dimension structure nano crystalline substance cobalt acetate powders.
The preparation method of double pore dimension structure nano crystalline substance cobalt acetate powders of the present invention is carried out according to the following steps：
(1) by cobalt nitrate and water according to mol ratio 1:The ratio mixing of (12~50), obtains cobalt nitrate aqueous solution；
(2) absolute ethyl alcohol, butyl titanate and complexing agent are stirred mixing, solution A, wherein butyl titanate is made
Mol ratio with complexing agent is 1:(0.7~3.5)；The mass ratio of absolute ethyl alcohol and butyl titanate is (9~21):1；
(3) under agitation, glacial acetic acid is instilled in solution A, to pH value 2.5~6, B solution is made；
(4) under agitation, cobalt nitrate aqueous solution is instilled in B solution, the addition of cobalt nitrate aqueous solution presses nitric acid
The mol ratio of cobalt and butyl titanate is 1:1, instillation continues stirring until to form cobalt titanate colloidal sol after terminating；
(5) cobalt titanate colloidal sol is stirred continuously until under water bath condition and obtains cobalt titanate gel, bath temperature scope 40
~70 DEG C；
(6) gained cobalt titanate gel is dried at least 2h under the conditions of 80~105 DEG C, is then calcined 1 at 550~750 DEG C
~4h, obtain double pore dimension structure nano crystalline substance cobalt acetate powders.
Above-mentioned complexing agent is diethanol amine or acetylacetone,2,4-pentanedione.
In above-mentioned step (4), the instillation speed of cobalt nitrate aqueous solution is 1~4mL/min.
In above-mentioned step (4), mixing speed is 500~1000rpm.
The present invention has the advantages that：(1) by sol-gal process be prepared with 2~40nm and 150~
The nanocrystalline barium titanate cobalt powder body material of the high gas sensitivity of two kinds of pore dimension structures of 500nm；(2) nanocrystalline barium titanate prepared
Cobalt powder body has three-D pore structure, and macroporous wall is formed by the accumulation of cobalt titanate nano-crystalline granule, particle packing fine pore
Interlaced with macrovoid, big with specific surface area, gas diffusion transports easily progress and specific surface area effective rate of utilization height etc.
Advantage；(3) when overcoming existing via sol-gel template method and preparing porous material, template synthesis difficulty, complex process, cost
The shortcomings of being mutually communicated property difference between too high and duct, and it is simple to operate, synthesis temperature is low, low without complex device, cost.
Brief description of the drawings
Fig. 1 is the XRD of double pore dimension structure nano crystalline substance cobalt acetate powders in embodiment 2；
Fig. 2 is the scanning electron microscope (SEM) photograph of double pore dimension structure nano crystalline substance cobalt acetate powders in embodiment 2；(a) is in figure
The pattern of big pore size distribution on 10000 × powder, (b) are the accumulation of 60000 × lower nano-crystalline granule into the mesoporous pattern of small yardstick；
Fig. 3 be double pore dimension structure nano crystalline substance cobalt acetate powders in embodiment 2 BJH absorption pore size distribution curve and
Absorption/desorption isothermal curve figure.
Embodiment
Cobalt nitrate hexahydrate, absolute ethyl alcohol, butyl titanate, diethanol amine, the acetylacetone,2,4-pentanedione used in the embodiment of the present invention
It is AR purchased in market with glacial acetic acid.
The water used in the embodiment of the present invention is deionized water.
Material phase analysis test uses Shimadzu XRD-7000 type X-ray diffractometers in the embodiment of the present invention.
Microscopic appearance detection uses Hitachi SU8010 field emission scanning electron microscopes in the embodiment of the present invention.
The equipment that the detection of central hole structure of the embodiment of the present invention uses is the specific surface areas of V-Sorb 4800 and Porosimetry.
Embodiment 1
Using 1.94g cobalt nitrate hexahydrates, by cobalt nitrate and water according to mol ratio 1:20 ratio mixing, obtains cobalt nitrate water
Solution；
Absolute ethyl alcohol, butyl titanate and complexing agent diethanol amine are stirred mixing, solution A, the fourth of metatitanic acid four is made
The mol ratio of ester and complexing agent is 1:0.7；The mass ratio of absolute ethyl alcohol and butyl titanate is 18:1；
Under agitation, glacial acetic acid is instilled in solution A, is 4.5 to pH value, B solution is made；
Under the conditions of low whipping speed 500rpm, cobalt nitrate aqueous solution is instilled in B solution, instillation speed is 1mL/min, nitre
The addition of the sour cobalt aqueous solution is 1 by the mol ratio of cobalt nitrate and butyl titanate:1, instillation continues stirring until to be formed after terminating
Cobalt titanate colloidal sol (according to Tyndall phenomenon)；
Container equipped with cobalt titanate colloidal sol is placed in water-bath, is stirred continuously until and obtains cobalt titanate gel, bath temperature
40℃；
Gained cobalt titanate gel is put into baking oven, 3h is dried under the conditions of 90 DEG C；Muffle furnace is then placed in, at 550 DEG C
4h is calcined, obtains double pore dimension structure nano crystalline substance cobalt acetate powders；
The crystallite dimension of double pore dimension structure nano crystalline substance cobalt acetate powders is 50~100nm, and crystal grain accumulates Special composition
Structure, the space structure has 150~500nm macrovoid, while macroporous hole wall has 2~40nm meso-hole structure,
Form double pore dimension structures, specific surface area 92.6m2/ g, cobalt titanate weight content 98.7%.
Embodiment 2
With embodiment 1, difference is method：
(1) mol ratio 1 of cobalt nitrate and water:12；
(2) mol ratio of butyl titanate and complexing agent is 1 in solution A:1.5；The matter of absolute ethyl alcohol and butyl titanate
It is 21 to measure ratio:1；
(3) it is 3.5 that glacial acetic acid, which instills solution A to pH value,；
(4) under the conditions of low whipping speed 600rpm, cobalt nitrate aqueous solution is instilled in B solution, instillation speed is 1.5mL/
min；
(5) 45 DEG C of bath temperature；
(6) 105 DEG C of drying temperature, time 2h；650 DEG C of sintering temperature, time 2h；
The specific surface area of double pore dimension structure nano crystalline substance cobalt acetate powders is 102.5m2/ g, cobalt titanate weight content
98.9%；
Thing phase composition XRD analysis be calcined as shown in figure 1, as seen from the figure, at 650 DEG C cobalt titanate that 2h obtains 23.9 °,
32.8 °, 35.39 °, 40.5 °, 49.0 °, 53.4 °, 56.8 °, 61.9 °, 63.8 ° and 71.3 ° have characteristic peak, correspond to metatitanic acid respectively
(012) of cobalt, (104), (110) (113), (024), (116), (018), (214), (300) and (119) crystal face, with standard card
Piece JCPDS：It is consistent in 15-0866；
Electron-microscope scanning result is as shown in Fig. 2 from Fig. 2 (a) and (b), and product has two kinds of pore dimension structures, greatly
Pore diameter is evenly distributed on powder body material in the range of 150~500nm；The large scale hole be using polymer phase with
Solvent split-phase and formed, " solvent phase " volatilizees in drying process, so as to form the more uniform large scale hole of distribution；It is another
Aspect, the hole wall after roasting around large scale hole are formed by the accumulation of nanocrystalline barium titanate cobalt crystal grain, 50~100nm of crystallite dimension,
Crystal grain accumulates the pore diameter to be formed between 2~40nm, forms the hole of second of yardstick；
BJH adsorbs pore size distribution curve and absorption/desorption isotherm as shown in figure 3, the specific surface area that BET is calculated is
102.5m2/g；As seen from the figure, in N2 adsorption test pore diameter range (2~150nm), containing the mesoporous of 2~40nm in product,
Most probable pore size is 2-10nm；Absorption/desorption isotherm hysteresis loop is from low pressure point P/P0=0.35 initially forms, to P/P0=
Adsorbance is significantly raised at 0.95, shows the nanocrystalline barium titanate cobalt powder body material of the invention prepared in addition to mesoporous, also containing certain
The macropore of quantity.
Embodiment 3
With embodiment 1, difference is method：
(1) mol ratio 1 of cobalt nitrate and water:50；
(2) mol ratio of butyl titanate and complexing agent is 1 in solution A:2；The quality of absolute ethyl alcohol and butyl titanate
Than being 15:1；
(3) it is 2.5 that glacial acetic acid, which instills solution A to pH value,；
(4) under the conditions of low whipping speed 700rpm, cobalt nitrate aqueous solution is instilled in B solution, instillation speed is 2mL/
min；
(5) 50 DEG C of bath temperature；
(6) 95 DEG C of drying temperature, time 4h；600 DEG C of sintering temperature, time 3.5h；
The specific surface area of double pore dimension structure nano crystalline substance cobalt acetate powders is 95.3m2/ g, cobalt titanate weight content
98.3%.
Embodiment 4
With embodiment 1, difference is method：
(1) mol ratio 1 of cobalt nitrate and water:30；
(2) complexing agent is acetylacetone,2,4-pentanedione, and the mol ratio of butyl titanate and complexing agent is 1 in solution A:2.5；Absolute ethyl alcohol
Mass ratio with butyl titanate is 17:1；
(3) it is 5.5 that glacial acetic acid, which instills solution A to pH value,；
(4) under the conditions of low whipping speed 800rpm, cobalt nitrate aqueous solution is instilled in B solution, instillation speed is 2.5mL/
min；
(5) 55 DEG C of bath temperature；
(6) 85 DEG C of drying temperature, time 4.5h；700 DEG C of sintering temperature, time 2.5h；
The specific surface area of double pore dimension structure nano crystalline substance cobalt acetate powders is 90.3m2/ g, cobalt titanate weight content
98.5%.
Embodiment 5
With embodiment 1, difference is method：
(1) mol ratio 1 of cobalt nitrate and water:40；
(2) complexing agent is acetylacetone,2,4-pentanedione, and the mol ratio of butyl titanate and complexing agent is 1 in solution A:3；Absolute ethyl alcohol with
The mass ratio of butyl titanate is 14:1；
(3) it is 6 that glacial acetic acid, which instills solution A to pH value,；
(4) under the conditions of low whipping speed 900rpm, cobalt nitrate aqueous solution is instilled in B solution, instillation speed is 3mL/
min；
(5) 60 DEG C of bath temperature；
(6) 80 DEG C of drying temperature, time 5h；730 DEG C of sintering temperature, time 2h；
The specific surface area of double pore dimension structure nano crystalline substance cobalt acetate powders is 97.4m2/ g, cobalt titanate weight content
98.2%.
Embodiment 6
With embodiment 1, difference is method：
(1) mol ratio 1 of cobalt nitrate and water:35；
(2) complexing agent is acetylacetone,2,4-pentanedione, and the mol ratio of butyl titanate and complexing agent is 1 in solution A:3.5；Absolute ethyl alcohol
Mass ratio with butyl titanate is 9:1；
(3) it is 6 that glacial acetic acid, which instills solution A to pH value,；
(4) under the conditions of low whipping speed 1000rpm, cobalt nitrate aqueous solution is instilled in B solution, instillation speed is 4mL/
min；
(5) 70 DEG C of bath temperature；
(6) 100 DEG C of drying temperature, time 2h；750 DEG C of sintering temperature, time 1h；
The specific surface area of double pore dimension structure nano crystalline substance cobalt acetate powders is 91.5m2/ g, cobalt titanate weight content
98.1%.
Claims (7)
1. a kind of double pore dimension structure nano crystalline substance cobalt acetate powders, it is characterised in that crystallite dimension is 50~100nm, crystal grain heap
Product Special composition structure, the space structure has 150~500nm macrovoid, while macroporous hole wall has 2~40nm's
Meso-hole structure, form double pore dimension structures.
2. a kind of double pore dimension structure nano crystalline substance cobalt acetate powders according to claim 1, it is characterised in that it compares table
Area is 90.3~102.5m2/g。
A kind of 3. double pore dimension structure nano crystalline substance cobalt acetate powders according to claim 1, it is characterised in that wherein titanium
Weight content >=98.1% of sour cobalt.
A kind of 4. preparation method of double pore dimension structure nano crystalline substance cobalt acetate powders described in claim 1, it is characterised in that
Carry out according to the following steps：
(1) by cobalt nitrate and water according to mol ratio 1:The ratio mixing of (12~50), obtains cobalt nitrate aqueous solution；
(2) absolute ethyl alcohol, butyl titanate and complexing agent are stirred mixing, solution A, wherein butyl titanate and network is made
The mol ratio of mixture is 1:(0.7~3.5)；The mass ratio of absolute ethyl alcohol and butyl titanate is (9~21):1；
(3) under agitation, glacial acetic acid is instilled in solution A, to pH value 2.5~6, B solution is made；
(4) under agitation, cobalt nitrate aqueous solution is instilled in B solution, the addition of cobalt nitrate aqueous solution by cobalt nitrate with
The mol ratio of butyl titanate is 1:1, instillation continues stirring until to form cobalt titanate colloidal sol after terminating；
(5) cobalt titanate colloidal sol is stirred continuously until under water bath condition and obtains cobalt titanate gel, bath temperature scope 40~70
℃；
(6) gained cobalt titanate gel is dried at least 2h under the conditions of 80~105 DEG C, is then calcined 1~4h at 550~750 DEG C,
Obtain double pore dimension structure nano crystalline substance cobalt acetate powders.
5. the preparation method of double pore dimension structure nano crystalline substance cobalt acetate powders according to claim 4, it is characterised in that
Described complexing agent is diethanol amine or acetylacetone,2,4-pentanedione.
6. the preparation method of double pore dimension structure nano crystalline substance cobalt acetate powders according to claim 4, it is characterised in that
In step (4), the instillation speed of cobalt nitrate aqueous solution is 1~4mL/min.
7. the preparation method of double pore dimension structure nano crystalline substance cobalt acetate powders according to claim 4, it is characterised in that
In step (4), mixing speed is 500~1000rpm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108666544A (en) * | 2018-04-18 | 2018-10-16 | 燕山大学 | One kind is derived with MOF prepares carbon coating CoTiO3The synthetic method of nano microcrystalline material |
| CN109607518A (en) * | 2018-12-10 | 2019-04-12 | 陕西科技大学 | A kind of preparation method of the highly selective sensitive thin film of pair of alcohol gas |
| CN110104678A (en) * | 2019-05-16 | 2019-08-09 | 沈阳工业大学 | To the cobalt titanate gas sensitive and preparation method thereof of low-concentration ethanol high sensitivity |
| CN115304986A (en) * | 2022-08-25 | 2022-11-08 | 安徽中科思沃生物科技有限公司 | Shell powder-based photocatalytic self-cleaning mildew-proof interior wall coating and preparation method thereof |
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| CN103730259A (en) * | 2013-12-27 | 2014-04-16 | 沈阳工业大学 | Nanocrystalline titanium dioxide film of two-specification pore structure and manufacturing method of nanocrystalline titanium dioxide film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108666544A (en) * | 2018-04-18 | 2018-10-16 | 燕山大学 | One kind is derived with MOF prepares carbon coating CoTiO3The synthetic method of nano microcrystalline material |
| CN108666544B (en) * | 2018-04-18 | 2020-11-06 | 燕山大学 | Preparation of carbon-coated CoTiO by MOF derivatization3Synthesis method of nano microcrystalline material |
| CN109607518A (en) * | 2018-12-10 | 2019-04-12 | 陕西科技大学 | A kind of preparation method of the highly selective sensitive thin film of pair of alcohol gas |
| CN110104678A (en) * | 2019-05-16 | 2019-08-09 | 沈阳工业大学 | To the cobalt titanate gas sensitive and preparation method thereof of low-concentration ethanol high sensitivity |
| CN110104678B (en) * | 2019-05-16 | 2021-10-08 | 沈阳工业大学 | Cobalt titanate gas-sensitive material with high sensitivity to low-concentration ethanol and preparation method thereof |
| CN115304986A (en) * | 2022-08-25 | 2022-11-08 | 安徽中科思沃生物科技有限公司 | Shell powder-based photocatalytic self-cleaning mildew-proof interior wall coating and preparation method thereof |
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