CN102649590A - Method for preparing mesoporous material NiAl2O4 without specific surface active agent - Google Patents

Method for preparing mesoporous material NiAl2O4 without specific surface active agent Download PDF

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CN102649590A
CN102649590A CN2012101350179A CN201210135017A CN102649590A CN 102649590 A CN102649590 A CN 102649590A CN 2012101350179 A CN2012101350179 A CN 2012101350179A CN 201210135017 A CN201210135017 A CN 201210135017A CN 102649590 A CN102649590 A CN 102649590A
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aluminum
nickel
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汪学广
尚兴付
丁伟中
陆东亮
黄震
鲁雄刚
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a preparation method for a worm-like mesoporous material NiAl2O4 and belongs to the technical field of inorganic nano materials. The preparation method comprises the following steps: dissolving nickel salt and aluminum salt into a certain amount of deionized water to prepare stock solution; adding ammonium carbonate solution at the concentration of 1 mol/L into the stock solution dropwise by controlling the quantity of the ammonium carbonate, which is 1.5 times of the sum of the aluminum ions and the nickel ions; transferring colloid formed after titration into a drying oven and drying at the temperature of 110 DEG C for 12 hours; roasting at a temperature ranging from 500 and 800 DEG C for 20 hours at the heating speed of 10 DEG C per minute; and grinding to obtain the worm-like mesoporous material NiAl2O4 with the surface area of 80 to 250 m<2>/g and pore diameter distribution of 4 to 15 nm. The preparation method is simple in process, low in cost, high in purity, high in specific surface area, easy to control and easy to industrialize. The product can be applied in the fields of high-performance composite materials such as catalytic materials, adsorption materials, luminescent materials, magnetic materials, separating materials, high-temperature-resistant materials and the like.

Description

Incomparable tensio-active agent prepares mesoporous NiAl 2O 4The method of material
Technical field
The present invention relates to the worm meso-porous NiAl of a kind of regular pore size distribution 2O 4Preparation methods belongs to technical field of inorganic nanometer material.
Background technology
The definition of pure applied chemistry association (IUPAC) in according to the world, porous material can be divided three classes according to the size of their bore dias: the aperture is poromerics (microporousmaterials) less than the material of 2 nm; The aperture is mesoporous material (mesoporous materials) at the material of 2-50 nm; The aperture is large pore material (macroporous materials) greater than the material of 50 nm.Because mesoporous material has bigger internal surface and the hole that allows molecule to get into, thus bigger molecule or group can be handled, so new world has been opened up in the catalytic cracking that is used for heavy oil, residual oil of said material.Because the influence of quantum size effect and interface coupling effect, the order mesoporous heterogeneous material compound of acquisition will have unusual physics, chemical property.In bigger mesopore molecular sieve duct, carry out the bioorganic chemistry simulation and also become possibility; In addition, at selective oxidation, perfect combustion, NO xFields such as degraded, hydrodesulfurization process, photocatalysis to degrade organic matter and solid acid catalysis, fractionation by adsorption have also caused people's extensive concern.Said material will have huge potential application foreground at numerous areas such as chemistry, photoelectronics, electromagnetism, materialogy, environmentalisms.
About NiAl 2O 4Report is also few, Journal of Inorganic Materials 8 (4), among 1993 499-502 through the Al that is 1:1 1350 ℃ of roasting mol ratios 2O 3Get NiAl with the NiO compounding substances 2O 4, and the NiAl that utilized XRD and XPS analysis 2O 4Microtexture.Synthesized specific surface less than 10 m with the burning urea method among the int ernational journal of hydrogen energy 35 (2010) 11725-11732 2The NiAl of/g 2O 4And studied the catalytic performance of methane reforming hydrogen manufacturing.At present about mesoporous NiAl 2O 4The report of material is also few, Chem. Mater. 2000, 12,Reported among the 331-335 and used NH 4OH is as precipitation agent, prepares specific surface up to 177 m 500-700 ℃ of roasting 2The mesoporous NiAl of/g 2O 4, but pore size distribution is very wide, very irregular, and the application of material is had very big restriction.Mesoporous material synthetic generally will be used organism and done template, and operational condition is generally relatively harsher.Thereby develop a kind of raw material and be easy to get, with low cost, simple to operate, convenient processing, reaction conditions is gentle, is easy to industrialized mesoporous NiAl 2O 4Material synthesis method is significant.
Summary of the invention
The purpose of this invention is to provide a kind of vermiform mesoporous NiAl that narrow pore size distribution is arranged 2O 4Preparation methods.
A kind of mesoporous NiAl that narrow pore size distribution is arranged of the present invention 2O 4Preparation methods is characterized in that having following preparation process and step:
A. a certain amount of aluminium salt and nickel salt are dissolved in the deionized water aluminum ion solution of preparation 1～4 mol/L and the nickel ion solution of 0.5～2 mol/L; Aluminum ions concentration is 2 times of nickel ion concentration;
B. at 30～90 ℃, dropwise splash into the sal volatile that concentration is 1～4 mol/L while stirring, the volume of control volatile salt, making the volatile salt amount of substance is 1.5 times of nickel aluminum ion amount sum; Obtain gel through reaction;
C. with the gel that forms after titration constant temperature ageing 24 hours under temperature of reaction, change baking oven subsequently over to, 110 ℃ dry 12 hours down;
D. with the temperature rise rate of above-mentioned dried gel,, finally make mesoporous NiAl 500～800 ℃ of calcinings 20 hours with 10 ℃/min 2O 4Material.
Described aluminium salt is any in aluminum nitrate, aluminum chloride, the Tai-Ace S 150; With the aluminum nitrate is preferential; Described nickel salt is any in nickelous nitrate, nickelous chloride, the single nickel salt, is preferential with the nickelous nitrate.
Present method is prepared white lake and nickel hydroxide colloidal sol through the method for aluminum soluble salt and nickel salt hydrolysis.Deviate from free water after the drying, form white lake and nickel hydroxide xerogel.Calcining and decomposing an ammonium nitrate with lose after the intramolecularly water, formed mesoporous NiAl 2O 4Material.Reaction equation is following:
2Al(NO 3) 3+3(NH 4) 2CO 3 + 3H 2O=2Al(OH) 3 +6NH 4NO 3 + 3CO 2↑
Ni(NO 3) 2+ (NH 4) 2CO 3 + H 2O=Ni(OH) 2+2NH 4NO 3+CO 2 ↑
NH 4NO 3=HNO 3+ NH 3↑ or NH 4NO 3=N 2O ↑+2H 2O
Ni(OH) 2 +2Al(OH) 3
Figure 2012101350179100002DEST_PATH_IMAGE002
NiAl 2O 4 + 4H 2O
Characteristics of the present invention and advantage are described below:
(1) the present invention adopts the saline hydrolysis sol-gel method, and product has a kind of worm meso-porous NiAl with narrow pore size distribution of favorable reproducibility 2O 4, for good basis has been established in the research and development of functional materials.
(2) the selected system of the inventive method is a raw material with the volatile salt that is easy to get in the industry, synthesizes a kind of worm meso-porous NiAl 2O 4Thereby, greatly reduce production cost, improved the production efficiency of nano material.
(3) the inventive method only needs two kinds of RMs, can synthesize the worm meso-porous NiAl of narrow pore size distribution through easy reaction 2O 4, and used solvent is a water in the reaction, can recycling, therefore have easy and simple to handle, processing unit is simple, free of contamination advantage, is beneficial to suitability for industrialized production.
Description of drawings
Fig. 1 is the structure iron that the product X ray powder diffraction (XRD) of the embodiment of the invention one obtains.
Fig. 2 is product high power transmission electron microscope (TEM) photo of the embodiment of the invention one.
Fig. 3 is the product nitrogen adsorption desorption and the graph of pore diameter distribution of the embodiment of the invention one.
Fig. 4 is the product nitrogen adsorption desorption and the graph of pore diameter distribution of the embodiment of the invention two.
Fig. 5 is the product nitrogen adsorption desorption and the graph of pore diameter distribution of the embodiment of the invention three.
Fig. 6 is the product nitrogen adsorption desorption and the graph of pore diameter distribution of the embodiment of the invention four.
Fig. 7 is the product nitrogen adsorption desorption and the graph of pore diameter distribution of the embodiment of the invention five.
Embodiment
After specific embodiment of the present invention being described at present.
Embodiment 1
Preparation process in the present embodiment is following:
(a) stir down, with 0.1mol aluminum nitrate 0.05mol nickelous nitrate be dissolved in the 50 mL deionized waters, form the solution that mixes;
(b) 70 ℃ of constant temperature stir down, and with 225mL, the sal volatile of 1 mol/L dropwise splashes in the above-mentioned solution, forms colloidal sol;
(c), transfer in the baking oven 110 ℃ of oven dry 12 hours with the ageing 24 hours under 70 ℃ of constant temperature of above-mentioned uniform sol;
(d) with the sample of step c gained with the temperature rise rate of 10 ℃/min 800 ℃ of roastings 20 hours, grind and promptly obtain mesoporous NiAl 2O 4Material.
With this instance products therefrom, carry out the XRD figure spectrum and measure, and N 2Adsorption/desorption is measured the BET specific surface area and the pore size distribution of material and is measured.Visible from Fig. 1, XRD result shows that product is NiAl 2O 4(consistent) with 10-0339 JCPDS card.Fig. 2 is high power transmission electron microscope (TEM) figure of sample.Can clearly find out the vermiform pore passage structure by figure.Fig. 3 is routine 1 sample N 2Suction-desorption isothermal curve and pore size distribution curve (built-in figure).Pore distribution curve is with pore volume aperture one subdifferential to be mapped, and ordinate zou should be dV/dr, the cm of unit -3.g -1.nm -1, represent the velocity of variation of pore volume with the aperture, X-coordinate is the aperture, unit is nm.The adsorption isotherm line chart, X-coordinate P/P0 represents relative pressure, is non-dimensional numerical value, and P is the psia of TP nitrogen, and Po is the saturation vapour pressure of nitrogen under the probe temperature, and the adsorption equilibrium pressure that relative pressure is nitrogen is with respect to its saturation vapour pressure size; Ordinate zou is an adsorptive capacity, and being has dimension numerical value, the amount of the adsorbate that the unit vol sorbent material adsorbs under equilibrium temperature and pressure when referring to balance.(amount of sorbent material is measured in mass, and the amount of adsorbate is then with volume, quality or amount of substance metering, but mostly with adsorbate gas volume metering under the normal conditions (STP), therefore common unit dimension is cm 3/ g or mL/g are with STP to be indicated as being the normal conditions thereafter.) the products therefrom specific surface is 105.27 m 2/ g, mean pore size is 7.23 nm, pore volume is 0.19cm 3/ g, the narrow rule of pore size distribution.
Embodiment 2
Concrete steps are following:
(a) stir down, 0.1mol aluminum nitrate 0.05mol nickelous nitrate is dissolved in the 20 mL deionized waters, form the solution that mixes;
(b) 50 ℃ of constant temperature stir down, and with 225mL, the sal volatile of 1mol/L dropwise splashes in the above-mentioned solution, forms colloidal sol;
(c) above-mentioned uniform sol is changeed under 50 ℃ of constant temperature ageing 24 hours, move on in the baking oven 110 ℃ of oven dry 12 hours;
(d) with the sample of step c gained with the temperature rise rate of 10 ℃/min 500 ℃ of roastings 20 hours, grind and promptly obtain mesoporous NiAl 2O 4Material.
The pore size distribution curve of present embodiment products therefrom and N 2Suction-desorption isothermal curve is as shown in Figure 4.The products therefrom specific surface is 234.01 m 2/ g, mean pore size is 4.6 nm, pore volume 0.27 cm 3/ g, the narrow rule of pore size distribution.
Embodiment 3
Concrete steps are following:
(a) stir down, with 0.1mol aluminum nitrate 0.05mol nickelous nitrate be dissolved in the 50 mL deionized waters, form the solution that mixes;
(b) 30 ℃ of constant temperature stir down, and with 112.5mL, the sal volatile of 2 mol/L dropwise splashes in the above-mentioned solution, forms colloidal sol;
(c), transfer in the baking oven 110 ℃ of oven dry 12 hours with the ageing 24 hours under 30 ℃ of constant temperature of above-mentioned uniform sol;
(d) with the sample of step c gained with the temperature rise rate of 10 ℃/min 800 ℃ of roastings 20 hours, promptly obtain mesoporous NiAl 2O 4Material.
Fig. 5 is present embodiment gained sample pore size distribution curve and N 2Suction-desorption isothermal curve.The products therefrom specific surface is 87.15m 2/ g, mean pore size is 13.5 nm, pore volume is 0.30 cm 3/ g, the narrow rule of pore size distribution.
Embodiment 4
Concrete steps are following:
(a) stir down, with 0.1mol aluminum nitrate 0.05mol nickelous nitrate be dissolved in the 100 mL deionized waters, form the solution that mixes;
(b) 50 ℃ of constant temperature stir down, and with 225 mL, the sal volatile of 1mol/L dropwise splashes in the above-mentioned solution, forms colloidal sol;
(c), transfer in the baking oven 110 ℃ of oven dry 12 hours with the ageing 24 hours under 50 ℃ of constant temperature of above-mentioned uniform sol;
(d) with the sample of step c gained with the temperature rise rate of 10 ℃/min 500 ℃ of roastings 20 hours, promptly obtain mesoporous NiAl 2O 4Material.
Fig. 6 is present embodiment products therefrom pore size distribution curve and N 2Suction-desorption isothermal curve.The products therefrom specific surface is 234.92 m 2/ g, mean pore size is 4.70 nm, pore volume is 0.28cm 3/ g, the narrow rule of pore size distribution.
Embodiment 5
Concrete steps are following:
(a) stir down, with 0.1mol aluminum nitrate 0.05mol nickelous nitrate be dissolved in the 100 mL deionized waters, form the solution that mixes;
(b) 70 ℃ of constant temperature stir down, and with 56.25 mL, the sal volatile of 4mol/L dropwise splashes in the above-mentioned solution, forms colloidal sol;
(c), transfer in the baking oven 110 ℃ of oven dry 12 hours with the ageing 24 hours under 70 ℃ of constant temperature of above-mentioned uniform sol;
(d) with the sample of step c gained with the temperature rise rate of 10 ℃/min 600 ℃ of roastings 20 hours, promptly obtain mesoporous NiAl 2O 4Material.
Fig. 7 is present embodiment products therefrom N 2Suction-desorption isothermal curve and pore size distribution curve.The products therefrom specific surface is 219.46 m 2/ g, mean pore size is 4.7 nm, pore volume is 0.26 cm 3/ g, the narrow rule of pore size distribution.
The project that detects and the instrument of use thereof
The gained sample is carried out N 2Adsorption/desorption is measured, and BET specific surface area and the pore size distribution of measuring material; Used instrument is full-automatic specific surface area and a pore size distribution determinator fast of the ASAP2020 of U.S. Micromeritics company.Sample needs to slough other material of moisture and physical adsorption at 250 ℃ of degassing 5h.Sample carries out the XRD figure spectrum at Rigaku D/max-2550 X-ray diffractometer to be measured, to confirm prepared title product of experiment and purity.Condition determination is CuK α (λ=1.5406), 40KV, 100mA, Scan speed:0.02 ゜/s.The used instrument of transmission electron microscope photo is JEM-2010F microscope acceleration voltage 200 kV.

Claims (2)

1. worm meso-porous NiAl of narrow pore size distribution 2O 4Preparation methods is characterized in that having following preparation process and step:
A. a certain amount of aluminium salt and nickel salt are dissolved in the deionized water aluminum ion solution of preparation 1～4 mol/L and the nickel ion solution of 0.5～2.0mol/L; Aluminum ions concentration is 2 times of nickel ion concentration;
B. at 30～70 ℃, dropwise splash into the sal volatile that concentration is 1～4 mol/L while stirring, the volume of control volatile salt, making the volatile salt amount of substance is 1.5 times of nickel aluminum ion amount sum; Obtain gel through reaction;
C. with the gel that forms after titration constant temperature ageing 24 hours under temperature of reaction, change baking oven subsequently over to, 100-110 ℃ dry 12 hours down;
D. with the temperature rise rate of above-mentioned dried gel, burnt 20 hours, finally make mesoporous NiAl 500～800 ℃ of roastings with 10 ℃/min 2O 4Material.
2. a kind of worm meso-porous NiAl that narrow pore size distribution is arranged as claimed in claim 1 2O 4Preparation methods is characterized in that described aluminium salt is any in aluminum nitrate, aluminum chloride, the Tai-Ace S 150; With the aluminum nitrate is preferential; Described nickel salt is any in nickelous nitrate, nickelous chloride, the single nickel salt, is preferential with the nickelous nitrate.
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CN102910688A (en) * 2012-11-21 2013-02-06 绥化学院 Method for preparing high specific surface area nano nickel aluminate electrode material
CN104028271A (en) * 2014-01-02 2014-09-10 上海大学 Preparation method of mesoporous nickel-magnesium-aluminum oxide with high specific surface area
CN104128187A (en) * 2014-07-02 2014-11-05 上海大学 Ni/La2O3 catalyst used for reforming LPG low water carbon ratio water vapor and preparation method thereof
CN104549289A (en) * 2014-11-26 2015-04-29 上海大学 Mesoporous alumina nickel-based catalyst with high activity and high stability for CO2 reforming CH4 reaction and preparation method of mesoporous alumina nickel-based catalyst
CN105771994A (en) * 2016-03-26 2016-07-20 上海大学 Nano-mesoporous alumina-loaded nickel aluminate catalyst for reforming CH4 by CO2 and preparation method of nano-mesoporous alumina-loaded nickel aluminate catalyst
CN107460019A (en) * 2017-07-14 2017-12-12 华南农业大学 A kind of preparation method of nano-nickel oxide/nickel aluminate carrier of oxygen
CN111180199A (en) * 2019-12-27 2020-05-19 东佳电子（郴州）有限公司 Capacitor with cooling and heat dissipation functions
CN112844296A (en) * 2021-01-14 2021-05-28 辽宁大学 Preparation method of amino modified aluminate adsorbing material and application of amino modified aluminate adsorbing material in removal of various pollutants

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102910688A (en) * 2012-11-21 2013-02-06 绥化学院 Method for preparing high specific surface area nano nickel aluminate electrode material
CN102910688B (en) * 2012-11-21 2014-05-07 绥化学院 Method for preparing high specific surface area nano nickel aluminate electrode material
CN104028271A (en) * 2014-01-02 2014-09-10 上海大学 Preparation method of mesoporous nickel-magnesium-aluminum oxide with high specific surface area
CN104128187A (en) * 2014-07-02 2014-11-05 上海大学 Ni/La2O3 catalyst used for reforming LPG low water carbon ratio water vapor and preparation method thereof
CN104549289A (en) * 2014-11-26 2015-04-29 上海大学 Mesoporous alumina nickel-based catalyst with high activity and high stability for CO2 reforming CH4 reaction and preparation method of mesoporous alumina nickel-based catalyst
CN105771994A (en) * 2016-03-26 2016-07-20 上海大学 Nano-mesoporous alumina-loaded nickel aluminate catalyst for reforming CH4 by CO2 and preparation method of nano-mesoporous alumina-loaded nickel aluminate catalyst
CN107460019A (en) * 2017-07-14 2017-12-12 华南农业大学 A kind of preparation method of nano-nickel oxide/nickel aluminate carrier of oxygen
CN107460019B (en) * 2017-07-14 2019-06-28 华南农业大学 A kind of preparation method of nano-nickel oxide/nickel aluminate carrier of oxygen
CN111180199A (en) * 2019-12-27 2020-05-19 东佳电子（郴州）有限公司 Capacitor with cooling and heat dissipation functions
CN111180199B (en) * 2019-12-27 2021-09-10 东佳电子（郴州）有限公司 Capacitor with cooling and heat dissipation functions
CN112844296A (en) * 2021-01-14 2021-05-28 辽宁大学 Preparation method of amino modified aluminate adsorbing material and application of amino modified aluminate adsorbing material in removal of various pollutants
CN112844296B (en) * 2021-01-14 2024-03-22 辽宁大学 Preparation method of amino modified aluminate adsorption material and application of amino modified aluminate adsorption material in removal of various pollutants

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