CN105056851A - Preparation method of rare earth lanthanum-doped alumina nano-material - Google Patents
Preparation method of rare earth lanthanum-doped alumina nano-material Download PDFInfo
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- CN105056851A CN105056851A CN201510501280.9A CN201510501280A CN105056851A CN 105056851 A CN105056851 A CN 105056851A CN 201510501280 A CN201510501280 A CN 201510501280A CN 105056851 A CN105056851 A CN 105056851A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 204
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 229910052761 rare earth metal Inorganic materials 0.000 title abstract description 6
- 150000002910 rare earth metals Chemical class 0.000 title abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 47
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims abstract description 28
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 26
- 239000000725 suspension Substances 0.000 claims abstract description 26
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 25
- 239000011734 sodium Substances 0.000 claims abstract description 25
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 22
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- -1 lanthanum ions Chemical class 0.000 claims abstract description 13
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 46
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 42
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 21
- 238000002425 crystallisation Methods 0.000 claims description 20
- 230000008025 crystallization Effects 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 14
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 claims description 9
- PIMIEVIUUFJZGZ-UHFFFAOYSA-N [Cl].[La] Chemical compound [Cl].[La] PIMIEVIUUFJZGZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 6
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 239000013049 sediment Substances 0.000 abstract 2
- 239000006227 byproduct Substances 0.000 abstract 1
- 230000009977 dual effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 60
- 239000002253 acid Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical class CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method of a rare earth lanthanum-doped alumina nano-material. The preparation method comprises the following steps: 1, preparing an aluminium chloride solution; 2, preparing a lanthanum chloride solution according to the molar ratio (1:1)-(1:5) of lanthanum ions to aluminium ions; 3, respectively using sodium hydroxide and aluminium hydroxide to prepare a sodium metaaluminate solution according to the molar ratio (3:1)-(9:1) of sodium to aluminium; 4, adopting the dual dripping method to simultaneously drip the lanthanum chloride solution and the sodium metaaluminate solution into the aluminium chloride solution, and when the lanthanum chloride solution is completely dripped, using the sodium metaaluminate solution to adjust the pH value to be 1.0-8.4 to obtain a white suspension; 5, placing the white suspension at 60-180 DEG C to obtain a white sediment; 6, filtering, washing and drying the white sediment; 7, calcining to obtain the rare earth lanthanum-doped alumina nano-material. The rare earth lanthanum-doped alumina nano-material with relatively high thermal stability is prepared by the adoption of pollution-free and no-by-product hydrothermal method without adding a surfactant.
Description
Technical field
The present invention relates to the preparation method of rare-earth-doped glass nano material.More particularly, the present invention relates to a kind of preparation method of aluminium oxide nano material of rear earth lanthanum doping.
Background technology
The peculiar property that nano particle has makes it in catalyst, functional material, composite, optical material and ceramic material etc., have wide reality and potential application prospect.Such as, nano particle has high specific area and high surface-active, and using it for catalysis material has significant catalytic efficiency.
As everyone knows, can there is a series of phase transformation in aluminium oxide in calcination process, finally obtains the aluminium oxide (α-Al of stable phase
2o
3), wherein the crystal formation of intermediate state is transition state of alumina, and γ-Al in transition state of alumina
2o
3with δ-Al
2o
3because specific area is large, crystalline phase temperature range is wide, surface possesses again the characteristics such as acidity and is called as activated alumina, be widely used in catalyst carrier.But for the high temperature such as purifying vehicle exhaust, catalytic combustion reaction system, in practical operation, the temperature of beds is usually higher than 1000 degree, the sintering of alumina surface and α phase transformation can cause surface area reduce sharply and cause catalysqt deactivation, therefore at the activated alumina that catalytic field needs heat endurance high, the heat endurance improving aluminium oxide has important practical significance.
Research finds, add the heat endurance that impurity element can improve activated alumina, rare-earth oxide, alkaline earth oxide etc. is generally as the additive improving thermal stability of alumina, and Be very effective, at present when improving the heat endurance of aluminium oxide, usually adopt the mode of dipping (adding additive), namely to the modifying surface of aluminium oxide, increased the stability of aluminium oxide by modification, research is lacked to other addition manners.
In view of more than, under the invention provides a kind of condition not adding surfactant, adopt hydro-thermal reaction legal system for the aluminium oxide nano material of rear earth lanthanum doping.
Summary of the invention
The present invention is directed to the problems referred to above, provide a kind of preparation method of aluminium oxide nano material of rear earth lanthanum doping.
The aluminium oxide nano material that an object of the present invention is the rear earth lanthanum doping prepared by hydro-thermal method, compared with aluminium oxide nano material, has higher heat endurance.
For this reason, the invention provides a kind of preparation method of aluminium oxide nano material of rear earth lanthanum doping, comprise the following steps:
1, a preparation method for the aluminium oxide nano material of rear earth lanthanum doping, is characterized in that, comprise the following steps:
Step one, compound concentration are the liquor alumini chloridi of 0.8 ~ 0.9mol/L;
Step 2, be 1:1 ~ 1:5 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with lanthanum chloride solution;
Step 3, be 3:1 ~ 9:1 according to the mol ratio of sodium/aluminium, prepare sodium aluminate solution with NaOH and aluminium hydroxide respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described lanthanum chloride solution and described sodium aluminate solution are added drop-wise in described liquor alumini chloridi simultaneously, be added drop-wise in described liquor alumini chloridi completely to described lanthanum chloride solution, stop dripping when then pH value being adjusted to 1.0 ~ 8.4 with described sodium aluminate solution, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 60 ~ 180 DEG C temperature under the crystallization scheduled time, obtain white depositions;
Step 6, the white depositions obtained is completed to step 5 crystallization carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining the aluminium oxide nano material of rear earth lanthanum doping;
Step 7, the Muffle furnace presoma of the aluminium oxide nano material of described rear earth lanthanum doping being placed in 400 ~ 1200 DEG C are calcined, and obtain the aluminium oxide nano material of rear earth lanthanum doping.
The aluminium oxide nano material of rear earth lanthanum doping is prepared by hydrothermal synthesis method, from rare earth oxide in the past to alumina surface-modified different, the lattice that lanthanum ion can enter aluminium oxide also passes through the aluminum ions diffusion of prevention and stablizes the structure of aluminium oxide, contact between restriction particle, thus suppress sintering, make alumina support still can have certain specific area after high temperature ageing;
Adopt the two methods combined with certain mixing speed during preparation white suspension, even and stable dropping can be realized, make reaction more complete.When just having started to react, solution is rarer, therefore can select relatively slow mixing speed, and along with the carrying out dripped, the viscosity of solution increases gradually, suitably can improve mixing speed, the Uniform Doped therefore by regulating mixing speed to realize rare earth ion;
PH value when lanthanum chloride is precipitated as lanthanum hydroxide is 8.4, so doping quality can be had a strong impact on if there is lanthanum hydroxide precipitation, therefore the strict pH value controlling suspension in course of reaction is needed, the aluminium chloride of 0.8 ~ 0.9mol/L is acid solution, sodium metaaluminate is alkaline solution, the starting stage dripped, only less sodium metaaluminate is there is in white suspension, therefore suspension is in acid, and lanthanum chloride can not generate precipitation in an acidic solution, therefore to ensure that the pH value of white suspension in dropping process and after dripping can not more than 8.4;
Because crystallization temperature and calcining heat all can affect the specific area of nano aluminium oxide, therefore the aluminium oxide nano material selecting lower crystallization temperature and calcining heat to prepare the larger rear earth lanthanum doping of specific area can be used as adsorbent, and the aluminium oxide nano material selecting higher crystallization temperature and calcining heat to prepare the higher rear earth lanthanum doping of heat endurance can be used as catalyst carrier.
Preferably, wherein, in described step 3, the concrete preparation method of sodium aluminate solution is:
Be 3:1 ~ 9:1 according to the mol ratio of sodium/aluminium, solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in the temperature of 70 ~ 120 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 150 ~ 180 DEG C, leave standstill 2h, obtain described sodium aluminate solution.
The method of selection dynamic and static state, realizes sodium metaaluminate and aluminium hydroxide better reacts, and is more conducive to the sodium aluminate solution preparing different sodium/al mole ratio simultaneously, improves the practicality of sodium aluminate solution.
Preferably, wherein, the pH value in described step 4 is 6.0 ~ 7.0.
Preferably, wherein, the temperature in described step 5 is 80 ~ 90 DEG C.
Preferably, wherein, in described step 2, the volume of lanthanum chloride solution and the volume ratio of described liquor alumini chloridi are 1:15 ~ 1:20.
Preferably, wherein, the scheduled time in described step 5 is 2 ~ 18h.
Preferably, wherein, the described scheduled time is 4h.
Preferably, wherein, the inner bag of described autoclave is put into autoclave in the temperature of 90 DEG C, under the rotating speed of 30 ~ 50r/min, place 2h.
Preferably, wherein, described dwell temperature is 170 DEG C.
The present invention at least comprises following beneficial effect:
1, the present invention prepares the aluminium oxide nano material of rear earth lanthanum doping by hydrothermal synthesis method, from rare earth oxide in the past to alumina surface-modified different, by preparation method of the present invention, the lattice that lanthanum ion can enter aluminium oxide also passes through the aluminum ions diffusion of prevention and stablizes the structure of aluminium oxide, contact between restriction particle, thus suppress sintering, make alumina support still can have certain specific area after high temperature ageing.
2, the method that during preparation white suspension, employing two and certain mixing speed combine, can realize even and stable dropping, make reaction more complete.When just having started to react, solution is rarer, therefore can select relatively slow mixing speed, and along with the carrying out dripped, the viscosity of solution increases gradually, suitably can improve mixing speed, the Uniform Doped therefore by regulating mixing speed to realize rare earth ion.
3, pH value when lanthanum chloride is precipitated as lanthanum hydroxide in the present invention is 8.4, so doping quality can be had a strong impact on if there is lanthanum hydroxide precipitation, therefore the strict pH value controlling suspension in course of reaction is needed, the aluminium chloride of 0.8 ~ 0.9mol/L is acid solution, sodium metaaluminate is alkaline solution, the starting stage dripped, only less sodium metaaluminate is there is in white suspension, therefore suspension is in acid, and lanthanum chloride can not generate precipitation in an acidic solution, therefore to ensure that the pH value of white suspension in dropping process and after dripping can not more than 8.4.
4, because crystallization temperature and calcining heat all can affect the specific area of nano aluminium oxide, therefore the aluminium oxide nano material selecting lower crystallization temperature and calcining heat to prepare the larger rear earth lanthanum doping of specific area can be used as adsorbent, and the aluminium oxide nano material selecting higher crystallization temperature and calcining heat to prepare the higher rear earth lanthanum doping of heat endurance can be used as catalyst carrier.
5, the present invention is with aluminium hydroxide and NaOH for raw material, selects the method for dynamic and static state, can prepare the sodium aluminate solution of different sodium/aluminum ratio, improve the practicality of sodium aluminate solution.
6, the present invention does not add the hydro-thermal method of surfactant by pollution-free, no coupling product, and the aluminium oxide nano material of the rear earth lanthanum doping prepared has high thermal stability.
Part is embodied by explanation below by other advantage of the present invention, target and feature, part also will by research and practice of the present invention by those skilled in the art is understood.
Accompanying drawing explanation
Fig. 1 is XRD schematic diagram in one embodiment of the present of invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail, can implement according to this with reference to description word to make those skilled in the art.
< embodiment 1>
Step one, preparation 100mL concentration are the liquor alumini chloridi of 0.8mol/L;
Step 2, be 1:1 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with 5mL lanthanum chloride solution;
Step 3, prepare with NaOH and aluminium hydroxide the sodium aluminate solution that sodium/aluminum ratio is 3:1 respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described lanthanum chloride solution and described sodium aluminate solution are added drop-wise in described liquor alumini chloridi simultaneously, be added drop-wise in described sodium aluminate solution completely to described lanthanum chloride solution, stop dripping when then pH value being adjusted to 1.0 with described sodium aluminate solution, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 80 DEG C temperature under crystallization 18h, obtain white depositions;
Step 6, step 5 crystallization is completed the white depositions obtained carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining the aluminium oxide nano material of rear earth lanthanum doping.
Step 7, the Muffle furnace presoma of the aluminium oxide nano material of described rear earth lanthanum doping being placed in 400 DEG C are calcined, and obtain the aluminium oxide nano material of rear earth lanthanum doping.
Wherein, in described step 3, the concrete preparation method of sodium aluminate solution is:
Solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in 70 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 180 DEG C of standing 2h, the molar ratio obtaining sodium/aluminium is the sodium aluminate solution of 3:1.
< embodiment 2>
Step one, preparation 100mL concentration are the liquor alumini chloridi of 0.8mol/L;
Step 2, be 1:5 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with 5mL lanthanum chloride solution;
Step 3, prepare with NaOH and aluminium hydroxide the sodium aluminate solution that sodium/aluminum ratio is 5:1 respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described lanthanum chloride solution and described sodium aluminate solution are added drop-wise in described liquor alumini chloridi simultaneously, be added drop-wise in described sodium aluminate solution completely to described lanthanum chloride solution, stop dripping when then pH value being adjusted to 6.0 with described sodium aluminate solution, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 120 DEG C temperature under crystallization 2h, obtain white depositions;
Step 6, step 5 crystallization is completed the white depositions obtained carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining the aluminium oxide nano material of rear earth lanthanum doping;
Step 7, the Muffle furnace presoma of the aluminium oxide nano material of described rear earth lanthanum doping being placed in 1000 DEG C are calcined, and obtain the aluminium oxide nano material of rear earth lanthanum doping.
Wherein, in described step 3, the concrete preparation method of sodium aluminate solution is:
Solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in 120 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 150 DEG C of standing 2h, the molar ratio obtaining sodium/aluminium is the sodium aluminate solution of 5:1.
< embodiment 3>
Step one, preparation 100mL concentration are the liquor alumini chloridi of 0.9mol/L;
Step 2, be 1:3 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with 5mL lanthanum chloride solution;
Step 3, prepare with NaOH and aluminium hydroxide the sodium aluminate solution that sodium/aluminum ratio is 9:1 respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described lanthanum chloride solution and described sodium aluminate solution are added drop-wise in described liquor alumini chloridi simultaneously, be added drop-wise in described sodium aluminate solution completely to described lanthanum chloride solution, stop dripping when then pH value being adjusted to 8.4 with described sodium aluminate solution, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 90 DEG C temperature under crystallization 4h, obtain white depositions;
Step 6, step 5 crystallization is completed the white depositions obtained carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining the aluminium oxide nano material of rear earth lanthanum doping;
Step 7, the Muffle furnace presoma of the aluminium oxide nano material of described rear earth lanthanum doping being placed in 800 DEG C are calcined, and obtain the aluminium oxide nano material of rear earth lanthanum doping.
Wherein, in described step 3, the concrete preparation method of sodium aluminate solution is:
Solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in 90 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 170 DEG C of standing 2h, the molar ratio obtaining sodium/aluminium is the sodium aluminate solution of 9:1.
< embodiment 4>
Step one, preparation 100mL concentration are the liquor alumini chloridi of 0.9mol/L;
Step 2, be 1:2.5 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with 5mL lanthanum chloride solution;
Step 3, prepare with NaOH and aluminium hydroxide the sodium aluminate solution that sodium/aluminum ratio is 9:1 respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described lanthanum chloride solution and described sodium aluminate solution are added drop-wise in described liquor alumini chloridi simultaneously, be added drop-wise in described sodium aluminate solution completely to described lanthanum chloride solution, stop dripping when then pH value being adjusted to 7.0 with described sodium aluminate solution, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 100 DEG C temperature under crystallization 12h, obtain white depositions;
Step 6, step 5 crystallization is completed the white depositions obtained carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining the aluminium oxide nano material of rear earth lanthanum doping;
Step 7, the Muffle furnace presoma of the aluminium oxide nano material of described rear earth lanthanum doping being placed in 1200 DEG C are calcined, and obtain the aluminium oxide nano material of rear earth lanthanum doping.
Wherein, in described step 3, the concrete preparation method of sodium aluminate solution is:
Solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in 100 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 160 DEG C of standing 2h, the molar ratio obtaining sodium/aluminium is the sodium aluminate solution of 9:1.
< embodiment 5>
Step one, preparation 100mL concentration are the liquor alumini chloridi of 0.9mol/L;
Step 2, be 1:2.5 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with 5mL lanthanum chloride solution;
Step 3, prepare with NaOH and aluminium hydroxide the sodium aluminate solution that sodium/aluminum ratio is 9:1 respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described sodium aluminate solution is added drop-wise in described liquor alumini chloridi simultaneously, stops dripping when pH value being adjusted to 7.0, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 100 DEG C temperature under crystallization 12h, obtain white depositions;
Step 6, step 5 crystallization is completed the white depositions obtained carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining aluminium oxide nano material;
Step 7, the Muffle furnace presoma of described aluminium oxide nano material being placed in 1200 DEG C are calcined, and obtain aluminium oxide nano material.
Wherein, in described step 3, the concrete preparation method of sodium aluminate solution is:
Solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in 100 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 160 DEG C of standing 2h, the molar ratio obtaining sodium/aluminium is the sodium aluminate solution of 9:1.
In order to better illustrate that the heat endurance of the aluminium oxide nano material of rear earth lanthanum doping is higher than aluminium oxide nano material, the calcining in the Muffle furnace of 1200 DEG C obtained < embodiment 4> respectively obtains the aluminium oxide nano material that the aluminium oxide nano material of rear earth lanthanum doping and < embodiment 5> obtain and has carried out XRD analysis, in Fig. 1, a is doping lanthanum XRD, b is unadulterated XRD, as can be seen from spectrogram 1, a is α-Al
2o
3with θ-Al
2o
3mixed phase, and b is α-Al
2o
3pure phase, therefore the existence of lanthanum prevents the generation of α phase, can prove that the heat endurance of the aluminium oxide nano material of doping lanthanum is greater than the heat endurance of aluminium oxide nano material.
Although embodiment of the present invention are open as above, it is not restricted to listed in description and embodiment utilization.It can be applied to various applicable the field of the invention completely.For those skilled in the art, can easily realize other amendment.Therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (9)
1. a preparation method for the aluminium oxide nano material of rear earth lanthanum doping, is characterized in that, comprise the following steps:
Step one, compound concentration are the liquor alumini chloridi of 0.8 ~ 0.9mol/L;
Step 2, be 1:1 ~ 1:5 according to lanthanum ion and aluminum ions mol ratio, take solid chlorine lanthanum, and be mixed with lanthanum chloride solution;
Step 3, be 3:1 ~ 9:1 according to the mol ratio of sodium/aluminium, prepare sodium aluminate solution with NaOH and aluminium hydroxide respectively;
Step 4, employing two methods, under the mixing speed of 800 ~ 1300r/min, described lanthanum chloride solution and described sodium aluminate solution are added drop-wise in described liquor alumini chloridi simultaneously, be added drop-wise in described liquor alumini chloridi completely to described lanthanum chloride solution, stop dripping when then pH value being adjusted to 1.0 ~ 8.4 with described sodium aluminate solution, continue to stir 15min under the mixing speed of 1300r/min, obtain white suspension;
Step 5, described white suspension is placed in 60 ~ 180 DEG C temperature under the crystallization scheduled time, obtain white depositions;
Step 6, the white depositions obtained is completed to step 5 crystallization carry out filtration washing or centrifuge washing, the baking oven that the filter cake that washing obtains is placed in 60 DEG C is dried, after drying 4h, takes out the presoma obtaining the aluminium oxide nano material of rear earth lanthanum doping;
Step 7, the Muffle furnace presoma of the aluminium oxide nano material of described rear earth lanthanum doping being placed in 400 ~ 1200 DEG C are calcined, and obtain the aluminium oxide nano material of rear earth lanthanum doping.
2. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 1, it is characterized in that, in described step 3, the concrete preparation method of sodium aluminate solution is:
Be 3:1 ~ 9:1 according to the mol ratio of sodium/aluminium, solid sodium hydroxide and solid aluminum hydroxide is taken in the inner bag of autoclave, then 50g is added water to, the inner bag of described autoclave is put into autoclave in the temperature of 70 ~ 120 DEG C, 2h is placed under the rotating speed of 30 ~ 50r/min, then at 150 ~ 180 DEG C, leave standstill 2h, obtain described sodium aluminate solution.
3. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 1, it is characterized in that, the pH value in described step 4 is 6.0 ~ 7.0.
4. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 1, it is characterized in that, the temperature in described step 5 is 80 ~ 90 DEG C.
5. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 1, it is characterized in that, in described step 2, the volume of lanthanum chloride solution and the volume ratio of described liquor alumini chloridi are 1:15 ~ 1:20.
6. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 1, it is characterized in that, the scheduled time in described step 5 is 2 ~ 18h.
7. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 6, it is characterized in that, the described scheduled time is 4h.
8. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 2, is characterized in that, the inner bag of described autoclave is put into autoclave in the temperature of 90 DEG C, place 2h under the rotating speed of 30 ~ 50r/min.
9. the preparation method of the aluminium oxide nano material of rear earth lanthanum doping as claimed in claim 2, it is characterized in that, described dwell temperature is 170 DEG C.
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| CN103204527A (en) * | 2013-03-22 | 2013-07-17 | 清华大学深圳研究生院 | Gamma-alumina particles and method for manufacturing same |
| CN104549546A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Alumina carrier, preparation and silver catalyst |
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| CN103204527A (en) * | 2013-03-22 | 2013-07-17 | 清华大学深圳研究生院 | Gamma-alumina particles and method for manufacturing same |
| CN104549546A (en) * | 2013-10-29 | 2015-04-29 | 中国石油化工股份有限公司 | Alumina carrier, preparation and silver catalyst |
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