CN105056876B - A kind of preparation method and application of rare earth Yt doped aluminium oxide nano material - Google Patents
A kind of preparation method and application of rare earth Yt doped aluminium oxide nano material Download PDFInfo
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Abstract
The present invention provides a kind of preparation method and application of rare earth Yt doped aluminium oxide nano material, including：Step 1: preparing aluminum sulfate solution；Step 2: preparing sodium aluminate solution；Step 3: sodium aluminate solution is added drop-wise in aluminum sulfate solution, suspension is obtained；Step 4: suspension progress aging is obtained into white depositions；Step 5: being washed to white depositions；Step 6: white depositions after washing and cetyltriethylammonium bromide are added to the water, mixed liquor is obtained；Step 7: rare earth yttrium nitrate is added in mixed liquor, rare earth mixed liquor is obtained；Step 8: rare earth mixed liquor is carried out into static crystallization, then dry, obtain the presoma of rare earth Yt doped aluminium oxide nano material；Step 9: calcining to obtain rare earth Yt doped aluminium oxide nano material, use it for adsorbing the arsenic in water.Nano material prepared by the present invention has the uniform property of uniform doping and crystal aperture, and available for the arsenic in absorption water, has a good application prospect.
Description
Technical field
The present invention relates to the preparation method of rear-earth-doped oxidation aluminium nano material.It is more particularly related to a kind of
The preparation method of rare earth Yt doped aluminium oxide nano material.
Background technology
The peculiar property that nano particle has makes it in catalyst, functional material, composite, optical material and ceramic material
There is wide real and potential application prospect in terms of material.For example, nano particle has high specific surface area and high table
Face activity, using it for catalysis material has significant catalytic efficiency.
It is well known that a series of phase transformation can occur in calcination process for aluminum oxide, the aluminum oxide of stable phase is finally given
(α-Al2O3), wherein the crystal formation of intermediate state is γ-Al in transition state of alumina, and transition state of alumina2O3With δ-Al2O3By
In specific surface area is big, crystalline phase wide temperature range, surface be referred to as activated alumina but also with characteristics such as acidity, be widely used in and urge
Agent carrier.But for high temperature reaction systems, the temperature of beds in practical operation such as purifying vehicle exhaust, catalysis burnings
Degree is usually above 1000 degree, and the sintering and α phase transformations for aoxidizing aluminium surface can cause surface area to reduce sharply and cause catalyst inactivation, therefore
The high activated alumina of heat endurance is needed in catalytic field, improving the heat endurance of aluminum oxide has important practical significance.
Research finds that addition impurity element can improve the heat endurance of activated alumina, and as improving, oxidation aluminothermy is steady
Qualitatively additive is generally rare-earth oxide, alkaline earth oxide etc., and effect is significantly, is improving aluminum oxide at present
Heat endurance when, usually using dipping by the way of (addition additive), i.e., the surface of aluminum oxide is modified, passes through modification
To increase the stability of aluminum oxide, other addition manners are lacked and studied.
In view of more than, the invention provides a kind of preparation method and applications of rare earth Yt doped aluminium oxide nano material.
The content of the invention
The present invention is in view of the above-mentioned problems, there is provided a kind of uniform doping, the homogeneous rare earth Yt doped aluminum oxide in crystal aperture
The preparation method of nano material.
Received it is an object of the invention to the rare earth Yt doped aluminium oxide nano material prepared by hydro-thermal method with aluminum oxide
Rice material is compared, with higher heat endurance.
A further object of the invention is the arsenic that the rare earth Yt doped aluminium oxide nano material prepared can be used in absorption water,
And advantages of good adsorption effect.
Therefore, the invention provides a kind of preparation method of rare earth Yt doped aluminium oxide nano material, comprising the following steps：
Step 1: compound concentration is 0.2~0.7mol/L aluminum sulfate solution；
Step 2: being 2 according to the amount of the material of sodium/aluminium:1~8:1 ratio, hydrogen is weighed in the inner bag of autoclave
Sodium oxide molybdena and solid aluminum hydroxide, then add water to 100g, by the inner bag of the autoclave be put into autoclave in
70~120 DEG C, 2h is placed under 30~50r/min rotating speed, is then stood 2h at 150~180 DEG C, is obtained sodium aluminate solution；
Step 3: under 800~1300r/min mixing speed, by the sodium aluminate solution with 1~3 drop/sec of drop
Acceleration is added drop-wise in the aluminum sulfate solution, is 8.0~10.0 to pH value, is obtained suspension；
Step 4: the suspension is transferred in reactor, it is 50~80 DEG C, rotating speed that the reactor is placed in into temperature
For 6~10h of aging under conditions of 10~30r/min, white depositions are obtained；
Step 5: being washed with deionized water to the white depositions, do not generated with barium chloride reaction to cleaning solution
Precipitation and cleaning solution pH value be 7.0 untill, white depositions after being washed；
Step 6: according to white depositions after washing：Water：The mass ratio of cetyltriethylammonium bromide is 1:16:
0.02, white depositions after the washing and cetyltriethylammonium bromide are added to the water, mixed liquor is obtained；
Step 7: the ratio between amount of material according to rare earth yttrium nitrate and aluminum sulfate solution is 1%~10%, by the rare earth
Yttrium nitrate is added in the mixed liquor, obtains rare earth mixed liquor；
Step 8: the rare earth mixed liquor is transferred in reactor, carried out at a temperature of being placed in 120~200 DEG C quiet
State crystallization, then it is dried at 80 DEG C, obtains the presoma of rare earth Yt doped aluminium oxide nano material；
Step 9: the presoma of the rare earth Yt doped aluminium oxide nano material is calcined at 500~1200 DEG C,
Obtain rare earth Yt doped aluminium oxide nano material.
Rare earth Yt doped aluminium oxide nano material is prepared using two-step method, because rare-earth yttrium is easily given birth under alkaline environment
Into precipitation, in order to avoid influenceing effect of adulterating due to the generation that yttrium hydroxide is precipitated, select to generate in the basic conditions first
White depositions, the white depositions are the boehmite that aluminum sulfate reacts generation with sodium metaaluminate, by washing pH value
Drop to 7 or so and remove sulfate ion, then the doping of rare earth ion is being carried out, in order to ensure to mix during doping
The uniform pore diameter of miscellaneous uniform crystal, first with the addition of Surfactant CTAB, is then doped；Calcining heat can influence rare earth
The specific surface area of doped yttrium aluminium oxide nano material, therefore nano material prepared by different calcining heats has different purposes.
Preferably, wherein, in the step 8, time of static crystallization is 10~30h.
Preferably, wherein, the temperature of the step 4 is 60~70 DEG C, and ageing time is 8h.
Preferably, wherein, in the step 8 static crystallization time be 16h.
Preferably, wherein, in the step 9 calcining heat be 500~600 DEG C.
Preferably, wherein, in the step 3, when pH value is not more than 6.0, the mixing speed be 800~
1000r/min；When pH value is more than 6.0, the mixing speed is 1000~1300r/min.
A kind of described rare earth Yt doped aluminium oxide nano material is used to adsorb the arsenic in water, comprises the following steps：
Step 1: weighing rare earth Yt doped aluminium oxide nano material described in 0.1g~0.5g, 100mL is added it to be measured
In arsenic solution, continuously stir after 10~180min and filtered at room temperature, solution after being adsorbed；
Step 2: measuring molten after the arsenic solution to be measured and the absorption respectively using inductively coupled plasma mass spectrometry
The concentration of arsenic in liquid, and calculate adsorption rate and adsorption capacity.
Preferably, wherein, the adsorption rate and adsorption capacity are respectively：
W=(C0-Ct)/C0* 100%；
Q=(C0-Ct)V/m；
Wherein, W is adsorption rate, and Q is adsorption capacity, C0For the concentration of arsenic solution to be measured, CtSolution after being adsorbed for the t times
Concentration, V is the volume of arsenic solution to be measured；M is the quality of rare earth Yt doped aluminium oxide nano material.
The present invention at least includes following beneficial effect：
1st, the present invention prepares rare earth Yt doped aluminium oxide nano material by hydrothermal synthesis method, with conventional rare-earth oxidation
Thing is to alumina surface-modified difference, by the preparation method of the present invention, and rare earth ruthenium ion can enter the lattice of aluminum oxide and lead to
The contact crossed between the structure for preventing aluminum ions diffusion and stable aluminum oxide, limitation particle, so as to suppress sintering, makes aluminum oxide
Carrier is remained to after high temperature ageing with certain specific surface area.
2nd, the present invention prepares rare earth Yt doped aluminium oxide nano material using two-step method, due to the rare earth under alkaline environment
Yttrium easily generates precipitation, in order to avoid influenceing effect of adulterating due to the generation that yttrium hydroxide is precipitated, selects first in alkaline bar
White depositions are generated under part, the white depositions are the boehmite that aluminum sulfate reacts generation with sodium metaaluminate, by washing
Wash and pH value is dropped to 7 or so and sulfate ion is removed, then carrying out the doping of rare earth ion, be during doping
Ensure uniform doping and the uniform pore diameter of crystal, Surfactant CTAB is with the addition of first, be then doped；Calcining heat
The specific surface area of rare earth Yt doped aluminium oxide nano material can be influenceed, therefore nano material prepared by different calcining heats has not
Same purposes.
3rd, the rare earth Yt doped aluminium oxide nano material for preparing of the present invention has a uniform doping, homogeneous excellent in crystal aperture
Point, the nano material after high-temperature calcination has an excellent heat endurance, thus rare earth Yt doped aluminium oxide nano material compared with
Aluminium oxide nano material has the broader scope of application.
4th, rare earth Yt doped aluminium oxide nano material prepared by the relatively low calcining heat of present invention selection can be used for absorption water
In arsenic, and with excellent adsorption effect.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Embodiment
The present invention is described in further detail below, to make those skilled in the art being capable of evidence with reference to specification word
To implement.
<Embodiment 1>
A kind of preparation method of rare earth Yt doped aluminium oxide nano material, comprises the following steps：
Step 1: compound concentration is 0.2mol/L aluminum sulfate solution；
Step 2: being 2 according to the amount of the material of sodium/aluminium:1 ratio, hydroxide is weighed in the inner bag of autoclave
Sodium and solid aluminum hydroxide, then add water to 100g, and the inner bag of the autoclave is put into autoclave in 70 DEG C,
2h is placed under 30~50r/min rotating speed, then 2h is stood at 150 DEG C, obtains sodium aluminate solution；
Step 3: under 800~1300r/min mixing speed, by the sodium aluminate solution with 1 drop/sec of dropwise addition
Speed is added drop-wise in the aluminum sulfate solution, is 8.0 to pH value, is obtained suspension；When pH value is not more than 6.0, the stirring
Speed is 800~1000r/min；When pH value is more than 6.0, the mixing speed is 1000~1300r/min；
Step 4: the suspension is transferred in reactor, the reactor is placed in temperature for 50 DEG C, rotating speed is 10
Aging 6h under conditions of~30r/min, obtains white depositions；
Step 5: being washed with deionized water to the white depositions, do not generated with barium chloride reaction to cleaning solution
Precipitation and cleaning solution pH value be 7.0 untill, white depositions after being washed；
Step 6: according to white depositions after washing：Water：The mass ratio of cetyltriethylammonium bromide is 1:16:
0.02, white depositions after the washing and cetyltriethylammonium bromide are added to the water, mixed liquor is obtained；
Step 7: the ratio between amount of material according to rare earth yttrium nitrate and aluminum sulfate solution is 1%, by the rare earth yttrium nitrate
It is added in the mixed liquor, obtains rare earth mixed liquor；
Step 8: the rare earth mixed liquor is transferred in reactor, carried out at a temperature of being placed in 120 DEG C static brilliant
Change, then it is dried at 80 DEG C, obtain the presoma of rare earth Yt doped aluminium oxide nano material；
Step 9: the presoma of the rare earth Yt doped aluminium oxide nano material is calcined at 800 DEG C, obtain dilute
Native doped yttrium aluminium oxide nano material.
The particle diameter of the rare earth Yt doped aluminium oxide nano material is 18nm, and uniform particle sizes.Through 800 DEG C calcine obtain it is dilute
There is not the characteristic peak of yittrium oxide in native doped yttrium aluminium oxide nano material, is γ-Al2O3With θ-Al2O3Characteristic peak.
<Embodiment 2>
A kind of preparation method of rare earth Yt doped aluminium oxide nano material, comprises the following steps：
Step 1: compound concentration is 0.7mol/L aluminum sulfate solution；
Step 2: being 8 according to the amount of the material of sodium/aluminium:1 ratio, hydroxide is weighed in the inner bag of autoclave
Sodium and solid aluminum hydroxide, then add water to 100g, and the inner bag of the autoclave is put into autoclave in 120
DEG C, 2h is placed under 30~50r/min rotating speed, then 2h is stood at 180 DEG C, obtains sodium aluminate solution；
Step 3: under 800~1300r/min mixing speed, by the sodium aluminate solution with 3 drops/sec of dropwise addition
Speed is added drop-wise in the aluminum sulfate solution, is 10.0 to pH value, is obtained suspension；When pH value is not more than 6.0, the stirring
Speed is 800~1000r/min；When pH value is more than 6.0, the mixing speed is 1000~1300r/min；
Step 4: the suspension is transferred in reactor, the reactor is placed in temperature for 80 DEG C, rotating speed is 10
Aging 10h under conditions of~30r/min, obtains white depositions；
Step 5: being washed with deionized water to the white depositions, do not generated with barium chloride reaction to cleaning solution
Precipitation and cleaning solution pH value be 7.0 untill, white depositions after being washed；
Step 6: according to white depositions after washing：Water：The mass ratio of cetyltriethylammonium bromide is 1:16:
0.02, white depositions after the washing and cetyltriethylammonium bromide are added to the water, mixed liquor is obtained；
Step 7: the ratio between amount of material according to rare earth yttrium nitrate and aluminum sulfate solution is 10%, by the rare earth nitric acid
Yttrium is added in the mixed liquor, obtains rare earth mixed liquor；
Step 8: the rare earth mixed liquor is transferred in reactor, carried out at a temperature of being placed in 200 DEG C static brilliant
Change, then it is dried at 80 DEG C, obtain the presoma of rare earth Yt doped aluminium oxide nano material；
Step 9: the presoma of the rare earth Yt doped aluminium oxide nano material is calcined at 1200 DEG C, obtain
Rare earth Yt doped aluminium oxide nano material.
The particle diameter of the rare earth Yt doped aluminium oxide nano material is 35nm, uniform particle sizes.Through 1200 DEG C calcine obtain it is dilute
There is not the characteristic peak of yittrium oxide in native doped yttrium aluminium oxide nano material, is α-Al2O3With δ-Al2O3Characteristic peak.
<Embodiment 3>
A kind of preparation method of rare earth Yt doped aluminium oxide nano material, comprises the following steps：
Step 1: compound concentration is 0.2~0.7mol/L aluminum sulfate solution；
Step 2: being 2 according to the amount of the material of sodium/aluminium:1~8:1 ratio, hydrogen is weighed in the inner bag of autoclave
Sodium oxide molybdena and solid aluminum hydroxide, then add water to 100g, by the inner bag of the autoclave be put into autoclave in
70~120 DEG C, 2h is placed under 30~50r/min rotating speed, is then stood 2h at 150~180 DEG C, is obtained sodium aluminate solution；
Step 3: under 800~1300r/min mixing speed, by the sodium aluminate solution with 1~3 drop/sec of drop
Acceleration is added drop-wise in the aluminum sulfate solution, is 8.0~10.0 to pH value, is obtained suspension；When pH value is not more than 6.0,
The mixing speed is 800~1000r/min；When pH value is more than 6.0, the mixing speed is 1000~1300r/min.
Step 4: the suspension is transferred in reactor, the reactor is placed in temperature for 60 DEG C, rotating speed is 10
Aging 8h under conditions of~30r/min, obtains white depositions；
Step 5: being washed with deionized water to the white depositions, do not generated with barium chloride reaction to cleaning solution
Precipitation and cleaning solution pH value be 7.0 untill, white depositions after being washed；
Step 6: according to white depositions after washing：Water：The mass ratio of cetyltriethylammonium bromide is 1:16:
0.02, white depositions after the washing and cetyltriethylammonium bromide are added to the water, mixed liquor is obtained；
Step 7: the ratio between amount of material according to rare earth yttrium nitrate and aluminum sulfate solution is 5%, by the rare earth yttrium nitrate
It is added in the mixed liquor, obtains rare earth mixed liquor；
Step 8: the rare earth mixed liquor is transferred in reactor, carried out at a temperature of being placed in 120~200 DEG C quiet
State crystallization 16h, then it is dried at 80 DEG C, obtains the presoma of rare earth Yt doped aluminium oxide nano material；
Step 9: the presoma of the rare earth Yt doped aluminium oxide nano material is calcined at 500 DEG C, obtain dilute
Native doped yttrium aluminium oxide nano material.
The particle diameter of the rare earth Yt doped aluminium oxide nano material is 15nm, uniform particle sizes.Through 1200 DEG C calcine obtain it is dilute
There is not the characteristic peak of yittrium oxide in native doped yttrium aluminium oxide nano material, is γ-Al2O3With a small amount of AlOOH characteristic peak.
The rare earth Yt doped aluminium oxide nano material that embodiment 3 is obtained is used to adsorb the arsenic in water, concretely comprises the following steps：
Step 1: weighing rare earth Yt doped aluminium oxide nano material described in 0.1g, 100mL arsenic solutions to be measured are added it to
In, continuously stir after 10~180min and filtered at room temperature, solution after being adsorbed；
Step 2: measuring molten after the arsenic solution to be measured and the absorption respectively using inductively coupled plasma mass spectrometry
The concentration of arsenic in liquid, and calculate adsorption rate and adsorption capacity.
Wherein, adsorption rate and adsorption capacity are respectively：
W=(C0-Ct)/C0* 100%；
Q=(C0-Ct)V/m；
W is adsorption rate, and Q is adsorption capacity, C0For the concentration of arsenic solution to be measured, CtThe concentration of solution, V after being adsorbed for the t times
For the volume of arsenic solution to be measured；M is the quality of rare earth Yt doped aluminium oxide nano material.
Test result is：The concentration of arsenic solution to be measured is 1.0mg/L, and the concentration of solution is 0.250 × 10 after absorption-3mg/
L, is calculated, adsorption rate W=99.96%, adsorption capacity Q=0.2000mg/g.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With.It can be applied to various suitable the field of the invention completely., can be easily for those skilled in the art
Realize other modification.Therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details.
Claims (8)
1. a kind of preparation method of rare earth Yt doped aluminium oxide nano material, it is characterised in that comprise the following steps：
Step 1: compound concentration is 0.2~0.7mol/L aluminum sulfate solution；
Step 2: being 2 according to the amount of the material of sodium/aluminium:1~8:1 ratio, hydroxide is weighed in the inner bag of autoclave
Sodium and solid aluminum hydroxide, then add water to 100g, the inner bag of the autoclave is put into autoclave in 70~
120 DEG C, 2h is placed under 30~50r/min rotating speed, is then stood 2h at 150~180 DEG C, is obtained sodium aluminate solution；
Step 3: under 800~1300r/min mixing speed, by the sodium aluminate solution with 1~3 drop/sec of dropwise addition speed
Degree is added drop-wise in the aluminum sulfate solution, is 8.0~10.0 to pH value, is obtained suspension；
Step 4: the suspension is transferred in reactor, the reactor is placed in temperature for 50~80 DEG C, rotating speed is 10
6~10h of aging under conditions of~30r/min, obtains white depositions；
Step 5: being washed with deionized water to the white depositions, precipitation is not generated to cleaning solution and barium chloride reaction
And untill the pH value of cleaning solution is 7.0, white depositions after being washed；
Step 6: according to white depositions after washing：Water：The mass ratio of cetyltriethylammonium bromide is 1:16:0.02, will
White depositions and cetyltriethylammonium bromide are added to the water after the washing, obtain mixed liquor；
Step 7: the ratio between amount of material according to rare earth yttrium nitrate and aluminum sulfate solution is 1%~10%, by the rare earth nitric acid
Yttrium is added in the mixed liquor, obtains rare earth mixed liquor；
Step 8: the rare earth mixed liquor is transferred in reactor, carried out at a temperature of being placed in 120~200 DEG C static brilliant
Change, then it is dried at 80 DEG C, obtain the presoma of rare earth Yt doped aluminium oxide nano material；
Step 9: the presoma of the rare earth Yt doped aluminium oxide nano material is calcined at 500~1200 DEG C, obtain
Rare earth Yt doped aluminium oxide nano material.
2. the preparation method of rare earth Yt doped aluminium oxide nano material as claimed in claim 1, it is characterised in that the step
In eight, the time of static crystallization is 10~30h.
3. the preparation method of rare earth Yt doped aluminium oxide nano material as claimed in claim 1, it is characterised in that the step
Four temperature is 60~70 DEG C, and ageing time is 8h.
4. the preparation method of rare earth Yt doped aluminium oxide nano material as claimed in claim 2, it is characterised in that the step
The static crystallization time is 16h in eight.
5. the preparation method of rare earth Yt doped aluminium oxide nano material as claimed in claim 1, it is characterised in that the step
Calcining heat is 500~600 DEG C in nine.
6. the preparation method of rare earth Yt doped aluminium oxide nano material as claimed in claim 1, it is characterised in that the step
In three, when pH value is not more than 6.0, the mixing speed is 800~1000r/min；When pH value is more than 6.0, the stirring
Speed is 1000~1300r/min.
7. rare earth Yt doped aluminium oxide nano material prepared by a kind of the method as described in claim 1 is used to adsorb in water
Arsenic, it is characterised in that comprise the following steps：
Step 1: weighing rare earth Yt doped aluminium oxide nano material described in 0.1g~0.5g, 100mL arsenic to be measured is added it to molten
In liquid, continuously stir after 10~180min and filtered at room temperature, solution after being adsorbed；
Step 2: being measured respectively using inductively coupled plasma mass spectrometry after the arsenic solution to be measured and the absorption in solution
The concentration of arsenic, and calculate adsorption rate and adsorption capacity.
8. rare earth Yt doped aluminium oxide nano material as claimed in claim 7 is used to adsorb the arsenic in water, it is characterised in that institute
State adsorption rate and adsorption capacity is respectively：
W=(C0-Ct)/C0* 100%；
Q=(C0-Ct)V/m；
Wherein, W is adsorption rate, and Q is adsorption capacity, C0For the concentration of arsenic solution to be measured, CtThe concentration of solution after being adsorbed for the t times,
V is the volume of arsenic solution to be measured；M is the quality of rare earth Yt doped aluminium oxide nano material.
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