CN105460963B - Preparation method of nanometer mesoporous alumina - Google Patents
Preparation method of nanometer mesoporous alumina Download PDFInfo
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- CN105460963B CN105460963B CN201510918871.6A CN201510918871A CN105460963B CN 105460963 B CN105460963 B CN 105460963B CN 201510918871 A CN201510918871 A CN 201510918871A CN 105460963 B CN105460963 B CN 105460963B
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Abstract
The invention provides a preparation method of nanometer mesoporous alumina. The preparation method comprises the steps that firstly, a red pomegranate extracting solution is prepared; secondly, aluminum sulfate is weighed and dissolved in the red pomegranate extracting solution to prepare an aluminum sulfate solution; thirdly, ammonium hydroxide is dropwise added into the aluminum sulfate solution till the pH value is 8.0-9.5, and alumina sol is obtained; fourthly, aging treatment at gradient temperature is carried out on the alumina sol to obtain alumina gel; fifthly, the alumina gel is filtered, washed and dried after being cooled to room temperature, and the dried alumina gel is roasted to obtain the nanometer mesoporous alumina. The pore size of the nanometer mesoporous alumina prepared through the preparation method is 3-4 nm, the specific surface area of the alumina is large, the good adsorption performance is good, and meanwhile the nanometer mesoporous alumina is simple in preparation technology, low in cost and environmentally friendly.
Description
Technical field
The present invention relates to the preparation method of nano material.It is more particularly related to a kind of mesoporous nano-alumina
Preparation method.
Background technology
The peculiar property that nano particle has makes it in catalyst, functional material, composite, optical material and ceramic material
The aspects such as material have wide reality with potential application prospect.For example, nano particle has high specific surface area and high table
Face activity, using it for catalysis material has significant catalytic efficiency.
Aluminum oxide, particularly γ-Al2O3, with suitable specific surface area, pore volume and pore-size distribution, good mechanical strength
And heat endurance, it is widely used in chemical industry as catalyst, carrier and adsorbent.The preparation of aluminum oxide generally adopts soda acid
Neutralization generates boehmite, then forms aluminum oxide by roasting.Following a few classes can be divided into according to raw material:(1) acid precipitation method,
That is the neutralization reaction of aluminium salt and alkali, the aluminium salt of employing has aluminium chloride, aluminum nitrate and aluminum sulfate etc., alkali have ammoniacal liquor, NaOH and
Potassium hydroxide etc.;(2) alkaline precipitation, i.e. aluminate and the neutralization reaction of acid, aluminium salt used is mainly sodium metaaluminate and inclined aluminium
Sour potassium, acid used has nitric acid, sulfuric acid, hydrochloric acid and carbon dioxide etc.;(3) the double decomposition neutralization reaction of aluminium salt and aluminate.
In view of more than, it would be highly desirable to have a kind of in the case of without template, prepare the high mesoporous nano of specific surface area
Aluminum oxide.
The content of the invention
The present invention is directed to the problems referred to above, there is provided a kind of preparation method of mesoporous nano-alumina, the preparation method technique
Process is simple, environmental friendliness, and the specific surface area of the aluminum oxide for preparing is high and particle diameter is mesoporous nano.
For this purpose, the invention provides a kind of preparation method of mesoporous nano-alumina, comprises the following steps:
Step one, dry red pomegranate flower is added in the ethanol that percent by volume is 80% it is heated to reflux, is obtained
To alcohol extracting thing;The alcohol extracting thing is extracted successively with petroleum ether, chloroform, ethyl acetate and n-butanol, is extracted
Part and aqueous fraction;By the aqueous fraction Jing after molecular sieve adsorption, with the methyl alcohol that percent by volume is 100% to adsorption liquid
Eluted, collected eluent, the eluent is added in activated carbon and is decolourized, obtained red pomegranate extract;
Step 2, a certain amount of aluminum sulfate is weighed, in being dissolved in the red pomegranate extract, it is made into concentration for 0.3~
The aluminum sulfate solution of 0.6mol/L;
Step 3,1000~3000r/min mixing speed and 30~40 DEG C at a temperature of, by concentration be 1~3mol/
The ammonium hydroxide of L is slowly added drop-wise in aluminum sulfate solution described in 200mL, is 8.0~9.5 to pH value, obtains Alumina gel;
Step 4, the Alumina gel is transferred in reactor, the burin-in process of gradient temperature is carried out to the reactor,
Alumina gel is obtained, wherein, the burin-in process of the gradient temperature is specifically divided into three temperature stages;
Step 5, the alumina gel is cooled to after room temperature carries out filtration washing, by the aluminum oxide after filtration washing
Gel is placed in 60~80 DEG C of baking oven and is dried, by the alumina gel after drying at 400~1200 DEG C roasting 2.5~
3.5h, that is, obtain mesoporous nano-alumina.
Preferably, wherein, in the step 4, the burin-in process of the gradient temperature is specially:
First temperature stage:Temperature be 30~50 DEG C, mixing speed be 300~500r/min, heating rate be 3~6 DEG C/
Min, ageing time is 5~10h;
The second temperature stage:Temperature be 50~70 DEG C, mixing speed be 200~300r/min, heating rate be 2~4 DEG C/
Min, ageing time is 4~8h;
3rd temperature stage:Temperature be 70~90 DEG C, mixing speed be 0~50r/min, heating rate be 1~3 DEG C/
Min, ageing time is 3~5h.
Preferably, wherein, in the step 5, the filtration washing is specially:
Deionized water is heated to into 40~60 DEG C, deionized water after being heated;With deionized water after the heating to institute
Stating presoma carries out multiple times of filtration, to remove sulfate ion, finally carries out filtration washing with ether.
Preferably, wherein, in the step one, dry 5~10g red pomegranates flower is added to into volume for 150~
200mL, percent by volume be 80% ethanol in be heated to reflux, obtain alcohol extracting thing.
Preferably, wherein, in the step one, the volume ratio of the petroleum ether, chloroform, ethyl acetate and n-butanol is
1~3:1~6:1~5:1~2.
Preferably, wherein, in the step 3, pH value is 9.0.
Preferably, wherein, in the step 4, the burin-in process of the gradient temperature is specially:
First temperature stage:Temperature is 40 DEG C, and mixing speed is 400r/min, and heating rate is 5 DEG C/min, ageing time
For 7h;
The second temperature stage:Temperature is 60 DEG C, and mixing speed is 230r/min, and heating rate is 3 DEG C/min, ageing time
For 5h;
3rd temperature stage:Temperature is 80 DEG C, and mixing speed is 0r/min, and heating rate is 2 DEG C/min, and ageing time is
4h。
Preferably, wherein, in the step 2, the concentration of aluminum sulfate is 0.5mol/L.
Preferably, wherein, in the step 5, the drying temperature be 65 DEG C.
The present invention at least includes following beneficial effect:
1st, the invention provides a kind of preparation method of mesoporous nano-alumina, the method preparation process is simple, environment friend
It is good, and the specific surface area of the aluminum oxide for preparing is high, advantages of good adsorption effect, pore size is 3~4nm.
2nd, the present invention has used the aging handling process of gradient temperature during mesoporous nano-alumina is prepared, due to
The generation of crystal needs the formation for experiencing nucleus, the process for growing and growing up, and the temperature that these processes need is different, and the present invention is carried
For temperature beneficial to crystal formation.
3rd, present invention uses red pomegranate flower extract, the electronegative group contained in red pomegranate flower extract, trivalent aluminium
Ion A l3+It is easy to by coordination and these electronegative group complexings.After adding alkali lye, the aluminium ion sustained release of complexing is hydroxide
Aluminium simultaneously interacts with organo-functional group.Jing certain heat treatment, alumina precursor dehydration is converted into mesoporous nano-alumina,
The remaining a small amount of group of simultaneous oxidation aluminium surface, therefore good adsorptivity can be shown during Adsorption of Heavy Metals
Can, and the presence of red pomegranate flower extract is also beneficial to the aluminum oxide that generation is mesoporous.
The further advantage of the present invention, target and feature embody part by description below, and part will also be by this
The research of invention and practice and be understood by the person skilled in the art.
Specific embodiment
Below the present invention is described in further detail, with make those skilled in the art with reference to specification word being capable of evidence
To implement.
<Embodiment 1>
The invention provides a kind of preparation method of mesoporous nano-alumina, comprises the following steps:
Step one, dry 5g red pomegranates flower is added to into volume to enter in 150mL, the ethanol that percent by volume is 80%
Row is heated to reflux, and obtains alcohol extracting thing;The alcohol extracting thing is carried out successively with petroleum ether, chloroform, ethyl acetate and n-butanol
Extraction, obtains extraction part and aqueous fraction;The volume ratio of the petroleum ether, chloroform, ethyl acetate and n-butanol is 1:3:2:
1;By the aqueous fraction Jing after molecular sieve adsorption, adsorption liquid is eluted with the methyl alcohol that percent by volume is 100%, collected
Eluent, the eluent is added in activated carbon and is decolourized, and obtains red pomegranate extract;
Step 2, a certain amount of aluminum sulfate is weighed, in being dissolved in the red pomegranate extract, being made into concentration is
The aluminum sulfate solution of 0.3mol/L;
Step 3,1000r/min mixing speed and 30 DEG C at a temperature of, concentration is delayed for the ammonium hydroxide of 1mol/L
Slow is added drop-wise in aluminum sulfate solution described in 200mL, is 8.0 to pH value, obtains Alumina gel;
Step 4, the Alumina gel is transferred in reactor, the burin-in process of gradient temperature is carried out to the reactor,
Alumina gel is obtained, wherein, the burin-in process of the gradient temperature is specifically divided into three temperature stages;Burin-in process is specially:
First temperature stage:Temperature is 30 DEG C, and mixing speed is 300r/min, and heating rate is 6 DEG C/min, ageing time
For 10h;
The second temperature stage:Temperature is 50 DEG C, and mixing speed is 200r/min, and heating rate is 4 DEG C/min, ageing time
For 8h;
3rd temperature stage:Temperature is 80 DEG C, and mixing speed is 50r/min, and heating rate is 1~3 DEG C/min, when aging
Between be 5h;
Step 5, the alumina gel is cooled to after room temperature carries out filtration washing, by the aluminum oxide after filtration washing
Gel is placed in 60 DEG C of baking oven and is dried, by the alumina gel after drying at 1200 DEG C roasting 2.5h, that is, received
Rice meso-porous alumina.
Wherein, the filtration washing is specially:
Deionized water is heated to into 40 DEG C, deionized water after being heated;With deionized water after the heating to before described
Driving body carries out multiple times of filtration, to remove sulfate ion, finally carries out filtration washing with ether.
The specific surface area of the mesoporous nano-alumina is 100m2/ g, aperture is 3.5nm, and heavy metal chromium ion (concentration
For 1mg/L) adsorbance be 100mg/g.
<Embodiment 2>
The invention provides a kind of preparation method of mesoporous nano-alumina, comprises the following steps:
Step one, dry 8g red pomegranates flower is added to into volume to enter in 200mL, the ethanol that percent by volume is 80%
Row is heated to reflux, and obtains alcohol extracting thing;The alcohol extracting thing is carried out successively with petroleum ether, chloroform, ethyl acetate and n-butanol
Extraction, obtains extraction part and aqueous fraction;It is 100% with percent by volume by the aqueous fraction Jing after molecular sieve adsorption
Methyl alcohol adsorption liquid is eluted, collect eluent, the eluent is added in activated carbon and is decolourized, obtain red stone
Pomegranate extract;The volume ratio of the petroleum ether, chloroform, ethyl acetate and n-butanol is 3:6:5:2.
Step 2, a certain amount of aluminum sulfate is weighed, in being dissolved in the red pomegranate extract, being made into concentration is
The aluminum sulfate solution of 0.5mol/L;
Step 3,3000r/min mixing speed and 40 DEG C at a temperature of, concentration is delayed for the ammonium hydroxide of 2mol/L
Slow is added drop-wise in aluminum sulfate solution described in 200mL, is 9.0 to pH value, obtains Alumina gel;
Step 4, the Alumina gel is transferred in reactor, the burin-in process of gradient temperature is carried out to the reactor,
Alumina gel is obtained, wherein, the burin-in process of the gradient temperature is specifically divided into three temperature stages;The gradient temperature it is old
Change is processed and is specially:
First temperature stage:Temperature is 40 DEG C, and mixing speed is 400r/min, and heating rate is 5 DEG C/min, ageing time
For 7h;
The second temperature stage:Temperature is 60 DEG C, and mixing speed is 230r/min, and heating rate is 3 DEG C/min, ageing time
For 5h;
3rd temperature stage:Temperature is 80 DEG C, and mixing speed is 0r/min, and heating rate is 2 DEG C/min, and ageing time is
4h。
Step 5, the alumina gel is cooled to after room temperature carries out filtration washing, by the aluminum oxide after filtration washing
Gel is put in 65 DEG C of baking oven and is dried, by the alumina gel after drying at 500 DEG C roasting 3h, that is, obtain mesoporous nano
Aluminum oxide.
The filtration washing is specially:
Deionized water is heated to into 50 DEG C, deionized water after being heated;With deionized water after the heating to before described
Driving body carries out multiple times of filtration, to remove sulfate ion, finally carries out filtration washing with ether.
The specific surface area of the mesoporous nano-alumina is 300m2/ g, aperture is 4.5nm, and heavy metal chromium ion (concentration
For 1mg/L) adsorbance be 200mg/g.
<Embodiment 3>
The invention provides a kind of preparation method of mesoporous nano-alumina, comprises the following steps:
Step one, dry 10g red pomegranates flower is added to into volume in 200mL, the ethanol that percent by volume is 80%
It is heated to reflux, is obtained alcohol extracting thing;The alcohol extracting thing is entered successively with petroleum ether, chloroform, ethyl acetate and n-butanol
Row extraction, obtains extraction part and aqueous fraction;By the aqueous fraction Jing after molecular sieve adsorption, it is with percent by volume
100% methyl alcohol is eluted to adsorption liquid, collects eluent, the eluent is added in activated carbon and is decolourized, and is obtained
Obtain red pomegranate extract;The volume ratio of the petroleum ether, chloroform, ethyl acetate and n-butanol is 1:1:1:1.
Step 2, a certain amount of aluminum sulfate is weighed, in being dissolved in the red pomegranate extract, being made into concentration is
The aluminum sulfate solution of 0.6mol/L;
Step 3,2000r/min mixing speed and 30 DEG C at a temperature of, concentration is delayed for the ammonium hydroxide of 3mol/L
Slow is added drop-wise in aluminum sulfate solution described in 200mL, is 9.5 to pH value, obtains Alumina gel;
Step 4, the Alumina gel is transferred in reactor, the burin-in process of gradient temperature is carried out to the reactor,
Alumina gel is obtained, wherein, the burin-in process of the gradient temperature is specifically divided into three temperature stages;The gradient temperature it is old
Change is processed and is specially:
First temperature stage:Temperature is 50 DEG C, and mixing speed is 500r/min, and heating rate is 3~6 DEG C/min, aging
Time is 5h;
The second temperature stage:Temperature is 70 DEG C, and mixing speed is 300r/min, and heating rate is 2~4 DEG C/min, aging
Time is 8h;
3rd temperature stage:Temperature is 90 DEG C, and mixing speed is 20r/min, and heating rate is 1~3 DEG C/min, when aging
Between be 5h.
Step 5, the alumina gel is cooled to after room temperature carries out filtration washing, by the aluminum oxide after filtration washing
Gel is placed in 80 DEG C of baking oven and is dried, by the alumina gel after drying at 400 DEG C roasting 3.5h, that is, obtain nanometer
Meso-porous alumina.
The filtration washing is specially:
Deionized water is heated to into 60 DEG C, deionized water after being heated;With deionized water after the heating to before described
Driving body carries out multiple times of filtration, to remove sulfate ion, finally carries out filtration washing with ether.
The specific surface area of the mesoporous nano-alumina is 400m2/ g, aperture is 5.5nm, and heavy metal chromium ion (concentration
For 1mg/L) adsorbance be 300mg/g.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and embodiment
With.It can be applied to completely various suitable the field of the invention.For those skilled in the art, can be easily
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 (5)
1. a kind of preparation method of mesoporous nano-alumina, it is characterised in that comprise the following steps:
Step one, dry 5~10g red pomegranates flower is added to into the second that volume is 150~200mL, percent by volume is 80%
It is heated to reflux in alcohol, is obtained alcohol extracting thing;The alcohol extracting thing is used successively petroleum ether, chloroform, ethyl acetate and positive fourth
Alcohol is extracted, and obtains extraction part and aqueous fraction;The volume ratio of the petroleum ether, chloroform, ethyl acetate and n-butanol is 1
~3:1~6:1~5:1~2;By the aqueous fraction Jing after molecular sieve adsorption, with the methyl alcohol that percent by volume is 100% to inhaling
Attached liquid is eluted, and collects eluent, the eluent is added in activated carbon and is decolourized, and obtains red pomegranate extract;
Step 2, a certain amount of aluminum sulfate is weighed, in being dissolved in the red pomegranate extract, it is made into concentration for 0.3~
The aluminum sulfate solution of 0.6mol/L;
Step 3,1000~3000r/min mixing speed and 30~40 DEG C at a temperature of, be 1~3mol/L's by concentration
Ammonium hydroxide is slowly added drop-wise in aluminum sulfate solution described in 200mL, is 8.0~9.5 to pH value, obtains Alumina gel;
Step 4, the Alumina gel is transferred in reactor, the burin-in process of gradient temperature is carried out to the reactor, obtain oxygen
Change alumina gel, wherein, the burin-in process of the gradient temperature is specifically divided into three temperature stages;
Step 5, the alumina gel is cooled to after room temperature carries out filtration washing, by the alumina gel after filtration washing
Be placed in 60~80 DEG C of baking oven and dried, by the alumina gel after drying at 400~1200 DEG C roasting 2.5~
3.5h, that is, obtain mesoporous nano-alumina;
In the step 4, the burin-in process of the gradient temperature is specially:
First temperature stage:Temperature is 40 DEG C, and mixing speed is 400r/min, and heating rate is 5 DEG C/min, and ageing time is
7h;
The second temperature stage:Temperature is 60 DEG C, and mixing speed is 230r/min, and heating rate is 3 DEG C/min, and ageing time is
5h;
3rd temperature stage:Temperature is 80 DEG C, and mixing speed is 0r/min, and heating rate is 2 DEG C/min, and ageing time is 4h.
2. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterised in that described in the step 5
Filtration washing is specially:
Deionized water is heated to into 40~60 DEG C, deionized water after being heated;With deionized water after the heating to the oxygen
Changing alumina gel carries out multiple times of filtration, to remove sulfate ion, finally carries out filtration washing with ether.
3. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterised in that in the step 3, pH value
For 9.0.
4. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterised in that in the step 2, sulfuric acid
The concentration of aluminium is 0.5mol/L.
5. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterised in that described in the step 5
Drying temperature is 65 DEG C.
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CN110156057A (en) * | 2019-06-18 | 2019-08-23 | 苏州贝尔德新材料科技有限公司 | The preparation method of high purity aluminium oxide |
CN110732305B (en) * | 2019-11-20 | 2023-03-31 | 迈海(苏州)环保科技有限公司 | Aluminum-based modified composite oxide, preparation method and application |
CN115490250A (en) * | 2022-10-24 | 2022-12-20 | 河北铭万精细化工有限公司 | Industrial production process of high-purity nano aluminum oxide |
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CN102491388A (en) * | 2011-12-02 | 2012-06-13 | 厦门大学 | Preparation method of nano mesoporous alumina |
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KR20100128024A (en) * | 2009-05-27 | 2010-12-07 | 한국지질자원연구원 | Aging method of gamma-bohemite sol with auto claver reactor for the preparation of mesoporous gamma-alumina |
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CN1594101A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
CN102491388A (en) * | 2011-12-02 | 2012-06-13 | 厦门大学 | Preparation method of nano mesoporous alumina |
CN104743572A (en) * | 2013-12-27 | 2015-07-01 | 陕西煤化工技术工程中心有限公司 | Method for synthesis of high silica-alumina ratio ultrafine NaY molecular sieve |
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Effective date of registration: 20171208 Address after: 536000, the Guangxi Zhuang Autonomous Region, Beihai, Taiwan Road, Jilin Road, Northeast China Electronics Beihai Industrial Park, room 04 East Patentee after: Beihai Ke Ke Qi Electronic Technology Co., Ltd. Address before: No. five li 17, south of the south of the Yangtze River, the Guangxi Zhuang Autonomous Region, the Guangxi Zhuang Autonomous Region Patentee before: Li Jinxiu |