CN105460963A - Preparation method of nanometer mesoporous alumina - Google Patents
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- CN105460963A CN105460963A CN201510918871.6A CN201510918871A CN105460963A CN 105460963 A CN105460963 A CN 105460963A CN 201510918871 A CN201510918871 A CN 201510918871A CN 105460963 A CN105460963 A CN 105460963A
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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.More particularly, the present invention relates to a kind of preparation method of mesoporous nano-alumina.
Background technology
The peculiar property that nano particle has makes it in catalyzer, functional materials, matrix material, optical material and stupalith etc., have wide reality and potential application prospect.Such as, nano particle has high specific surface area and high surfactivity, and using it for catalytic material has significant catalytic efficiency.
Aluminum oxide, particularly γ-Al
2o
3, there is suitable specific surface area, pore volume and pore size distribution, good physical strength and thermostability, be widely used in chemical industry as catalyzer, carrier and sorbent material.The preparation of aluminum oxide adopts acid-base neutralisation to generate pseudo-boehmite usually, then forms aluminum oxide by roasting.Can be divided into following a few class according to raw material: (1) acid precipitation method, the i.e. neutralization reaction of aluminium salt and alkali, the aluminium salt of employing has aluminum chloride, aluminum nitrate and Tai-Ace S 150 etc., and alkali has ammoniacal liquor, sodium hydroxide and potassium hydroxide etc.; (2) alkaline precipitation, i.e. the neutralization reaction of aluminate and acid, aluminium salt used mainly sodium metaaluminate and potassium metaaluminate, acid used has nitric acid, sulfuric acid, hydrochloric acid and carbonic acid gas etc.; (3) the metathesis neutralization reaction of aluminium salt and aluminate.
In view of more than, urgently having a kind of when there is no template, preparing the aluminum oxide of the high mesoporous nano of specific surface area.
Summary of the invention
The present invention is directed to the problems referred to above, provide a kind of preparation method of mesoporous nano-alumina, this preparation method's technological process is simple, environmental friendliness, and the specific surface area of the aluminum oxide of preparation is high and particle diameter is mesoporous nano.
For this reason, the invention provides a kind of preparation method of mesoporous nano-alumina, comprise the following steps:
Step one, the red Pomegranate Flower of drying is joined volume percent is carry out reflux in the ethanol of 80%, obtains alcohol extract; Described alcohol extract is extracted with sherwood oil, chloroform, ethyl acetate and propyl carbinol successively, is extracted part and aqueous fraction; By described aqueous fraction after molecular sieve adsorption, be that the methyl alcohol of 100% carries out wash-out to adsorption liquid by volume percent, collect elutriant, described elutriant is joined in gac and decolours, obtain red pomegranate extracting solution;
Step 2, take a certain amount of Tai-Ace S 150, be dissolved in described red pomegranate extracting solution, be made into the alum liquor that concentration is 0.3 ~ 0.6mol/L;
Step 3, at the temperature of the stirring velocity of 1000 ~ 3000r/min and 30 ~ 40 DEG C, the ammonium hydroxide being 1 ~ 3mol/L by concentration is added drop-wise in alum liquor described in 200mL slowly, is 8.0 ~ 9.5, obtains Alumina gel to pH value;
Step 4, be transferred in reactor by described Alumina gel, described reactor is carried out to the burin-in process of gradient temperature, obtain alumina gel, wherein, the burin-in process of described gradient temperature is specifically divided into three temperature stage;
Step 5, described alumina gel is cooled to room temperature after carry out filtration washing, the baking oven that alumina gel after filtration washing is placed in 60 ~ 80 DEG C is dried, by the alumina gel roasting 2.5 ~ 3.5h at 400 ~ 1200 DEG C after oven dry, namely obtain mesoporous nano-alumina.
Preferably, wherein, in described step 4, the burin-in process of described gradient temperature is specially:
First temperature stage: temperature is 30 ~ 50 DEG C, stirring velocity is 300 ~ 500r/min, and temperature rise rate is 3 ~ 6 DEG C/min, and digestion time is 5 ~ 10h;
Second temperature stage: temperature is 50 ~ 70 DEG C, stirring velocity is 200 ~ 300r/min, and temperature rise rate is 2 ~ 4 DEG C/min, and digestion time is 4 ~ 8h;
3rd temperature stage: temperature is 70 ~ 90 DEG C, stirring velocity is 0 ~ 50r/min, and temperature rise rate is 1 ~ 3 DEG C/min, and digestion time is 3 ~ 5h.
Preferably, wherein, in described step 5, described filtration washing is specially:
Deionized water is heated to 40 ~ 60 DEG C, obtains heating rear deionized water; With deionized water after described heating, multiple times of filtration is carried out to described presoma, to remove sulfate ion, finally carry out filtration washing with ether.
Preferably, wherein, in described step one, red for 5 ~ 10g of drying Pomegranate Flower is joined volume is 150 ~ 200mL, volume percent is carry out reflux in the ethanol of 80%, obtain alcohol extract.
Preferably, wherein, in described step one, the volume ratio of described sherwood oil, chloroform, ethyl acetate and propyl carbinol is 1 ~ 3:1 ~ 6:1 ~ 5:1 ~ 2.
Preferably, wherein, in described step 3, pH value is 9.0.
Preferably, wherein, in described step 4, the burin-in process of described gradient temperature is specially:
First temperature stage: temperature is 40 DEG C, stirring velocity is 400r/min, and temperature rise rate is 5 DEG C/min, and digestion time is 7h;
Second temperature stage: temperature is 60 DEG C, stirring velocity is 230r/min, and temperature rise rate is 3 DEG C/min, and digestion time is 5h;
3rd temperature stage: temperature is 80 DEG C, stirring velocity is 0r/min, and temperature rise rate is 2 DEG C/min, and digestion time is 4h.
Preferably, wherein, in described step 2, the concentration of Tai-Ace S 150 is 0.5mol/L.
Preferably, wherein, in described step 5, described bake out temperature is 65 DEG C.
The present invention at least comprises following beneficial effect:
1, the invention provides a kind of preparation method of mesoporous nano-alumina, the method preparation technology is simple, environmental friendliness, and the specific surface area of the aluminum oxide of preparation is high, and advantages of good adsorption effect, pore size is 3 ~ 4nm.
2, the present invention employs the aging treatment process of gradient temperature in the process preparing mesoporous nano-alumina, generation due to crystal needs the formation experiencing nucleus, the process growing and grow up, the temperature of these process needs is different, and temperature provided by the invention is beneficial to the formation of crystal.
3, present invention uses red Pomegranate Flower extracting solution, the electronegative group contained in red Pomegranate Flower extracting solution, trivalent aluminium ion Al
3+easily via coordination and these electronegative group complexings.After adding alkali lye, the aluminum ion slowly-releasing of complexing is aluminium hydroxide and interacts with organo-functional group.Through certain thermal treatment, alumina precursor dehydration is converted into mesoporous nano-alumina, the a small amount of group of simultaneous oxidation aluminium surface residual, therefore can show good absorption property in the process of Adsorption of Heavy Metals, and the existence of red Pomegranate Flower extracting solution is also beneficial to the mesoporous aluminum oxide of generation.
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.
Embodiment
The present invention is described in further detail below, can implement according to this with reference to specification sheets word to make those skilled in the art.
< embodiment 1>
The invention provides a kind of preparation method of mesoporous nano-alumina, comprise the following steps:
Step one, red for the 5g of drying Pomegranate Flower joined volume is 150mL, volume percent is carry out reflux in the ethanol of 80%, obtain alcohol extract; Described alcohol extract is extracted with sherwood oil, chloroform, ethyl acetate and propyl carbinol successively, is extracted part and aqueous fraction; The volume ratio of described sherwood oil, chloroform, ethyl acetate and propyl carbinol is 1:3:2:1; By described aqueous fraction after molecular sieve adsorption, be that the methyl alcohol of 100% carries out wash-out to adsorption liquid by volume percent, collect elutriant, described elutriant is joined in gac and decolours, obtain red pomegranate extracting solution;
Step 2, take a certain amount of Tai-Ace S 150, be dissolved in described red pomegranate extracting solution, be made into the alum liquor that concentration is 0.3mol/L;
Step 3, at the temperature of the stirring velocity of 1000r/min and 30 DEG C, the ammonium hydroxide being 1mol/L by concentration is added drop-wise in alum liquor described in 200mL slowly, is 8.0, obtains Alumina gel to pH value;
Step 4, be transferred in reactor by described Alumina gel, described reactor is carried out to the burin-in process of gradient temperature, obtain alumina gel, wherein, the burin-in process of described gradient temperature is specifically divided into three temperature stage; Burin-in process is specially:
First temperature stage: temperature is 30 DEG C, stirring velocity is 300r/min, and temperature rise rate is 6 DEG C/min, and digestion time is 10h;
Second temperature stage: temperature is 50 DEG C, stirring velocity is 200r/min, and temperature rise rate is 4 DEG C/min, and digestion time is 8h;
3rd temperature stage: temperature is 80 DEG C, stirring velocity is 50r/min, and temperature rise rate is 1 ~ 3 DEG C/min, and digestion time is 5h;
Step 5, described alumina gel is cooled to room temperature after carry out filtration washing, the baking oven that the alumina gel after filtration washing is placed in 60 DEG C is dried, by dry after alumina gel roasting 2.5h at 1200 DEG C, namely obtain mesoporous nano-alumina.
Wherein, described filtration washing is specially:
Deionized water is heated to 40 DEG C, obtains heating rear deionized water; With deionized water after described heating, multiple times of filtration is carried out to described presoma, to remove sulfate ion, finally carry out filtration washing with ether.
The specific surface area of this mesoporous nano-alumina is 100m
2/ g, aperture is 3.5nm, and the adsorptive capacity of heavy metal chromium ion (concentration is 1mg/L) is 100mg/g.
< embodiment 2>
The invention provides a kind of preparation method of mesoporous nano-alumina, comprise the following steps:
Step one, red for the 8g of drying Pomegranate Flower joined volume is 200mL, volume percent is carry out reflux in the ethanol of 80%, obtain alcohol extract; Described alcohol extract is extracted with sherwood oil, chloroform, ethyl acetate and propyl carbinol successively, is extracted part and aqueous fraction; By described aqueous fraction after molecular sieve adsorption, be that the methyl alcohol of 100% carries out wash-out to adsorption liquid by volume percent, collect elutriant, described elutriant is joined in gac and decolours, obtain red pomegranate extracting solution; The volume ratio of described sherwood oil, chloroform, ethyl acetate and propyl carbinol is 3:6:5:2.
Step 2, take a certain amount of Tai-Ace S 150, be dissolved in described red pomegranate extracting solution, be made into the alum liquor that concentration is 0.5mol/L;
Step 3, at the temperature of the stirring velocity of 3000r/min and 40 DEG C, the ammonium hydroxide being 2mol/L by concentration is added drop-wise in alum liquor described in 200mL slowly, is 9.0, obtains Alumina gel to pH value;
Step 4, be transferred in reactor by described Alumina gel, described reactor is carried out to the burin-in process of gradient temperature, obtain alumina gel, wherein, the burin-in process of described gradient temperature is specifically divided into three temperature stage; The burin-in process of described gradient temperature is specially:
First temperature stage: temperature is 40 DEG C, stirring velocity is 400r/min, and temperature rise rate is 5 DEG C/min, and digestion time is 7h;
Second temperature stage: temperature is 60 DEG C, stirring velocity is 230r/min, and temperature rise rate is 3 DEG C/min, and digestion time is 5h;
3rd temperature stage: temperature is 80 DEG C, stirring velocity is 0r/min, and temperature rise rate is 2 DEG C/min, and digestion time is 4h.
Step 5, described alumina gel is cooled to room temperature after carry out filtration washing, the alumina gel after filtration washing is put in the baking oven of 65 DEG C and dries, by dry after alumina gel roasting 3h at 500 DEG C, namely obtain mesoporous nano-alumina.
Described filtration washing is specially:
Deionized water is heated to 50 DEG C, obtains heating rear deionized water; With deionized water after described heating, multiple times of filtration is carried out to described presoma, to remove sulfate ion, finally carry out filtration washing with ether.
The specific surface area of this mesoporous nano-alumina is 300m
2/ g, aperture is 4.5nm, and the adsorptive capacity of heavy metal chromium ion (concentration is 1mg/L) is 200mg/g.
< embodiment 3>
The invention provides a kind of preparation method of mesoporous nano-alumina, comprise the following steps:
Step one, red for the 10g of drying Pomegranate Flower joined volume is 200mL, volume percent is carry out reflux in the ethanol of 80%, obtain alcohol extract; Described alcohol extract is extracted with sherwood oil, chloroform, ethyl acetate and propyl carbinol successively, is extracted part and aqueous fraction; By described aqueous fraction after molecular sieve adsorption, be that the methyl alcohol of 100% carries out wash-out to adsorption liquid by volume percent, collect elutriant, described elutriant is joined in gac and decolours, obtain red pomegranate extracting solution; The volume ratio of described sherwood oil, chloroform, ethyl acetate and propyl carbinol is 1:1:1:1.
Step 2, take a certain amount of Tai-Ace S 150, be dissolved in described red pomegranate extracting solution, be made into the alum liquor that concentration is 0.6mol/L;
Step 3, at the temperature of the stirring velocity of 2000r/min and 30 DEG C, the ammonium hydroxide being 3mol/L by concentration is added drop-wise in alum liquor described in 200mL slowly, is 9.5, obtains Alumina gel to pH value;
Step 4, be transferred in reactor by described Alumina gel, described reactor is carried out to the burin-in process of gradient temperature, obtain alumina gel, wherein, the burin-in process of described gradient temperature is specifically divided into three temperature stage; The burin-in process of described gradient temperature is specially:
First temperature stage: temperature is 50 DEG C, stirring velocity is 500r/min, and temperature rise rate is 3 ~ 6 DEG C/min, and digestion time is 5h;
Second temperature stage: temperature is 70 DEG C, stirring velocity is 300r/min, and temperature rise rate is 2 ~ 4 DEG C/min, and digestion time is 8h;
3rd temperature stage: temperature is 90 DEG C, stirring velocity is 20r/min, and temperature rise rate is 1 ~ 3 DEG C/min, and digestion time is 5h.
Step 5, described alumina gel is cooled to room temperature after carry out filtration washing, the baking oven that the alumina gel after filtration washing is placed in 80 DEG C is dried, by dry after alumina gel roasting 3.5h at 400 DEG C, namely obtain mesoporous nano-alumina.
Described filtration washing is specially:
Deionized water is heated to 60 DEG C, obtains heating rear deionized water; With deionized water after described heating, multiple times of filtration is carried out to described presoma, to remove sulfate ion, finally carry out filtration washing with ether.
The specific surface area of this mesoporous nano-alumina is 400m
2/ g, aperture is 5.5nm, and the adsorptive capacity of heavy metal chromium ion (concentration is 1mg/L) is 300mg/g.
Although embodiment of the present invention are open as above, it is not restricted to listed in specification sheets 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.
Claims (9)
1. a preparation method for mesoporous nano-alumina, is characterized in that, comprises the following steps:
Step one, the red Pomegranate Flower of drying is joined volume percent is carry out reflux in the ethanol of 80%, obtains alcohol extract; Described alcohol extract is extracted with sherwood oil, chloroform, ethyl acetate and propyl carbinol successively, is extracted part and aqueous fraction; By described aqueous fraction after molecular sieve adsorption, be that the methyl alcohol of 100% carries out wash-out to adsorption liquid by volume percent, collect elutriant, described elutriant is joined in gac and decolours, obtain red pomegranate extracting solution;
Step 2, take a certain amount of Tai-Ace S 150, be dissolved in described red pomegranate extracting solution, be made into the alum liquor that concentration is 0.3 ~ 0.6mol/L;
Step 3, at the temperature of the stirring velocity of 1000 ~ 3000r/min and 30 ~ 40 DEG C, the ammonium hydroxide being 1 ~ 3mol/L by concentration is added drop-wise in alum liquor described in 200mL slowly, is 8.0 ~ 9.5, obtains Alumina gel to pH value;
Step 4, be transferred in reactor by described Alumina gel, described reactor is carried out to the burin-in process of gradient temperature, obtain alumina gel, wherein, the burin-in process of described gradient temperature is specifically divided into three temperature stage;
Step 5, described alumina gel is cooled to room temperature after carry out filtration washing, the baking oven that alumina gel after filtration washing is placed in 60 ~ 80 DEG C is dried, by the alumina gel roasting 2.5 ~ 3.5h at 400 ~ 1200 DEG C after oven dry, namely obtain mesoporous nano-alumina.
2. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step 4, the burin-in process of described gradient temperature is specially:
First temperature stage: temperature is 30 ~ 50 DEG C, stirring velocity is 300 ~ 500r/min, and temperature rise rate is 3 ~ 6 DEG C/min, and digestion time is 5 ~ 10h;
Second temperature stage: temperature is 50 ~ 70 DEG C, stirring velocity is 200 ~ 300r/min, and temperature rise rate is 2 ~ 4 DEG C/min, and digestion time is 4 ~ 8h;
3rd temperature stage: temperature is 70 ~ 90 DEG C, stirring velocity is 0 ~ 50r/min, and temperature rise rate is 1 ~ 3 DEG C/min, and digestion time is 3 ~ 5h.
3. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step 5, described filtration washing is specially:
Deionized water is heated to 40 ~ 60 DEG C, obtains heating rear deionized water; With deionized water after described heating, multiple times of filtration is carried out to described presoma, to remove sulfate ion, finally carry out filtration washing with ether.
4. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step one, red for 5 ~ 10g of drying Pomegranate Flower is joined volume is 150 ~ 200mL, volume percent is carry out reflux in the ethanol of 80%, obtain alcohol extract.
5. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step one, the volume ratio of described sherwood oil, chloroform, ethyl acetate and propyl carbinol is 1 ~ 3:1 ~ 6:1 ~ 5:1 ~ 2.
6. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step 3, pH value is 9.0.
7. the preparation method of mesoporous nano-alumina as claimed in claim 2, it is characterized in that, in described step 4, the burin-in process of described gradient temperature is specially:
First temperature stage: temperature is 40 DEG C, stirring velocity is 400r/min, and temperature rise rate is 5 DEG C/min, and digestion time is 7h;
Second temperature stage: temperature is 60 DEG C, stirring velocity is 230r/min, and temperature rise rate is 3 DEG C/min, and digestion time is 5h;
3rd temperature stage: temperature is 80 DEG C, stirring velocity is 0r/min, and temperature rise rate is 2 DEG C/min, and digestion time is 4h.
8. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step 2, the concentration of Tai-Ace S 150 is 0.5mol/L.
9. the preparation method of mesoporous nano-alumina as claimed in claim 1, it is characterized in that, in described step 5, described bake out temperature is 65 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110732305A (en) * | 2019-11-20 | 2020-01-31 | 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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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 |