CN109701484A - A kind of preparation method of aluminium doped silicon dioxide composite adsorbing material - Google Patents
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Abstract
The invention discloses a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material, by using preparing SiO respectively2Colloidal sol, Al2O3Colloidal sol, then by SiO2Colloidal sol and Al2O3Colloidal sol mixing drying, roasts, grind into powder at a certain temperature, obtains aluminium doping type SiO2Composite adsorbing material, by SiO2Material introduces the aluminium with suction-operated, can improve SiO2The adsorption capacity of material, and improve SiO2The adsorption efficiency of material, the preparation method is simple, there is good practicability.
Description
Technical field
The invention belongs to adsorbent material technical fields, and in particular to a kind of aluminium doped silicon dioxide composite adsorbing material
Preparation method.
Background technique
Currently, freshwater resources are increasingly in short supply, and according to statistics, there is the water shortage of more than 100 country's various degrees in the whole world
Problem, wherein there is 28 countries to be listed in water shortage state or serious water shortage state.China water resource occupancy volume per person is 2200m3, only
The 1/4 of world average level is poorest one of the country of global per capita water resource.In China while shortage of fresh water,
Water pollution is also constantly aggravating.Wherein waste water from dyestuff due to coloration it is higher, complicated component, it has also become industrial wastewater it is important come
One of source.It is counted according to dyestuff Industry in China association, the dyestuff annual output position in China is at the forefront in the world.During DYE PRODUCTION,
One ton of dyestuff of every production, with the product of waste water loss 2%, and loss amount is bigger in dyeing process, not only causes resource
Significant wastage also causes seriously to pollute to water body and environment, affects the production and living of the mankind.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material, solve existing
There is SiO2The lower problem of the adsorption efficiency and adsorption capacity of material.
The technical scheme adopted by the invention is that a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material,
It is specifically implemented according to the following steps:
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.05~0.15ml/s, is stirred at a certain temperature
It mixes uniformly, obtains homogeneous phase solution；Take certain density HNO3Solution and water, by mixed solution with 0.05~0.15ml/s's
Above-mentioned homogeneous phase solution is added in rate, stirs evenly, after a period of time of flowing back after be cooled to room temperature, obtain SiO2 colloidal sol；
Step 2, pure water is heated to 75~85 DEG C, aluminium isopropoxide is added in above-mentioned pure water and stirs 1~3h, to isopropyl
After being fully hydrolyzed with the rate of 0.05~0.15ml/s HNO is added in aluminium alcoholates3, stir evenly, at a certain temperature flow back one section when
Between, it is cooled to room temperature, obtains the Al of stable transparent2O3Colloidal sol；
Step 3, it is Al:TEOS=0~2:1 according to molar ratio, is made step 2 with the drop rate of 0.05~0.15ml/s
The Al got ready2O3SiO prepared by step 1 is added in colloidal sol2To get Al in colloidal sol2O3/SiO2Adsorb colloidal sol；
Step 4, Al step 3 obtained2O3/SiO2Absorption colloidal sol is dried in vacuo a period of time at low temperature, in air or
It roasts in person's nitrogen atmosphere, is cooled to room temperature after roasting, be ground into powder, the aluminium doping type SiO as prepared2Compound suction
Enclosure material.
The characteristics of of the invention, also resides in,
Mixing time is 0.5~1.5h in step 1, and temperature range is 0~30 DEG C, HNO3The concentration of solution be 1.0~
4.0mol/L, reflux temperature are 50~75 DEG C, and return time is 2~4h.
Ethyl orthosilicate in step 1, dehydrated alcohol, water, nitric acid molar ratio be 1:4.2~7.0:4.0~9.0:0.03
~0.12.
HNO is added in step 23Concentration be 1.0~4.0mol/L, temperature range be 80 DEG C~90 DEG C, return time 7
~9h.
Heating device in step 2 is heat collecting type constant temperature blender with magnetic force.
Aluminium isopropoxide in step 2, water, nitric acid molar ratio be 1:80~160:0.15~0.45.
Whipping temp is 10~45 DEG C in step 3, and mixing time is 0.5~1.0h.
In step 4 vacuum drying time be 3~6 days, maturing temperature be 350~800 DEG C, roasting rate be 0.5~5 DEG C/
Min, calcining time are 2~5h, and cooling rate is 1~10 DEG C/min.
The diameter of particle ground in step 4 is 1~20nm.
The invention has the advantages that aluminium doping type SiO of the present invention2The preparation method of composite adsorbing material, improves SiO2
Material reduces costs the adsorption capacity and adsorption efficiency of Wastewater Dyes, and the preparation method is simple, there is good reality
With value.
Detailed description of the invention
Fig. 1 is aluminium doping type SiO prepared by the present invention2Composite adsorbing material (B) and SiO2Absorption of the material (A) to dyestuff
Capacity comparison figure；
Fig. 2 is aluminium doping type SiO prepared by the present invention2Composite adsorbing material (B) and SiO2Material (A) imitates Dye Adsorption
Rate comparison diagram.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of aluminium doped silicon dioxide composite adsorbing material of the present invention, it is specifically real according to the following steps
It applies:
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.05~0.15ml/s, is stirred using constant temperature magnetic force
It mixes device and stirs 0.5~1.5h, temperature range is 0~30 DEG C, obtains homogeneous phase solution, and taking concentration is 1.0~4.0mol/L's
HNO3Solution and pure water mixing, are added dropwise to above-mentioned homogeneous phase solution for mixed solution using constant pressure funnel, drop rate is
0.05~0.15ml/s is stirred evenly, and is cooled to room temperature after the 2~4h that flows back at a temperature of 50~75 DEG C, is obtained SiO2Colloidal sol.
Wherein, the molar ratio of ethyl orthosilicate (TEOS), dehydrated alcohol (ETOH), water, nitric acid are as follows: 1:4.2~7.0:4.0
~9.0:0.03~0.12.
Step 2, pure water is heated to 75~85 DEG C using heat collecting type constant temperature blender with magnetic force, aluminium isopropoxide is added to the water
And 1~3h is stirred, the HNO for being 1.0~4.0mol/L by concentration with constant pressure funnel after being fully hydrolyzed3After solution is added dropwise to reaction
In system, drop rate is 0.05~0.15ml/s, is stirred at reflux 7~9h at a temperature of 80 DEG C~90 DEG C, is cooled to room temperature, i.e.,
Obtain the Al of stable transparent2O3Colloidal sol.
Wherein, the molar ratio of aluminium isopropoxide (AIP), water, nitric acid are as follows: 1:80~160:0.15~0.45.
Step 3, it according to molar ratio Al:TEOS=0~2:1, with the drop rate of 0.05~0.15ml/s prepared by step 2
Good Al2O3SiO prepared by step 1 is added in colloidal sol2In colloidal sol, 0.5~1.0h is stirred at 10~45 DEG C to get Al2O3/
SiO2Adsorb colloidal sol.
Step 4, Al step 3 prepared2O3/SiO2It adsorbs colloidal sol to be dried in vacuo 3~6 days, then in air or nitrogen
In gas atmosphere, 350~800 DEG C are warming up to the speed of 0.5~5 DEG C/min, roasts 2~5h, then with the speed of 1~10 DEG C/min
It is cooled to room temperature to obtain free-standing film material, being ground into partial size is 1~20nm powder up to aluminium doping type SiO2Compound suction
Enclosure material.
The aluminium doping type SiO of the method for the present invention preparation2Composite adsorbing material improves SiO2Material is to Wastewater Dyes
Adsorption capacity and adsorption efficiency, reduce costs, and have good practical value.
As shown in Figure 1, being aluminium doping type SiO prepared by the present invention2Composite adsorbing material (B) and SiO2Material (A) is to dyestuff
Adsorption capacity comparison diagram.SiO2Material reactant ethyl orthosilicate, dehydrated alcohol, water, nitric acid molar ratio be 1:5.5:6.0:
0.08, it will be seen from figure 1 that SiO2The adsorption capacity of material (A) is 9.275mg/g, and aluminium adulterates SiO2Composite adsorbing material (B)
Adsorption capacity be 21mg/g, in contrast, aluminium doping type SiO prepared by the present invention2The adsorption capacity of composite adsorbing material mentions
High 11.725mg/g.
As shown in Fig. 2, being aluminium doping type SiO prepared by the present invention2Composite adsorbing material (B) and SiO2Material (A) is to dyestuff
Adsorption efficiency comparison diagram.Figure it is seen that SiO2The adsorption efficiency of material (A) is 37.1%, and aluminium adulterates SiO2Composite adsorption
The adsorption efficiency of material (B) is 84%, in contrast, aluminium doping type SiO prepared by the present invention2The absorption of composite adsorbing material is imitated
Rate improves 46.9%.
Embodiment 1
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.05ml/s, utilizes constant-temperature magnetic stirring device
0.5h is stirred, temperature is 30 DEG C, obtains homogeneous phase solution, and then taking concentration is the HNO of 1.0mol/L3Solution and pure water mixing, benefit
Mixed solution is added dropwise to above-mentioned homogeneous phase solution with constant pressure funnel, drop rate 0.05ml/s is stirred evenly, at 50 DEG C
At a temperature of be stirred at reflux 2h after be cooled to room temperature, obtain SiO2Colloidal sol.
Wherein, the molar ratio of ethyl orthosilicate (TEOS), dehydrated alcohol (ETOH), water, nitric acid are as follows: 1:4.2:4.0:
0.03。
Step 2, pure water is heated to 75 DEG C using heat collecting type constant temperature blender with magnetic force, aluminium isopropoxide is added to the water and is stirred
1h is mixed, the HNO for being 1.0mol/L by concentration with constant pressure funnel after being fully hydrolyzed3Solution is added in the system after reaction, and speed is added dropwise
Rate is 0.05ml/s, is stirred at reflux 9h at a temperature of 80 DEG C, obtains the Al of stable transparent2O3Colloidal sol.
Wherein, the molar ratio of aluminium isopropoxide (AIP), water, nitric acid are as follows: 1:80:0.15.
Step 3, step 2 is prepared according to molar ratio Al:TEOS=0.4:1, with the drop rate of 0.05ml/s
Al2O3SiO prepared by step 1 is added in colloidal sol2In colloidal sol, 0.5h is stirred at 15 DEG C to get Al2O3/SiO2Adsorb colloidal sol.
Step 4, Al step 3 obtained2O3/SiO2Colloidal sol is adsorbed to be dried in vacuo 3 days, then in air atmosphere, with
0.5 DEG C/min is warming up to 350 DEG C, roasts 2 hours, then be cooled to room temperature to obtain free-standing film material with the speed of 1 DEG C/min, will
It is 1~20nm powder up to aluminium doping type SiO that it, which is ground into partial size,2Composite adsorbing material.
Embodiment 2
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.08ml/s, utilizes constant-temperature magnetic stirring device
1h is stirred, temperature is 24 DEG C, obtains homogeneous phase solution, and taking concentration is the HNO of 2.0mol/L3Solution and pure water mixing, utilize constant pressure
Mixed solution is added dropwise to above-mentioned homogeneous phase solution by funnel, and drop rate 0.08ml/s is stirred evenly, at a temperature of 60 DEG C
It is cooled to room temperature after being stirred at reflux 3h, obtains SiO2Colloidal sol.
Wherein, the molar ratio of ethyl orthosilicate (TEOS), dehydrated alcohol (ETOH), water, nitric acid are as follows: 1:4.5:5.0:
0.06。
Step 2, pure water is heated to 80 DEG C using heat collecting type constant temperature blender with magnetic force, aluminium isopropoxide is added to the water and is stirred
1.5h is mixed, the HNO for being 2.0mol/L by concentration with constant pressure funnel after being fully hydrolyzed3Solution is added in the system after reaction, is added dropwise
Rate is 0.08ml/s, is stirred at reflux 9h at a temperature of 85 DEG C, obtains the Al of stable transparent2O3Colloidal sol.
Wherein, the molar ratio of aluminium isopropoxide (AIP), water, nitric acid are as follows: 1:100:0.23.
Step 3, step 2 is prepared according to molar ratio Al:TEOS=0.8:1, with the drop rate of 0.08ml/s
Al2O3SiO prepared by step 1 is added in colloidal sol2In colloidal sol, 45min is stirred at 25 DEG C to get Al2O3/SiO2Adsorb colloidal sol.
Step 4, Al step 3 prepared2O3/SiO2Colloidal sol is adsorbed to be dried in vacuo 4 days, then in nitrogen atmosphere, with
2 DEG C/min is warming up to 400 DEG C, roasts 3 hours, then be cooled to room temperature to obtain free-standing film material with the speed of 3 DEG C/min, by it
Being ground into partial size is 1~20nm powder up to aluminium doping type SiO2Composite adsorbing material.
Embodiment 3
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.08ml/s, utilizes constant-temperature magnetic stirring device
50min is stirred, temperature is 18 DEG C, obtains homogeneous phase solution, and then taking concentration is the HNO of 3.0mol/L3Solution and pure water mixing, benefit
Mixed solution is added dropwise to above-mentioned homogeneous phase solution with constant pressure funnel, drop rate 0.08ml/s is stirred evenly, at 65 DEG C
At a temperature of be stirred at reflux 3.5h after be cooled to room temperature, obtain SiO2Colloidal sol.
Wherein, the molar ratio of ethyl orthosilicate (TEOS), dehydrated alcohol (ETOH), water, nitric acid are as follows: 1:5.5:6.0:
0.08。
Step 2, pure water is heated to 80 DEG C using heat collecting type constant temperature blender with magnetic force, aluminium isopropoxide is added to the water and is stirred
2h is mixed, the HNO for being 3.0mol/L by concentration with constant pressure funnel after being fully hydrolyzed3Solution is added in the system after reaction, and speed is added dropwise
Rate is 0.08ml/s, is stirred at reflux 8h at a temperature of 85 DEG C, obtains the Al of stable transparent2O3Colloidal sol.
Wherein, the molar ratio of aluminium isopropoxide (AIP), water, nitric acid are as follows: 1:120:0.30.
Step 3, step 2 is prepared according to molar ratio Al:TEOS=1.2:1, with the drop rate of 0.08ml/s
Al2O3SiO prepared by step 1 is added in colloidal sol2In colloidal sol, 45min is stirred at 30 DEG C to get Al2O3/SiO2Adsorb colloidal sol.
Step 4, Al step 3 prepared2O3/SiO2Colloidal sol is adsorbed to be dried in vacuo 5 days, then in air atmosphere,
500 DEG C are warming up to 3 DEG C/min, is roasted 3.5 hours, then be cooled to room temperature to obtain free-standing film material with the speed of 6 DEG C/min,
Being ground into partial size is 1~20nm powder up to aluminium doping type SiO2Composite adsorbing material.
Embodiment 4
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.12ml/s, utilizes constant-temperature magnetic stirring device
1h is stirred, temperature is 12 DEG C, obtains homogeneous phase solution, and then taking concentration is the HNO of 3.5mol/L3Solution and pure water mixing, utilize
Mixed solution is added dropwise to above-mentioned homogeneous phase solution by constant pressure funnel, and drop rate 0.12ml/s is stirred evenly, in 70 DEG C of temperature
It is cooled to room temperature after being stirred at reflux 4.5h under degree, obtains SiO2Colloidal sol.
Wherein, the molar ratio of ethyl orthosilicate (TEOS), dehydrated alcohol (ETOH), water, nitric acid are as follows: 1:6.2:7.0:
0.10。
Step 2, pure water is heated to 85 DEG C using heat collecting type constant temperature blender with magnetic force, aluminium isopropoxide is added to the water and is stirred
2.5h is mixed, the HNO for being 3.5mol/L by concentration with constant pressure funnel after being fully hydrolyzed3Solution is added in the system after reaction, is added dropwise
Rate is 0.12ml/s, is stirred at reflux 8h at a temperature of 85 DEG C, obtains the Al of stable transparent2O3Colloidal sol.
Wherein, the molar ratio of aluminium isopropoxide (AIP), water, nitric acid are as follows: 1:140:0.38.
Step 3, step 2 is prepared according to molar ratio Al:TEOS=1.6:1, with the drop rate of 0.12ml/s
Al2O3SiO prepared by step 1 is added in colloidal sol2In colloidal sol, 0.5h is stirred at 15 DEG C to get Al2O3/SiO2Adsorb colloidal sol.
Step 4, Al step 3 prepared2O3/SiO2Colloidal sol is adsorbed to be dried in vacuo 6 days, then in nitrogen atmosphere, with
4 DEG C/min is warming up to 700 DEG C, roasts 4 hours, then be cooled to room temperature to obtain free-standing film material with the speed of 8 DEG C/min, by it
Being ground into partial size is 1~20nm powder up to aluminium doping type SIO2 composite adsorbing material.
Embodiment 5
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.15ml/s, utilizes constant-temperature magnetic stirring device
1.5h is stirred, temperature is 6 DEG C, obtains homogeneous phase solution, and then taking concentration is the HNO of 4.0mol/L3Solution and pure water mixing, utilize
Mixed solution is added dropwise to above-mentioned homogeneous phase solution by constant pressure funnel, and drop rate 0.15ml/s is stirred at a temperature of 75 DEG C
It is cooled to room temperature after reflux 5h, obtains SiO2Colloidal sol.
Wherein, the molar ratio of ethyl orthosilicate (TEOS), dehydrated alcohol (ETOH), water, nitric acid are as follows: 1:7.0:9.0:
0.12。
Step 2, pure water is heated to 85 DEG C using heat collecting type constant temperature blender with magnetic force, load weighted aluminium isopropoxide is added
In water and 3h is stirred, the HNO for being 4.0mol/L by concentration with constant pressure funnel after being fully hydrolyzed3The system after reaction is added in solution
In, drop rate 0.15ml/s is stirred at reflux 9h at a temperature of 90 DEG C, obtains the Al of stable transparent2O3Colloidal sol.
Wherein, the molar ratio of aluminium isopropoxide (AIP), water, nitric acid are as follows: 1:160:0.45.
Step 3, step 2 is prepared according to molar ratio Al:TEOS=2:1, with the drop rate of 0.15ml/s
Al2O3SiO prepared by step 1 is added in colloidal sol2In colloidal sol, 1h is stirred at 45 DEG C to get Al2O3/SiO2Adsorb colloidal sol.
Step 4, Al step 3 prepared2O3/SiO2Colloidal sol is adsorbed to be dried in vacuo 6 days, then in air atmosphere, with
5 DEG C/min is warming up to 800 DEG C, roasts 5h, then be cooled to room temperature to obtain free-standing film material with the speed of 10 DEG C/min, is ground
Wearing into partial size is 1~20nm powder up to aluminium doping type SiO2Composite adsorbing material.
Claims (9)
1. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material, which is characterized in that specifically according to the following steps
Implement:
Step 1, ethyl orthosilicate is added to absolute ethanol with the rate of 0.05~0.15ml/s, stirring is equal at a certain temperature
It is even, obtain homogeneous phase solution；Take certain density HNO3Solution and water, by mixed solution with the rate of 0.05~0.15ml/s
Above-mentioned homogeneous phase solution is added, stirs evenly, flow back a period of time after after be cooled to room temperature, obtain SiO2Colloidal sol；
Step 2, pure water is heated to 75~85 DEG C, aluminium isopropoxide is added in above-mentioned pure water and stirs 1~3h, to aluminium isopropoxide
HNO is added with the rate of 0.05~0.15ml/s after being fully hydrolyzed3, stir evenly, reflux a period of time, cold at a certain temperature
But to room temperature, the Al of stable transparent is obtained2O3Colloidal sol；
Step 3, it is Al:TEOS=0~2:1 according to molar ratio, is prepared step 2 with the drop rate of 0.05~0.15ml/s
Al2O3SiO prepared by step 1 is added in colloidal sol2To get Al in colloidal sol2O3/SiO2Adsorb colloidal sol；
Step 4, Al step 3 obtained2O3/SiO2Absorption colloidal sol is dried in vacuo a period of time at low temperature, in air or nitrogen
It roasts in gas atmosphere, is cooled to room temperature after roasting, be ground into powder, the aluminium doping type SiO as prepared2Composite adsorption material
Material.
2. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as described in claim 1, which is characterized in that
Mixing time is 0.5~1.5h in the step 1, and temperature range is 0~30 DEG C, HNO3The concentration of solution is 1.0~4.0mol/
L, reflux temperature are 50~75 DEG C, and return time is 2~4h.
3. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as claimed in claim 2, which is characterized in that
The molar ratio of ethyl orthosilicate, dehydrated alcohol, water, nitric acid in the step 1 are as follows: 1:4.2~7.0:4.0~9.0:0.03~
0.12。
4. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as described in claim 1, which is characterized in that
HNO is added in the step 23Concentration be 1.0~4.0mol/L, temperature range be 80 DEG C~90 DEG C, return time be 7~
9h。
5. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as claimed in claim 4, which is characterized in that
Heating device in the step 2 is heat collecting type constant temperature blender with magnetic force.
6. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as described in claim 4 or 5, feature exist
In the molar ratio of aluminium isopropoxide, water, nitric acid in the step 2 are as follows: 1:80~160:0.15~0.45.
7. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as described in claim 1, which is characterized in that
Whipping temp is 10~45 DEG C in the step 3, and mixing time is 0.5~1.0h.
8. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as described in claim 1, which is characterized in that
Vacuum drying time is 3~6 days in the step 4, and maturing temperature is 350~800 DEG C, and roasting rate is 0.5~5 DEG C/min,
Calcining time is 2~5h, and cooling rate is 1~10 DEG C/min.
9. a kind of preparation method of aluminium doped silicon dioxide composite adsorbing material as described in claim 1, which is characterized in that
The diameter of particle ground in the step 4 is 1~20nm.
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