CN110203938A - A kind of method and its application preparing multi-stage porous silicon dioxide ultrafine powder body for template based on glucan - Google Patents
A kind of method and its application preparing multi-stage porous silicon dioxide ultrafine powder body for template based on glucan Download PDFInfo
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Abstract
The invention discloses a kind of method and its application for preparing multi-stage porous silicon dioxide ultrafine powder body for template based on glucan, using silane as silicon source, using glucan or cetyl trimethylammonium bromide-glucan mixture as template, using water and ethyl alcohol as solvent, under acidic catalyst effect, polycondensation reaction is hydrolyzed at 25-80 DEG C, silica solution process is aged, is filtered, washed, drying and roasting technique process, final to obtain the porous silica superfine powder with high-ratio surface, which has preferable application prospect in gas absorption separation field.The preparation process advantage be it is low in cost, it is easy to operate, the silicon dioxide ultrafine powder body rich in micropore is made in a kind of simple, green method, has the characteristics that high-ratio surface and macropore hold and structure is adjustable.
Description
Technical field
The invention belongs to field of inorganic materials, and in particular to it is a kind of based on glucan be template high-ratio surface multi-stage porous
Silicon dioxide ultrafine powder preparation and its application.
Background technique
In recent years, porous silica powder body material is since it is with high-specific surface area, macropore appearance, good thermal stability
And the advantages that bio-compatibility, easy functionalization, porous silica powder body material is widely used as good carrier
The fields such as catalysis, separation, absorption and medicine controlled releasing.
The method of synthesis porous silica powder body material is numerous at present, and classical synthetic method is formed with surfactant
Supermolecule be template organic species and inorganic species are assembled between interface using sol-gel technology, but should
There is certain deficiency in method, conventional template agent is generally chemical petroleum product, high production cost, toxicity in the synthesis process
Greatly, raw material is non-renewable, there is serious problem of environmental pollution during the preparation process.Therefore, go deep into research, in recent years
Many researchers are that template prepares porous silica silicon powder using resourceful, renewable and inexpensive biomass polysaccharides
Material, which reduces synthesis cost, while also reducing environmental pollution.
Retuert et al. (J.Mater.Res, 2003,18:487-494) is with chitosan (Mw 1.2 × 106) it is template
Agent, silica solution are silicon source, synthesize the silicon-dioxide powdery material with meso-hole structure, but obtained mesoporous silicon dioxide powder
The specific surface area of material is lower, the method and the document the difference is that, be template with glucan, obtain high-ratio surface
Micropore-mesopore silicon dioxide ultrafine powder body material；Wang Lixia et al. (J Mater Sci (2010) 45:4470-4479) points
Not with chitosan, cetyl trimethylammonium bromide and chitosan compound are template, are prepared with micropore, micropore-Jie
The Nano particles of silicon dioxide in hole changes micropore in porous material by adjusting the concentration of chitosan concentration and ethyl orthosilicate
Content and specific surface, this method obtains the sub- specific surface area of micropore-mesoporous silicon dioxide nano particle using chitosan by template
More relatively low (300-600m2/g)；Such as Jiang Mengmeng (RCS Advances, 2016,6 (80) 76824-76828) and patent CN
(201610364720.5) dication surfactant cetyl trimethylammonium bromide (CTAB) and double dodecyls are utilized
Ditallowdimethyl ammonium bromide (DDAB) is used as structure directing agent, and beta-cyclodextrin prepares mesoporous silicon dioxide nano particle as inducer
Son changes the microstructure of mesoporous silicon oxide by adjusting the additional amount of beta-cyclodextrin；The method and document difference
It is, using glucan as template and structure directing agent, silica is adjusted by the inventory for changing glucan by changing
Pore structure.Based on current present Research, a kind of high ratio of the biological template agent that inexpensive, pollution-free, raw material is easy to get synthesis is found
Porous surface silica has certain realistic meaning and application value.
Summary of the invention
In view of the deficiencies of the prior art, it is template preparation that the purpose of the present invention is to provide one kind based on glucan
The method and its application of multi-stage porous silicon dioxide ultrafine powder body with high-specific surface area.
Technical solution of the present invention is summarized as follows:
A method of based on glucan it is that template prepares multi-stage porous silicon dioxide ultrafine powder body: using silane as silicon source,
Using glucan or glucan-CTAB mixture as template, polycondensation reaction is hydrolyzed under acidic catalyst effect, specifically
The following steps are included:
Step 1: the glucan of certain molecular weight is completely dissolved in deionized water or CTAB solution, glucan is obtained
Solution or glucan-CTAB mixed solution, i.e. template solution；
Step 2: at room temperature, addition silane and certain density hydrochloric acid solution in Xiang Shangshu template solution, 25-80 DEG C
Sustained response a few hours, obtain silica solution；
Step 3: above-mentioned silica solution is sealed, it is aged, by being filtered, washed, drying, roasting process, obtains at room temperature
The multi-stage porous silicon dioxide ultrafine powder body of high-ratio surface.
Preferably, dextran solution preparation process specifically includes in the step 1: being 2000-5000 by molecular weight
Glucan be scattered in deionized water, the dissolution of 50 DEG C of stirring in water bath；Glucan and deionized water quality ratio are (2-3): 36.
Preferably, glucan-CTAB mixed solution preparation process specifically includes in the step 1:
By by molecular weight be 2000-5000 glucan water-bath be dissolved in a certain amount of deionized water, make glucan with
Deionized water quality ratio is (0.1-1.8): 20；
Deionized water and dehydrated alcohol are mixed by the volume ratio of 16:15, then cetyl trimethylammonium bromide is dispersed in
In mixed liquor, 30 DEG C of stirring in water bath dissolutions；
Then dissolved dextran solution is slowly dropped in cetyl trimethylammonium bromide solution, stirs 10-
30min；Glucan, cetyl trimethylammonium bromide, deionized water mass ratio be (0.1-1.8): (1-2.4): 36.
Preferably, the step 2 specifically includes: silane being dissolved into dehydrated alcohol, step 1 institute is slowly dropped to
It obtains in template solution, is added with stirring 0.5-1mol/LHCl solution, 25-80 DEG C of sustained response 2-10h obtains silica solution；
The volume ratio of deionized water is 3:10:0.018:12 in silane, dehydrated alcohol, HCl and template solution.
Preferably, the silane includes at least ethyl orthosilicate, methyl orthosilicate, methyl triethylsilane and propyl three
One of Ethoxysilane.
Preferably, the step 3 specifically includes:
Ageing and drying: silica solution is sealed in conical flask, is aged 24-48h at room temperature, colloidal sol is poured into culture dish
In, it is placed in 25 DEG C of convection ovens, is dried, obtain xerogel and roasted at a certain temperature；
Washing and filtering: above-mentioned xerogel being ground, with deionized water and ethyl alcohol respectively from neutrality is washed till, is filtered,
It is dry in 60 DEG C of convection ovens；
Roasting: in air atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C, 550 DEG C of constant temperature 6h from room temperature, final to obtain
Porous silicon dioxide nano particle.
Multi-stage porous silicon dioxide ultrafine powder body be applied to gas absorption with separate.
Detailed description of the invention
Fig. 1 is that the present invention is based on the processes of the preparation method for the multi-stage porous silicon dioxide ultrafine powder body that glucan is template
Figure；
Fig. 2 is the stereoscan photograph that multi-stage porous silica is synthesized in embodiment 2；
Fig. 3 is the X-ray diffractogram that multi-stage porous silica is synthesized in embodiment 4；
Fig. 4 is the CO that multi-stage porous silica is synthesized in embodiment 12Adsorption isothermal curve；
Fig. 5 is the nitrogen adsorption desorption curve and graph of pore diameter distribution that multi-stage porous silica is synthesized in embodiment 1.
Beneficial effects of the present invention:
1, the present invention is led using glucan or cetyl trimethylammonium bromide and glucan mixture as template and structure
To agent, using silane such as ethyl orthosilicate, methyl orthosilicate, methyl triethylsilane and propyl-triethoxysilicanes as silicon source,
Under acidic catalyst effect, there is height by sol-gel method, and by operating process, preparations such as washing, dry and roastings
The porous silicon dioxide nano particle of specific surface changes porous silica by adjusting the feed ratio of CTAB and glucan
Hole parameter makes its specific surface area may be up to 1000m2/g。
2, preparation method advantage of the present invention is low in cost, easy to operate, and richness is made in a kind of simple, green method
Containing the mesoporous silicon dioxide ultrafine powder body of micropore-, have the characteristics that high-ratio surface and hierarchical porous structure.
Specific embodiment
Below in conjunction with embodiment of the present invention, the concrete scheme of embodiment of the invention is carried out detailed, clear
Description, it is clear that described embodiment is a part of embodiment of the invention, rather than whole embodiments, base
In embodiment of the invention, those skilled in the art do not make institute obtained under the premise of creative labor
There are other embodiments, belongs to the scope of protection of the invention more.
As shown in Figure 1, the preparation method of the present disclosure provides a kind of multi-stage porous silica with high-ratio surface,
This method is using silane as silicon source, using glucan or glucan-CTAB mixture as template, under acidic catalyst effect into
Row hydrolysis condensation reaction, the multi-stage porous silica produced be applied to gas absorption with separate, specifically includes the following steps:
Step 1: the glucan of certain molecular weight is completely dissolved in deionized water or CTAB solution, glucan is obtained
Solution or glucan-CTAB mixed solution, i.e. template solution；
Wherein, dextran solution preparation process specifically includes: dispersing the glucan that molecular weight is 2000-5000 in
In ionized water, 50 DEG C of stirring in water bath dissolutions；Glucan and deionized water quality ratio are (2-3): 36；
Glucan-CTAB mixed solution preparation process specifically includes: by the glucan for being 2000-5000 by molecular weight
Water-bath is dissolved in a certain amount of deionized water, makes glucan and deionized water quality ratio (0.1-1.8): 20；By 16:15's
Volume ratio mixes deionized water and dehydrated alcohol, then cetyl trimethylammonium bromide is dispersed in mixed liquor, 30 DEG C of water-baths
Stirring and dissolving；Then dissolved dextran solution is slowly dropped in cetyl trimethylammonium bromide solution, stirs 10-
30min；Glucan, cetyl trimethylammonium bromide, deionized water mass ratio be (0.1-1.8): (1-2.4): 36；
Step 2: at room temperature, addition silane and certain density hydrochloric acid solution in Xiang Shangshu template solution, 25-80 DEG C
Sustained response a few hours, obtain silica solution；Specific steps are as follows:
Silane is dissolved into dehydrated alcohol, is slowly dropped in template solution obtained by step 1, is added with stirring
0.5-1mol/LHCl solution, 25-80 DEG C of sustained response 2-10h obtain silica solution；Silane, dehydrated alcohol, HCl and template are molten
The volume ratio of deionized water is 3:10:0.018:12 in liquid；The silane includes at least ethyl orthosilicate, methyl orthosilicate, first
One of base triethylsilane and propyl-triethoxysilicane；
Step 3: above-mentioned silica solution is sealed, it is aged, by being filtered, washed, drying, roasting process, obtains at room temperature
The multi-stage porous silicon dioxide ultrafine powder body of high-ratio surface；Specific steps are as follows:
Ageing and drying: silica solution is sealed in conical flask, is aged 24-48h at room temperature, colloidal sol is poured into culture dish
In, it is placed in 25 DEG C of convection ovens, is dried, obtain xerogel and roasted at a certain temperature；
Washing and filtering: above-mentioned xerogel being ground, with deionized water and ethyl alcohol respectively from neutrality is washed till, is filtered,
It is dry in 60 DEG C of convection ovens；
Roasting: in air atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C, 550 DEG C of constant temperature 6h from room temperature, final to obtain
Porous silicon dioxide nano particle.
Embodiment 1 prepares the multi-stage porous titanium dioxide of high-ratio surface using glucan as template, by silicon source of ethyl orthosilicate
Silicon superfine powder
The glucan that 2.4500g molecular weight is 2000 is weighed respectively, is dissolved into 36ml deionized water, 50 DEG C of water
Stirring and dissolving is bathed, 9.0ml ethyl orthosilicate is measured and is added in the ethanol solution of 30ml, be added drop-wise under magnetic agitation above-mentioned
In mixed liquor；It adds in the HCl solution of 54 μ l, 0.67 mol/l, 30 DEG C of reaction 6h, the sol solution formed after reaction
It is sealed in conical flask, is aged 2d at room temperature, then solution is poured into culture dish, in 25 DEG C of convection ovens after drying for 24 hours
Xerogel is obtained, gained xerogel is ground, with deionized water and ethyl alcohol respectively from neutrality is washed till, is filtered, in 60 DEG C of drums
Dry 3h in wind baking oven, by resulting dry gel powder in air atmosphere, 10 DEG C/min of temperature programming rises to 550 from room temperature
DEG C, 550 DEG C of constant temperature 6h are final to obtain porous silica superfine powder, and gained silicon dioxide ultrafine powder surface area per unit volume product is
401m2/g。
Embodiment 2 prepares high-ratio surface as template, by silicon source of ethyl orthosilicate using glucan-CTAB mixture
Multi-stage porous silicon dioxide ultrafine powder body
The glucan that the CTAB and 0.1584g molecular weight of 2.0400g is 2000 is weighed respectively, and CTAB is placed in three-necked flask
In, with the water and 15ml dehydrated alcohol of 16ml, 30 DEG C of stirring in water bath dissolutions dissolve glucan with the deionized water water-bath of 20ml,
Dissolved dextran solution is added drop-wise in CTAB solution, mixed solution is formed；9.0ml ethyl orthosilicate is measured to be added to
In the ethanol solution of 30ml, it is added drop-wise under magnetic agitation in above-mentioned mixed liquor；Add the HCl solution of 54 μ l 0.67mol/l
In, 30 DEG C of reaction 6h, the sol solution formed after reaction is sealed in conical flask, is aged 2d at room temperature, then by solution
It pours into culture dish, drying obtains xerogel afterwards for 24 hours in 25 DEG C of convection ovens, and gained xerogel is ground, deionized water is used
It with ethyl alcohol respectively from neutrality is washed till, is filtered, the dry 3h in 60 DEG C of convection ovens, by resulting dry gel powder in air
In atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C, 550 DEG C of constant temperature 6h from room temperature, and the final multi-stage porous silica that obtains surpasses
Fine powder, specific surface area 810m2/g。
Embodiment 3 prepares high-ratio surface as template, by silicon source of methyl orthosilicate using glucan-CTAB mixture
Multi-stage porous silicon dioxide ultrafine powder body
The glucan that the CTAB and 0.7954g molecular weight of 1.4500g is 2000 is weighed respectively, and CTAB is placed in three-necked flask
In, with the water and 15ml dehydrated alcohol of 16ml, the glucan deionization water-bath of 20ml is dissolved in 30 DEG C of stirring in water bath dissolutions,
Dissolved dextran solution is added drop-wise in CTAB solution, mixed solution is formed；9.0ml methyl orthosilicate is measured to be added to
In the ethanol solution of 30ml, it is added drop-wise under magnetic agitation in above-mentioned mixed liquor；Add the HCl solution of 54 μ l 0.67mol/l
In, 30 DEG C of reaction 6h, the sol solution formed after reaction is sealed in conical flask, is aged 2d at room temperature, then by solution
It pours into culture dish, drying obtains xerogel afterwards for 24 hours in 25 DEG C of convection ovens, and gained xerogel is ground, deionized water is used
It with ethyl alcohol respectively from neutrality is washed till, is filtered, the dry 3h in 60 DEG C of convection ovens, by resulting dry gel powder in air
In atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C, 550 DEG C of constant temperature 6h from room temperature, and final acquisition porous silica is ultra-fine
Powder, gained silica nanometer superfine powder specific surface area are 1017m2/g。
Embodiment 4 using glucan-CTAB mixture as template, by silicon source of methyl triethylsilane prepare Gao Bibiao
The multi-stage porous silicon dioxide ultrafine powder body in face
The glucan that the CTAB and 0.6500g molecular weight of 1.8000g is 2000 is weighed respectively, and CTAB is placed in three-necked flask
In, with the water and 15ml dehydrated alcohol of 16ml, the glucan deionization water-bath of 20ml is dissolved in 30 DEG C of stirring in water bath dissolutions,
Dissolved dextran solution is added drop-wise in CTAB solution, mixed solution is formed；9.0ml methyl triethylsilane is measured to be added
To in the ethanol solution of 30ml, it is added drop-wise under magnetic agitation in above-mentioned mixed liquor；The HCl for adding 54 μ l 0.67mol/l is molten
In liquid, 30 DEG C of reaction 6h, the sol solution formed after reaction is sealed in conical flask, is aged 2d at room temperature, then will be molten
Liquid pours into culture dish, and drying obtains xerogel afterwards for 24 hours in 25 DEG C of convection ovens, and gained xerogel is ground, deionization is used
Water and ethyl alcohol are filtered respectively from neutrality is washed till, the dry 3h in 60 DEG C of convection ovens, by resulting dry gel powder in sky
In gas atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C, 550 DEG C of constant temperature 6h from room temperature, and the final porous silica that obtains surpasses
Fine powder, gained Nano particles of silicon dioxide superfine powder specific surface area are 1098m2/g。
Embodiment 5 prepares high ratio as template, by silicon source of propyl-triethoxysilicane using glucan-CTAB mixture
The multi-stage porous silicon dioxide ultrafine powder body on surface
The glucan that the CTAB and 0.8500g molecular weight of 1.7000g is 2000 is weighed respectively, and CTAB is placed in three-necked flask
In, with the water and 15ml dehydrated alcohol of 16ml, the glucan deionization water-bath of 20ml is dissolved in 30 DEG C of stirring in water bath dissolutions,
Dissolved dextran solution is added drop-wise in CTAB solution, mixed solution is formed；9.0ml propyl-triethoxysilicane is measured to add
Enter in the ethanol solution of 30ml, is added drop-wise under magnetic agitation in above-mentioned mixed liquor；Add the HCl of 54 μ l 0.67mol/l
In solution, 30 DEG C of reaction 6h, the sol solution formed after reaction is sealed in conical flask, is aged 2d at room temperature, then will
Solution pours into culture dish, in 25 DEG C of convection ovens drying obtain xerogel afterwards for 24 hours, gained xerogel is ground, spend from
Sub- water and ethyl alcohol are filtered respectively from neutrality is washed till, and dry 3h, resulting dry gel powder is existed in 60 DEG C of convection ovens
In air atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C from room temperature, and 550 DEG C of constant temperature 6h finally obtain porous silica
Superfine powder, gained silicon dioxide ultrafine powder body, specific surface area 1082m2/g。
Analysis of experiments is carried out to the multi-stage porous silica that above-described embodiment is produced:
The three-dimensional appearance for the multi-stage porous silica that embodiment 2 is produced is observed with scanning electron microscope, and shoots photo,
Fig. 2 is the stereoscan photograph of the multi-stage porous silica.
The multi-stage porous silica produced with X ray diffracting spectrum characterization embodiment 4, Fig. 3 are the multi-stage porous silica
X-ray diffractogram.
CO is made to the multi-stage porous silica that embodiment 1 is produced2Gas absorption test, Fig. 4 are the multi-stage porous silica
CO2Adsorption isothermal curve, test method are as follows:
CO2Gas absorption measures room temperature carbon dioxide gas using the full-automatic specific surface area of precise and tiny Gao Bo and pore analysis instrument
The adsorbance of body, specific steps are as follows: 100mg multi-stage porous silicon-dioxide powdery is added in sample cell, and is pre-processed, is taken out
After 180 DEG C of 8h of heating in vacuum, it is cooled to room temperature.
Nitrogen adsorption desorption test is made to the multi-stage porous silica that embodiment 1 is produced, and observes its pore-size distribution situation,
Fig. 5 is the nitrogen adsorption desorption curve and graph of pore diameter distribution of the multi-stage porous silica.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (7)
1. a kind of method for preparing multi-stage porous silicon dioxide ultrafine powder body based on glucan for template, it is characterised in that: with silicon
Alkane is silicon source, and using glucan or glucan-CTAB mixture as template, polycondensation is hydrolyzed under acidic catalyst effect
Reaction, specifically includes the following steps:
Step 1: the glucan of certain molecular weight is completely dissolved in deionized water or CTAB solution, dextran solution is obtained
Or glucan-CTAB mixed solution, i.e. template solution；
Step 2: at room temperature, silane and certain density hydrochloric acid solution are added in Xiang Shangshu template solution, 25-80 DEG C continues
A few hours are reacted, silica solution is obtained；
Step 3: above-mentioned silica solution is sealed, it is aged at room temperature, by being filtered, washed, drying, roasting process, obtains high ratio
The multi-stage porous silicon dioxide ultrafine powder body on surface.
2. a kind of side for preparing multi-stage porous silicon dioxide ultrafine powder body for template based on glucan according to claim 1
Method, it is characterised in that: dextran solution preparation process specifically includes in the step 1: the Portugal for being 2000-5000 by molecular weight
Glycan is scattered in deionized water, 50 DEG C of stirring in water bath dissolutions；Glucan and deionized water quality ratio are (2-3): 36.
3. a kind of side for preparing multi-stage porous silicon dioxide ultrafine powder body for template based on glucan according to claim 1
Method, it is characterised in that: glucan-CTAB mixed solution preparation process specifically includes in the step 1:
By by molecular weight be 2000-5000 glucan water-bath be dissolved in a certain amount of deionized water, make glucan and go from
Sub- water quality ratio is (0.1-1.8): 20；
Deionized water and dehydrated alcohol are mixed by the volume ratio of 16:15, then cetyl trimethylammonium bromide is dispersed in mixing
In liquid, 30 DEG C of stirring in water bath dissolutions；
Then dissolved dextran solution is slowly dropped in cetyl trimethylammonium bromide solution, stirs 10-
30min；Glucan, cetyl trimethylammonium bromide, deionized water mass ratio be (0.1-1.8): (1-2.4): 36.
4. requiring the preparation method of the multi-stage porous silicon dioxide ultrafine powder body according to right 1, it is characterised in that: the step 2
It specifically includes: silane is dissolved into dehydrated alcohol, be slowly dropped in template solution obtained by step 1, be added with stirring
0.5-1mol/LHCl solution, 25-80 DEG C of sustained response 2-10h obtain silica solution；Silane, dehydrated alcohol, HCl and template are molten
The volume ratio of deionized water is 3:10:0.018:12 in liquid.
5. according to claim 1 or 4 any described one kind are based on glucan and prepare multi-stage porous silicon dioxide ultrafine powder for template
The method of body, it is characterised in that: the silane includes at least ethyl orthosilicate, methyl orthosilicate, methyl triethylsilane and third
One of ethyl triethoxy silicane alkane.
6. requiring the preparation method of the multi-stage porous silicon dioxide ultrafine powder body according to right 1, it is characterised in that: the step 3
It specifically includes:
Ageing and drying: silica solution is sealed in conical flask, is aged 24-48h at room temperature, colloidal sol is poured into culture dish, is put
It in 25 DEG C of convection ovens, is dried, obtains xerogel and roasted at a certain temperature；
Washing and filtering: above-mentioned xerogel is ground, with deionized water and ethyl alcohol respectively from neutrality is washed till, is filtered, 60
It is dry in DEG C convection oven；
Roasting: in air atmosphere, 10 DEG C/min of temperature programming rises to 550 DEG C from room temperature, and 550 DEG C of constant temperature 6h are finally obtained porous
Nano particles of silicon dioxide.
7. as any described multi-stage porous silicon dioxide ultrafine powder body such as claim 1-6 applied to gas absorption with separate.
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