CN105152172A - Modified diatomite with multistage-pore structure and preparation method therefor - Google Patents
Modified diatomite with multistage-pore structure and preparation method therefor Download PDFInfo
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- CN105152172A CN105152172A CN201510451723.8A CN201510451723A CN105152172A CN 105152172 A CN105152172 A CN 105152172A CN 201510451723 A CN201510451723 A CN 201510451723A CN 105152172 A CN105152172 A CN 105152172A
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Abstract
The invention provides modified diatomite with a multistage-pore structure and a preparation method therefor. According to the method, pore passages of diatomite are modified, mesoporous and microporous structures are added into the original macroporous structure of the diatomite, and multistage-pore materials with microporous and mesoporous combination or mesoporous and macroporous combination or microporous and macroporous combination can be obtained specifically. According to the modified diatomite with the multistage-pore structure and the preparation method therefor, the preparation of the multistage-pore materials is realized, and the preparation method is quick and convenient in operation and low in cost.
Description
Technical field
The invention belongs to diatomite technical field of inorganic material, be specifically related to a kind of modification infusorial earth with hierarchical porous structure, still further provides the preparation method of modification infusorial earth simultaneously.
Technical background
Diatomite is a kind of siliceous organism sedimentogeneous rock formed by diatom, and main component is the amorphous Si O of porous
2, and containing a small amount of Fe
2o
3, CaO, MgO, Al
2o
3and organic impurity.The maximum feature of diatomite material has vesicular structure, and proportion is little.Industrial being commonly used to, as flocculating aids, lagging material, filler etc., has a wide range of applications at numerous areas such as filtration, resin, coating, coating, building materials, medicine.Diatomaceous pore distribution is single, and pore diameter range, at more than 500nm, belongs to large pore material substantially.Its pore structure has certain change with diatom kind difference, but substantially belongs to mutually through three-dimensional open-framework.Because diatomaceous pore passage structure is single, it is when as materials such as absorption, noise elimination noise abatements, and the scope that its performance regulates and controls further is less.
The hole dimension of porous material and pore passage structure have conclusive impact to its performance, can be roughly divided into micropore (being less than 2nm), mesoporous (2-50nm) and macropore (being greater than 50nm) three class according to its aperture.In actual applications, the aperture regulating and controlling porous material targetedly can be optimized material property.In recent years, the porous material that development has multistage aperture and pore passage structure causes people more and more to pay attention to, such as there is the multi-stage porous molecular screen material of micropore and meso-hole structure simultaneously, there is more excellent then shape catalytic performance and mass transfer ability, have important application potentiality in fields such as heavy oit pyrolysises.Diatomite is as a kind of natural porous material of rich reserves, if carry out modification by suitable modification technology to its pore size and structure, construct multi-stage artery structure, it can be used as a kind of novel multilevel hole material, must prior using value be played.
Summary of the invention
Object of the present invention is just to provide a kind of modification infusorial earth with hierarchical porous structure and preparation method thereof, by carrying out modification to diatomaceous duct, and obtains the modification infusorial earth material with hierarchical porous structure.
A kind of modification infusorial earth with hierarchical porous structure of the present invention, is characterized in that:
In common diatomaceous macroporous structure, add micropore and meso-hole structure, specifically can obtain and there is the multilevel hole material that micropore (aperture 2nm) and mesoporous (aperture 10nm ~ 20nm) combine or mesoporous (aperture 10nm ~ 20nm) and macropore (aperture 50nm ~ 200nm) combination or micropore (aperture 2nm) and macropore (aperture 50nm ~ 200nm) combine.
A kind of preparation method with the modification infusorial earth of hierarchical porous structure of the present invention, comprises the following steps:
1) get diatomite original soil 1kg and to be immersed in 1-2M hydrochloric acid soln 1 hour, diatomite original soil after pickling to be immersed in 1-2M sodium hydroxide solution 20 minutes, wash rear dry diatomite modified raw material with water;
2) get the diatomite modified raw material of step 1), ultrasonic disperse, in 10 liters of dehydrated alcohols, adds silicon source precursor, template, catalyzer and water, 25 DEG C ~ 40 DEG C constant temperature stirring reactions 12 hours;
Wherein, described silicon source precursor can be draw together tetramethoxy-silicane or tetraethoxysilane any one, the mass ratio of diatomite material and silicon source precursor is within the scope of 1:2 ~ 1:10;
Described catalyzer be Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide or TBAH any one, catalyzer mass concentration is in ethanol 0.1% ~ 1%;
Described template is cetyl trimethylammonium bromide, and template mass concentration is in ethanol in 0 ~ 1% scope;
Water mass concentration is in ethanol in 1% ~ 5% scope;
3) above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in 10 premium on currency, regulates and controls solution ph between 8.5-9.0,85 DEG C ~ 95 DEG C ageings 6 hours;
4), after step (3) reaction product centrifugation, drying obtains the modification infusorial earth with hierarchical porous structure.
The modification infusorial earth of hierarchical porous structure of the present invention has 2nm microvoid structure and 50nm ~ 100nm macroporous structure after testing.
positively effect of the present invention is:by carrying out modification to diatomaceous duct, in the macroporous structure of diatomite original soil, with the addition of mesoporous and microvoid structure, obtaining the modification infusorial earth material with hierarchical porous structure, realizing the preparation of multilevel hole material; The preparation method of modification infusorial earth operates rapid and convenient, with low cost.
Embodiment
By following examples, the present invention is described further, should be understood that following examples are exemplary, instead of restrictive, according to the technical scheme of foregoing invention and practical situation, concrete implementation method can be determined.
embodiment 1
1) get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours, obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2) get the above-mentioned diatomite material of 1kg, dispersed with stirring, in the ethanol of 10 liter 10%, adds 100g tetraethoxysilane, 13g Tetramethylammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3) above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4), after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 2nm microvoid structure and the combination of 50nm ~ 100nm macroporous structure.
embodiment 2
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 100g tetraethoxysilane, 10g cetyl trimethylammonium bromide, 13g tetraethyl ammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 10nm meso-hole structure and the combination of 50nm ~ 100nm macroporous structure.
embodiment 3
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 100g tetraethoxysilane, 10g cetyl trimethylammonium bromide, 13g TBAH and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 10nm meso-hole structure and the combination of 50nm ~ 100nm macroporous structure.
embodiment 4
1) get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours, obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2) get the above-mentioned diatomite material of 1kg, dispersed with stirring, in the ethanol of 10 liter 10%, adds 100g tetraethoxysilane, 13g tetraethyl ammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3) above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4), after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 2nm microvoid structure and the combination of 50nm ~ 100nm macroporous structure.
embodiment 5
1) get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours, obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2) get the above-mentioned diatomite material of 1kg, dispersed with stirring, in the ethanol of 10 liter 10%, adds 100g tetraethoxysilane, 13g TBAH and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3) above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4), after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 2nm microvoid structure and the combination of 50nm ~ 100nm macroporous structure.
embodiment 6
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 100g tetramethoxy-silicane, 10g cetyl trimethylammonium bromide, 13g tetraethyl ammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 10nm meso-hole structure and the combination of 50nm ~ 100nm macroporous structure.
embodiment 7
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 100g tetramethoxy-silicane, 10g cetyl trimethylammonium bromide, 100g tetraethyl ammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C.
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 10nm meso-hole structure and the combination of 100nm ~ 200nm macroporous structure.
embodiment 8
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 500g tetramethoxy-silicane, 10g cetyl trimethylammonium bromide, 13g TBAH and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 2nm microvoid structure and the combination of 10nm ~ 20nm meso-hole structure.
embodiment 9
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 100g tetramethoxy-silicane, 10g cetyl trimethylammonium bromide, 50g Tetramethylammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 85 DEG C;
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 2nm microvoid structure and the combination of 10nm ~ 20nm meso-hole structure.
embodiment 10
1. get diatomite original soil (more than secondary soil) 1kg, to be immersed in 1M hydrochloric acid soln 1 hour, elimination hydrochloric acid soln, adds water washing three times; Diatomite original soil after pickling to be immersed in 1M sodium hydroxide solution 20 minutes, elimination solution, adds water washing three times; 150 DEG C of forced air dryings 3 hours; Obtain the diatomite of dioxide-containing silica more than 98% as modified feedstock;
2. get the above-mentioned diatomite material of 1kg, dispersed with stirring, in 10 liters of ethanol, adds 500g tetraethoxysilane, 10g cetyl trimethylammonium bromide, 50g Tetramethylammonium hydroxide and 100g water, 35 DEG C of constant temperature stirring reactions 12 hours;
3. above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in high purity water solution, and regulation and control solution ph about 8.5, stirs ageing 6 hours at 90 DEG C;
4., after reaction product centrifugation, drying obtains the multi-stage porous modification infusorial earth with 2nm microvoid structure and the combination of 10nm ~ 20nm meso-hole structure.
Claims (2)
1. there is a modification infusorial earth for hierarchical porous structure, it is characterized in that (sign):
Add micropore and meso-hole structure in diatomaceous macroporous structure, specifically can obtain and there is the multilevel hole material that micropore (aperture 2nm) and mesoporous (aperture 10nm ~ 20nm) combine or mesoporous (aperture 10nm ~ 20nm) and macropore (aperture 50nm ~ 200nm) combination or micropore (aperture 2nm) and macropore (aperture 50nm ~ 200nm) combine.
2. a kind of preparation method with the modification infusorial earth of hierarchical porous structure according to claim 1, comprises the following steps:
1) get diatomite original soil 1kg and to be immersed in 1-2M hydrochloric acid soln 1 hour, diatomite original soil after pickling to be immersed in 1-2M sodium hydroxide solution 20 minutes, wash rear dry diatomite modified raw material with water;
2) get the diatomite modified raw material of step 1), ultrasonic disperse, in 10 liters of dehydrated alcohols, adds silicon source precursor, template, catalyzer and water, 25 DEG C ~ 40 DEG C constant temperature stirring reactions 12 hours;
Wherein, described silicon source precursor can be draw together tetramethoxy-silicane or tetraethoxysilane any one, the mass ratio of diatomite material and silicon source precursor is within the scope of 1:2 ~ 1:10;
Described catalyzer be Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide or TBAH any one, catalyzer mass concentration is in ethanol 0.1% ~ 1%;
Described template is cetyl trimethylammonium bromide, and template mass concentration is in ethanol in 0 ~ 1% scope;
Water mass concentration is in ethanol in 1% ~ 5% scope;
3) above-mentioned reaction after product centrifugation, after washing three times with water, is dispersed in 10 premium on currency, regulates and controls solution ph between 8.5-9.0,85 DEG C ~ 95 DEG C ageings 6 hours;
4), after step (3) reaction product centrifugation, drying obtains the modification infusorial earth with hierarchical porous structure.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109718810A (en) * | 2018-12-11 | 2019-05-07 | 南京杰科丰环保技术装备研究院有限公司 | A kind of preparation method of alkali modification clay-based Hydrobon catalyst |
| CN115254154A (en) * | 2022-08-10 | 2022-11-01 | 浙江库实健康科技有限公司 | Mineral particles with indoor VOCs purification function and preparation method thereof |
| CN117718042A (en) * | 2024-02-09 | 2024-03-19 | 北京理工大学 | Pd(OH) 2 Diatomite catalyst and preparation method and application thereof |
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2015
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109718810A (en) * | 2018-12-11 | 2019-05-07 | 南京杰科丰环保技术装备研究院有限公司 | A kind of preparation method of alkali modification clay-based Hydrobon catalyst |
| CN115254154A (en) * | 2022-08-10 | 2022-11-01 | 浙江库实健康科技有限公司 | Mineral particles with indoor VOCs purification function and preparation method thereof |
| CN117718042A (en) * | 2024-02-09 | 2024-03-19 | 北京理工大学 | Pd(OH) 2 Diatomite catalyst and preparation method and application thereof |
| CN117718042B (en) * | 2024-02-09 | 2024-05-28 | 北京理工大学 | Pd(OH)2Diatomite catalyst and preparation method and application thereof |
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