CN105967723A - Preparation method of silica porous material - Google Patents
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- CN105967723A CN105967723A CN201610292950.5A CN201610292950A CN105967723A CN 105967723 A CN105967723 A CN 105967723A CN 201610292950 A CN201610292950 A CN 201610292950A CN 105967723 A CN105967723 A CN 105967723A
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/785—Submicron sized grains, i.e. from 0,1 to 1 micron
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Abstract
The invention discloses a preparation method of a silica porous material. The preparation method utilizes ethyl orthosilicate as a raw material and anhydrous ethanol and deionized water as solvents and comprises uniformly dispersing silicon ions in a macromolecular complex structure through a plurality of dispersants, synthesizing xerogel for direct dry molding through an appropriate dispersant concentration, carrying out dry molding and carrying out heat treatment on the block to obtain the silica porous material. The preparation method has the advantages of simple processes, short preparation period, simple equipment and low cost. The silica porous material has uniform pore sizes and distribution.
Description
Technical field
The invention belongs to field of material technology, particularly to the preparation method of a kind of porous silica material.
Background technology
Porous material presents, with the form of porous, the feature that surface area is big, owing to having porous, surface area
Greatly, the activity feature such as big, easy recovery makes it be widely used in high-efficiency adsorbent and catalyst.Porous two
Silica material not only has that specific surface area is big, surface tension is little, gas permeability high, and
It also has the advantages such as chemical stability is good, high temperature resistant, good insulating, weatherability are strong, nonpoisonous and tasteless,
Occurring inflammable phenomenon unlike porous carbon material, this makes porous silica material have preferably application
Prospect.This patent proposes one and utilizes dispersant to make silicon ion be dispersed in system, recycles system
The viscosity one-shot forming self being had, makes the forming process conjunction of granule forming process and porous material structure
Two is one, and a step synthesizes porous silica material rapidly, for the preparation of porous silica material
Open up new preparation method, for its popularization and application.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of silicon dioxide many
The preparation method of Porous materials, has the advantages that production technology is simple, equipment requirements is simple, the cycle is short.
To achieve these goals, the technical solution used in the present invention is:
A kind of preparation method of porous silica material, with tetraethyl orthosilicate as raw material, dehydrated alcohol and
Deionized water is solvent, utilizes dispersant to make precursor solution, then through gelation, dry, dry-pressing
Porous silica material is obtained with heat treatment process.
Described dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, second
Glycol and Polyethylene Glycol composition.
The volume ratio of described dehydrated alcohol and deionized water is (2:1)～(3:1).
After described dispersant adds in solvent, the concentration range of dispersant each component is 0～0.4mol/L.
Described tetraethyl orthosilicate is 1:(1～1.5 with the mol ratio of citric acid).
Described dispersant adds in solvent, adds tetraethyl orthosilicate, regulates pH value with ammonia after dissolving
To 1～5 precursor solution, by precursor solution at 80～85 DEG C water-bath to gelation, then 140～
It is dried at 160 DEG C and forms xerogel, carry out ground sieve after naturally drying under room temperature and obtain dry gel powder
Body, more directly carry out dry-pressing formed by this xerogel powder body, forms block blank of material, after at heat
Manage and i.e. obtain porous earth silicon material.
Described heat treatment is to carry out burying burning in ZnO powder body, and temperature is 700～1000 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: compared with prior art, the present invention provides
Porous silica material preparation method in, with ethylenediaminetetraacetic acid, citric acid, diethylenetriamine
Pentacarboxylic acid, tartaric acid, ethylene glycol, Polyethylene Glycol etc. directly carry out the gel of complexation foaming as dispersant
Change process, by controlling the concentration of each material, the consumption of the most each dispersant, makes and is suitable for directly
The xerogel of molding, this is possible not only to reduce pelletize, old process, also can make crystallization process and sintering
One step completes.In conjunction with burying the heat treatment process of burning, organic foaming and decomposition combustion process is utilized to be formed
Porous silica material.This method processing step is few, manufacturing cycle is short, equipment is simple, low cost,
And the pore-size of gained porous silica material and distribution controllability good.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
(1) measure 50mL dehydrated alcohol and deionized water 2:1 mixing by volume, stir,
Weigh a certain amount of dispersant (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, winestone
Acid, ethylene glycol, Polyethylene Glycol composition, wherein Polyethylene Glycol includes again PEG400, Polyethylene Glycol
4000 and polyethylene glycol 6000) add in mixed liquor, the concentration of dispersant each component controls at 0.4mol/L.
After stirring and dissolving, add tetraethyl orthosilicate (wherein tetraethyl orthosilicate: citric acid (mol ratio)=1:
1) before, i.e. obtaining to 1～5 with ammonia (volumetric concentration 25～28%) regulation pH value after it dissolves
Drive liquid solution.
(2) by precursor solution at 80 DEG C water-bath to gelation, then be dried at 160 DEG C formed dry
Gel, by powder body is ground sieve after naturally drying under room temperature.
(3) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base
Body material carries out burying burning in ZnO powder body and i.e. obtains porous silica material, and heat treatment temperature is
1000℃.In gained porous silica material, silica particle sizes is about 30nm～150nm,
Gap size is 30nm～100nm.
Embodiment 2
(1) measure 50mL dehydrated alcohol and deionized water 3:1 mixing by volume, stir,
Weigh a certain amount of dispersant (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, winestone
Acid, ethylene glycol, Polyethylene Glycol composition.) add in mixed liquor, the concentration of dispersant each component is controlled respectively
Make 0.01,0.1,0.1,0.2,0.3,0.4mol/L, after stirring and dissolving, add tetraethyl orthosilicate
(wherein tetraethyl orthosilicate: citric acid (mol ratio)=1:1.5), (submits to ammonia after it dissolves
Concentration 25～28%) regulation pH value i.e. obtains precursor solution to 1～5.
(2) by precursor solution at 85 DEG C water-bath to gelation, then be dried at 140 DEG C formed dry
Gel, by powder body is ground sieve after naturally drying under room temperature.
(3) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base
Body material carries out burying burning in ZnO powder body and i.e. obtains porous silica material, and heat treatment temperature is
700℃.In gained porous silica material, silica particle sizes is about 30nm～150nm,
Gap a size of 30nm～100nm.
Embodiment 3
(1) measure 50mL dehydrated alcohol and deionized water 3:1 by volume, stir, claim
Measure a certain amount of dispersant (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid,
Ethylene glycol, Polyethylene Glycol form.) add in mixed liquor, the concentration of dispersant each component controls respectively
0.03,0.2,0.2,0.2,0.1,0.4mol/L, after stirring and dissolving, add tetraethyl orthosilicate (its
Middle tetraethyl orthosilicate: citric acid (mol ratio)=1:1.2), by ammonia (volumetric concentration after it dissolves
25～28%) regulation pH value i.e. obtains precursor solution to 1～5.
(2) by precursor solution at 80 DEG C water-bath to gelation, then be dried at 150 DEG C formed dry
Gel, by powder body is ground sieve after naturally drying under room temperature.
(3) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base
Body material carries out burying burning in ZnO powder body and i.e. obtains porous silica material, and heat treatment temperature is
900℃.In gained porous silica material, silica particle sizes is about 30nm～150nm,
Gap a size of 30nm～100nm.
Claims (7)
1. the preparation method of a porous silica material, it is characterised in that be former with tetraethyl orthosilicate
Material, dehydrated alcohol and deionized water are solvent, utilize dispersant to make precursor solution, then through gel
Change, dry, dry-pressing and heat treatment process obtain porous silica material.
The preparation method of porous silica material the most according to claim 1, it is characterised in that institute
State dispersant by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol and
Polyethylene Glycol forms.
The preparation method of porous silica material the most according to claim 1 or claim 2, it is characterised in that
The volume ratio of described dehydrated alcohol and deionized water is (2:1)～(3:1).
The preparation method of porous silica material the most according to claim 2, it is characterised in that institute
The mol ratio stating tetraethyl orthosilicate and citric acid is 1:(1～1.5).
5. according to the preparation method of porous silica material described in claim 1 or 4, it is characterised in that
Described dispersant adds in solvent, adds tetraethyl orthosilicate, after dissolving with ammonia regulation pH value to 1～
5 precursor solution, by precursor solution at 80～85 DEG C water-bath to gelation, then 140～
It is dried at 160 DEG C and forms xerogel, carry out ground sieve after naturally drying under room temperature and obtain dry gel powder
Body, more directly carry out dry-pressing formed by this xerogel powder body, forms block blank of material, after at heat
Manage and i.e. obtain porous earth silicon material.
The preparation method of porous silica material the most according to claim 5, it is characterised in that institute
Stating after dispersant adds in solvent, the concentration range of dispersant each component is 0～0.4mol/L.
The preparation method of porous silica material the most according to claim 5, it is characterised in that institute
Stating heat treatment is to carry out burying burning in ZnO powder body, and temperature is 700～1000 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106542847A (en) * | 2016-11-23 | 2017-03-29 | 河北大学 | A kind of porous material and preparation method thereof |
| CN106853367A (en) * | 2016-11-18 | 2017-06-16 | 江苏大学 | A kind of preparation method of the spherical xerogel catalyst of silver/silicon dioxide |
| CN108410596A (en) * | 2018-05-08 | 2018-08-17 | 罗彦明 | Multifunctional laundry liquid and its preparation process |
| CN109012570A (en) * | 2018-07-20 | 2018-12-18 | 济南大学 | A kind of plasticity alkalinity SiO2Plural gel, the preparation method of block materials and products obtained therefrom and application |
| CN111635541A (en) * | 2020-05-21 | 2020-09-08 | 常州可赛成功塑胶材料有限公司 | Preparation method of low-VOC silicone lubricating master batch for polyolefin composite material |
| CN113694214A (en) * | 2021-09-06 | 2021-11-26 | 西北大学 | PH/reduction double-sensitive calcium carbonate-silicon dioxide drug-loaded nano material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106853367A (en) * | 2016-11-18 | 2017-06-16 | 江苏大学 | A kind of preparation method of the spherical xerogel catalyst of silver/silicon dioxide |
| CN106542847A (en) * | 2016-11-23 | 2017-03-29 | 河北大学 | A kind of porous material and preparation method thereof |
| CN108410596A (en) * | 2018-05-08 | 2018-08-17 | 罗彦明 | Multifunctional laundry liquid and its preparation process |
| CN109012570A (en) * | 2018-07-20 | 2018-12-18 | 济南大学 | A kind of plasticity alkalinity SiO2Plural gel, the preparation method of block materials and products obtained therefrom and application |
| CN109012570B (en) * | 2018-07-20 | 2021-04-13 | 济南大学 | Plastic alkaline SiO2Preparation method of composite gel and block material, and obtained product and application |
| CN111635541A (en) * | 2020-05-21 | 2020-09-08 | 常州可赛成功塑胶材料有限公司 | Preparation method of low-VOC silicone lubricating master batch for polyolefin composite material |
| CN113694214A (en) * | 2021-09-06 | 2021-11-26 | 西北大学 | PH/reduction double-sensitive calcium carbonate-silicon dioxide drug-loaded nano material and preparation method thereof |
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Application publication date: 20160928 |