CN105967724A - Preparation method of zinc oxide porous material - Google Patents
Preparation method of zinc oxide porous material Download PDFInfo
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- CN105967724A CN105967724A CN201610293327.1A CN201610293327A CN105967724A CN 105967724 A CN105967724 A CN 105967724A CN 201610293327 A CN201610293327 A CN 201610293327A CN 105967724 A CN105967724 A CN 105967724A
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
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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
- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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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
- C04B35/632—Organic additives
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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
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- 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 zinc oxide porous material. The preparation method comprises dissolving zinc nitrate as a raw material in a sol-gel system under action of organics such as ethylene diamine tetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid, tartaric acid, glycol and polyethylene glycol so that zinc ions uniformly exist in the sol-gel system, controlling component concentrations, carrying out dry-pressing molding on the xerogel obtained by gelatinization and drying, and sintering the press-molded block to obtain the zinc oxide porous material. The preparation method has simple processes, utilizes simple equipment and realizes a low cost.
Description
Technical field
The invention belongs to field of material technology, particularly to the preparation method of a kind of zinc oxide porous material.
Background technology
Zinc oxide is a kind of broad-band gap group Ⅱ-Ⅵ compound semiconductor material, have chemical stability good and
The time property advantage such as good, nontoxic, photocatalytic degradation Organic substance, solaode, super hydrophobic material,
The each side such as sensor, luminescent material has a wide range of applications.Nano zinc oxide material has high ratio
Surface area, this makes it have high activity, thus at each effective catalyst, adsorbing material, storage material
The each side such as material, sensor, biomaterial have breakthrough, but high specific surface area and surface activity,
Make nano-particle material be easily generated agglomeration, thus have influence on performance and the application of nano zinc oxide material.
Synthesizing zinc oxide porous material, the existence of micropore not only can keep high specific surface area and surface activity,
And solve the agglomeration traits brought due to nano-powder material.Deposit in current preparation method
In the problem of manufacturing cycle length, this patent proposes the preparation side of the short porous oxidation Zinc material of a kind of periodicity
Method.
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 zinc oxide porous
The preparation method of material, 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 zinc oxide porous material, with zinc nitrate as raw material, dehydrated alcohol and deionization
Water is solvent, utilizes dispersant to make precursor solution, then through gelation, dry, dry-pressing and Re Chu
Reason process obtains zinc oxide porous material.
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 (1:1)～(2:1).
After described dispersant adds in solvent, the concentration range of dispersant each component is 0～0.4mol/L.
It is 1:(0.5～1 that described zinc nitrate amount ranges meets the mol ratio of zinc ion and citric acid).
Described dispersant adds in solvent, adds zinc nitrate, before after dissolving, regulation pH value obtains to 3～7
Driving liquid solution, by precursor solution, at 80～85 DEG C, water-bath is to gelation, then at 140～160 DEG C
It is dried and forms xerogel, carry out ground sieve after naturally drying under room temperature and obtain xerogel powder body, then by this
Xerogel powder body directly carries out dry-pressing formed, forms block blank of material, the most thermally treated i.e. obtains porous
Earth silicon material.
Described heat treatment is to carry out burying burning in ZnO powder body, and temperature is 1000 DEG C～1200 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: the zinc oxide porous material that the present invention provides
Preparation method in, with ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, second
Glycol, Polyethylene Glycol etc., as dispersant, use specific colloidal sol process for preparation, make ion more uniformly
It is present in gel, after gelation, is directly over being dried, the process such as briquetting, heat treatment obtains zinc oxide
Porous material.By controlling the concentration of each material during this, the kind of the most each dispersant and consumption,
Make the xerogel powder body of applicable straight forming, the method utilizes gelation process make zinc ion uniform
Stably it is present in gel powder body, makes grain formation process and loose structure forming process unite two into one,
This not only shortens manufacturing cycle, and utilizes gelation process, makes crystal structure process become more equal
Even, crystal grain particle diameter and being more evenly distributed, so that loose structure mesopore size and distribution are more equal
Even.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
The preparation method of a kind of zinc oxide porous material, comprises the steps:
(1) measure 50mL dehydrated alcohol and deionized water 1:1 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
0.4mol/L, after stirring and dissolving, adds zinc nitrate (zinc ion is 1:0.5 with the mol ratio of citric acid),
After it dissolves, regulate pH value i.e. obtain precursor solution to 3～7.
(2) by precursor solution at 80 DEG C water-bath to gelation, then be dried at 140 DEG C formed dry solidifying
Glue, 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 zinc oxide porous material, and heat treatment temperature is
1000℃.In gained zinc oxide porous material, crystallite dimension is about 200nm～700nm, and gap size is
150nm～300nm.
Embodiment 2
The preparation method of a kind of zinc oxide porous material, comprises the steps:
(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.) 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 zinc nitrate (zinc
Ion is 1:1 with the mol ratio of citric acid), after it dissolves, regulate pH value i.e. obtain forerunner to 3～7
Liquid solution.
(2) by precursor solution at 85 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 zinc oxide porous material, and heat treatment temperature is
1200℃.In gained zinc oxide porous material, crystallite dimension is about 200nm～700nm, and gap size is
150nm～300nm.
Embodiment 3
The preparation method of a kind of zinc oxide porous material, comprises the steps:
(1) measuring 50mL dehydrated alcohol and deionized water 1.5:1 mixing by volume, stirring is all
Even, weigh 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 is divided
Do not control 0.03,0.2,0.2,0.2,0.1,0.4mol/L, after stirring and dissolving, add zinc nitrate
(zinc ion is 1:0.6 with the mol ratio of citric acid), regulates pH value after it dissolves and i.e. obtains to 3～7
Obtain precursor solution.
(2) by precursor solution at 85 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 zinc oxide porous material, and heat treatment temperature is
1100℃.In gained zinc oxide porous material, crystallite dimension is about 200nm～700nm, and gap size is
150nm～300nm.
Claims (7)
1. the preparation method of a zinc oxide porous material, it is characterised in that with zinc nitrate as raw material, nothing
Water-ethanol and deionized water are solvent, utilize dispersant to make precursor solution, then through gelation, dry
Dry, dry-pressing and heat treatment process, it is thus achieved that zinc oxide porous material.
The preparation method of zinc oxide porous material the most according to claim 1, it is characterised in that described
Dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol and gathers
Ethylene glycol forms.
The preparation method of zinc oxide porous 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 (1:1)～(2:1).
The preparation method of zinc oxide porous material the most according to claim 2, it is characterised in that described
It is 1:(0.5～1 that zinc nitrate amount ranges meets the mol ratio of zinc ion and citric acid).
5. according to the preparation method of zinc oxide porous material described in claim 1 or 4, it is characterised in that
Described dispersant adds in solvent, adds zinc nitrate, regulates pH value and obtain presoma to 3～7 after dissolving
Solution, by gelation drier at 140～160 DEG C for precursor solution water-bath at 80～85 DEG C
Form xerogel, carry out ground sieve after naturally drying under room temperature and obtain xerogel powder body, then this is dry solidifying
Rubber powder body directly carries out dry-pressing formed, forms block blank of material, the most thermally treated i.e. obtains porous dioxy
Silicon nitride material.
The preparation method of zinc oxide porous material the most according to claim 5, it is characterised in that described
After dispersant adds in solvent, the concentration range of dispersant each component is 0～0.4mol/L.
The preparation method of zinc oxide porous material the most according to claim 5, it is characterised in that described
Heat treatment is to carry out burying burning in ZnO powder body, and temperature is 1000 DEG C～1200 DEG C.
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| CN201610293327.1A CN105967724A (en) | 2016-05-05 | 2016-05-05 | Preparation method of zinc oxide porous material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112316933A (en) * | 2020-12-14 | 2021-02-05 | 安徽锦华氧化锌有限公司 | Preparation method of zinc oxide with photocatalytic effect |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1166454A (en) * | 1997-01-20 | 1997-12-03 | 华东理工大学 | Liquid phase superfine zinc oxide preparing process through stepped nucleating growth |
| CN1587061A (en) * | 2004-08-26 | 2005-03-02 | 复旦大学 | Process for preparing sol-gel of nano zinc oxide by low temperature |
| CN1796552A (en) * | 2004-12-29 | 2006-07-05 | 华东理工大学 | Method for preparing porous material in lumpy in use for biological zymophore |
| JP2007070188A (en) * | 2005-09-08 | 2007-03-22 | Chiba Univ | Method for producing zinc oxide fine particle and aggregate and dispersion solution of the same |
| CN101734709A (en) * | 2008-11-12 | 2010-06-16 | 中国科学院宁波材料技术与工程研究所 | Controllable method for preparing nano zinc oxide powder |
| CN102515246A (en) * | 2011-12-02 | 2012-06-27 | 南京林业大学 | Preparation method of porous nano zinc oxide (ZnO) |
-
2016
- 2016-05-05 CN CN201610293327.1A patent/CN105967724A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1166454A (en) * | 1997-01-20 | 1997-12-03 | 华东理工大学 | Liquid phase superfine zinc oxide preparing process through stepped nucleating growth |
| CN1587061A (en) * | 2004-08-26 | 2005-03-02 | 复旦大学 | Process for preparing sol-gel of nano zinc oxide by low temperature |
| CN1796552A (en) * | 2004-12-29 | 2006-07-05 | 华东理工大学 | Method for preparing porous material in lumpy in use for biological zymophore |
| JP2007070188A (en) * | 2005-09-08 | 2007-03-22 | Chiba Univ | Method for producing zinc oxide fine particle and aggregate and dispersion solution of the same |
| CN101734709A (en) * | 2008-11-12 | 2010-06-16 | 中国科学院宁波材料技术与工程研究所 | Controllable method for preparing nano zinc oxide powder |
| CN102515246A (en) * | 2011-12-02 | 2012-06-27 | 南京林业大学 | Preparation method of porous nano zinc oxide (ZnO) |
Non-Patent Citations (2)
| Title |
|---|
| 米晓云等: "《Al2O3纳米粉体及透明陶瓷》", 31 March 2012, 吉林大学出版社 * |
| 衣宝廉: "《燃料电池-原理.技术.应用》", 31 August 2003, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112316933A (en) * | 2020-12-14 | 2021-02-05 | 安徽锦华氧化锌有限公司 | Preparation method of zinc oxide with photocatalytic effect |
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Application publication date: 20160928 |