CN102580713B - Method for preparing titanium dioxide/silicate mineral nano composites - Google Patents
Method for preparing titanium dioxide/silicate mineral nano composites Download PDFInfo
- Publication number
- CN102580713B CN102580713B CN 201210015970 CN201210015970A CN102580713B CN 102580713 B CN102580713 B CN 102580713B CN 201210015970 CN201210015970 CN 201210015970 CN 201210015970 A CN201210015970 A CN 201210015970A CN 102580713 B CN102580713 B CN 102580713B
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- silicate mineral
- titanium
- composite material
- nano composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a method for preparing titanium dioxide/silicate mineral nano composites. The method comprises the following steps of: firstly, adding silicate minerals to a titanium tetrachloride solution to activate the silicate minerals and dissolve foreign ions; secondly, adding a certain alkaline solution to convert titanium ions to titanium dioxide hydrate precipitates and washing off other foreign ions to obtain titanium dioxide hydrate/silicate mineral complex filter cakes; and thirdly, adding the filter cakes to the titanium tetrachloride solution, adopting the acid environment of the titanium tetrachloride solution to realize dissolution of the titanium dioxide hydrates, secondary activation of the silicate minerals and low temperature crystallization and growth of nanotitanium dioxide on the silicate minerals and carrying out filtering, washing, drying and grinding, thus finally preparing the titanium dioxide/silicate mineral nano composites. The method has the following advantages that the method is simple and practical in steps; the reaction conditions are mild; the raw materials are simple and have low cost; and the method is suitable for large-scale production and can be beneficial to effective improvement of the photocatalytic efficiency of titanium dioxide.
Description
Technical field
The present invention relates to the preparation method of a kind of titanium dioxide/silicate mineral nano composite material.
Background technology
Nano titanium oxide is a kind of typical photochemical catalyst, has advantages such as catalytic activity height, chemical property is stable, nontoxic, use is safe, and wide application prospect is arranged in wastewater treatment.Yet in the actual use of nano titanium oxide, exist shortcomings such as bad dispersibility, recovery difficulty, thereby limited its industrialized application.In recent years, utilize various preparing carriers load type titania photocatalysts to receive much concern, wherein silicate mineral has reserves are abundant, cheap, specific area is big, excellent absorption property and easy advantage such as recovery and obtained extensive use as carrier of photocatalyst.Chinese patent CN1970149A discloses a kind of bergmeal particle loaded nano TiO
2The preparation method, with dilute sulfuric acid acid treatment diatomite, the smart soil that makes is dispersed in the urea liquid earlier, add titanyl sulfate solution then, water-bath heating mixed liquor obtains the compound slurries, 300～800 ℃ of calcinings down, makes bergmeal particle loaded nano TiO at last
2Product.The weak point of this method is: use dilute sulfuric acid to handle original soil, the waste liquor contamination environment of generation increases if deal with cost in addition; Calcining back nano-titania particle is easily reunited, thereby influences the photocatalysis effect and recycle value not high.Chinese patent CN101607194A discloses a kind of preparation method of anatase type titanium dioxide/montmorillonite nano composite material, and this method uses titanate esters to do the titanium source, and expensive, preparation process has been used a large amount of organic solvents, is unfavorable for environmental protection.
Summary of the invention
In view of the existing problem of background technology, the object of the present invention is to provide a kind of titanium dioxide/silicate mineral nano composite material and the preparation method, the raw material sources that prepare this composite are abundant, cheap, and this method preparation technology is simple and can effectively improve optically catalytic TiO 2 efficient.
The invention provides the preparation method of a kind of titanium dioxide/silicate mineral nano composite material, comprise the steps:
1, at first silicate mineral is added titanium tetrachloride solution, the hydrochloric acid that utilizes the titanium tetrachloride solution hydrolysis to produce activates and the dissolved impurity ion silicate mineral;
2, add certain alkaline solution then the titanium ion in the solution is converted into the titanium dioxide hydrates precipitation, other foreign ions of flush away obtain titanium dioxide hydrates/silicate mineral complex filter cake;
3, again filter cake is added in the titanium tetrachloride solution, the sour environment that utilizes the titanium tetrachloride solution hydrolysis to produce is realized dissolving, the re-activation of silicate mineral, the low temperature crystallized and growth of nano titanium oxide on silicate mineral of titanium dioxide hydrates, filtration, washing, dry, pulverizing make titanium dioxide/silicate mineral nano composite material at last.
As preferably, the invention provides the preparation method of a kind of titanium dioxide/silicate mineral nano composite material, (the titanium dioxide: be 0.2～1: 1 silicate mineral) of the mass ratio of titanium dioxide and silicate mineral in the composite.The preparation method of this composite comprises the steps:
1, silicate mineral is added in the titanium tetrachloride solution of 0.5～3.0 mol, flooded under the room temperature 3～60 hours, obtain titanium dioxide precursor/silicate mineral slurries;
2, the temperature of the titanium dioxide precursor/silicate mineral slurries of regulating step 1 gained is 10～50 ℃, stir on one side, the pH value that adds the alkaline solution regulation system of 0.5～4.0 mol on one side is 1.6～3.0, filter, wash the electrical conductivity≤200 μ S/cm to filtrate, obtain titanium dioxide hydrates/silicate mineral complex filter cake;
3, the titanium dioxide hydrates/silicate mineral complex filter cake with step 2 gained adds in the titanium tetrachloride solution of 0.2～1.0 mol, be warming up to 60～100 ℃, insulated and stirred reaction 1～12 hour, pH value with the alkaline solution regulation system of 1.0～4.0 mol is 6.5～7.5, obtains titanium dioxide/silicate mineral nano composite material slurries;
4, with the composite dope filtration of step 3 gained, wash, 60-180 ℃ of drying pulverized, and namely gets titanium dioxide/silicate mineral nano composite material powder.
Silicate mineral described in the step 1 is a kind of in attapulgite, imvite, diatomite, sepiolite, mica, talcum, rectorite, illite, pyrophillite, the expanded perlite.
Described titanium tetrachloride solution consumption is by the quality of titanium dioxide that its complete reaction generates, and titanium dioxide and silicate mineral quality are than (titanium dioxide: be 0.1～0.8: 1 silicate mineral) in the step 1; Titanium dioxide and silicate mineral quality are than (titanium dioxide: be 0.1～0.2: 1 silicate mineral) in the step 3.
Alkaline solution described in the step 2,3 is a kind of in sodium hydroxide solution, potassium hydroxide solution, the ammoniacal liquor.
The invention has the advantages that:
1, utilize in the step 1 hydrochloric acid that the titanium tetrachloride solution hydrolysis produces the part solubility in acid impurity in the silicate mineral with the ionic species stripping, cation exchanges in titanium ion and the silicate mineral simultaneously, increase specific area and the absorption property of clay, improved load capacity; Titanium tetrachloride is simultaneously as titanium source and acid source, not only saved cost but also reduced pollution to environment.
2, titanium ion is converted into the titanium dioxide hydrates precipitation fully in step 2 system, foreign ion does not form the indissoluble thing simultaneously, can remove foreign ion fully through repeatedly washing, eliminate the influence of impurity to composite photocatalysis effect on the one hand, be the low temperature crystallized condition of having created of next step nano titanium oxide on the other hand.
3, in the step 3 titanium tetrachloride solution added in the filter cake after the washing, the sour environment that utilizes titanium tetrachloride hydrolysis to produce is realized dissolving, the re-activation of silicate mineral, the low temperature crystallized and growth of nano titanium oxide on silicate mineral of titanium dioxide hydrates, saved and added sour step, under temperate condition, prepared highly active titanium dioxide/silicate mineral nano composite material.
4, the method for the invention step is simple, and reaction condition gentleness and raw material are simple, and be cheap, is fit to large-scale production, and can effectively improves optically catalytic TiO 2 efficient.
The specific embodiment
Below in conjunction with embodiment and comparative example, the invention will be further described, but never limit the scope of the invention:
Embodiment 1: 10 kilograms of attapulgite powders are added in the titanium tetrachloride solution of 30 liter of 2.0 mol, dipping is 24 hours under the room temperature, obtains titanium dioxide precursor/attapulgite slurry.The temperature of control titanium dioxide precursor/attapulgite slurry is 30 ℃, stir on one side, the sodium hydroxide solution that adds on one side 2.0 mol in the slurries, when the pH of system value reaches 2.5, filter, wash to the electrical conductivity of filtrate be 150 μ S/cm, obtain titanium dioxide hydrates/attapulgite clay compounded body filter cake.Filter cake is added in the titanium tetrachloride solution of 30 liter of 0.5 mol, be warming up to 80 ℃, the insulated and stirred reaction is after 4 hours, pH value with the sodium hydroxide solution regulation system of 2.0 mol is 7.0, filter washing, 60 ℃ of dryings, pulverize, obtain titanium dioxide/attapulgite clay nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 54%, and crystallite dimension is 6.3nm, and rutile content is 46%, crystallite dimension is 8.0nm, the mass ratio of titanium dioxide and attapulgite (titanium dioxide: attapulgite) be 0.6: 1.
Embodiment 2: 10 kilograms of attapulgite powders are added in the titanium tetrachloride solution of 25 liter of 0.5 mol, dipping is 60 hours under the room temperature, obtains titanium dioxide precursor/attapulgite slurry.The temperature of control titanium dioxide precursor/attapulgite slurry is 10 ℃, stir on one side, the potassium hydroxide solution that adds on one side 4.0 mol in the slurries, when the pH of system value reaches 1.6, filter, wash to the electrical conductivity of filtrate be 105 μ S/cm, obtain titanium dioxide hydrates/attapulgite clay compounded body filter cake.Filter cake is added in the titanium tetrachloride solution of 62.5 liter of 0.2 mol, be warming up to 100 ℃, the insulated and stirred reaction is after 1 hour, pH value with the potassium hydroxide solution regulation system of 4.0 mol is 6.5, filter washing, 80 ℃ of dryings, pulverize, obtain titanium dioxide/attapulgite clay nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 48%, and crystallite dimension is 6.5nm, and rutile content is 52%, crystallite dimension is 8.2nm, the mass ratio of titanium dioxide and attapulgite (titanium dioxide: attapulgite) be 0.2: 1.
Embodiment 3: 10 kilograms of attapulgite powders are added in the titanium tetrachloride solution of 33.3 liter of 3.0 mol, dipping is 3 hours under the room temperature, obtains titanium dioxide precursor/attapulgite slurry.The temperature of control titanium dioxide precursor/attapulgite slurry is 50 ℃, stir on one side, the ammoniacal liquor that adds on one side 0.5 mol in the slurries, when the pH of system value reaches 3.0, filter, wash to the electrical conductivity of filtrate be 200 μ S/cm, obtain titanium dioxide hydrates/attapulgite clay compounded body filter cake.Filter cake is added in the titanium tetrachloride solution of 25 liter of 1.0 mol, be warming up to 60 ℃, the insulated and stirred reaction is after 12 hours, pH value with the ammoniacal liquor regulation system of 0.5 mol is 7.5, filters washing, 120 ℃ of dryings are pulverized, and obtain titanium dioxide/attapulgite clay nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 60%, and crystallite dimension is 6.9nm, and rutile content is 40%, crystallite dimension is 8.8nm, the mass ratio of titanium dioxide and attapulgite (titanium dioxide: attapulgite) be 1: 1.
Embodiment 4: 10 kilograms of calcium-base montmorillonite powders are added in the titanium tetrachloride solution of 32 liter of 1.0 mol, dipping is 45 hours under the room temperature, obtains titanium dioxide precursor/montmorillonite slurry.The temperature of control titanium dioxide precursor/montmorillonite slurry is 20 ℃, stir on one side, the sodium hydroxide solution that adds on one side 3.5 mol in the slurries, when the pH of system value reaches 2.0, filter, wash to the electrical conductivity of filtrate be 125 μ S/cm, obtain titanium dioxide hydrates/montmorillonite Composite body filter cake.Filter cake is added in the titanium tetrachloride solution of 30 liter of 0.6 mol, be warming up to 90 ℃, the insulated and stirred reaction is after 2 hours, pH value with the sodium hydroxide solution regulation system of 3.5 mol is 6.8, filter washing, 140 ℃ of dryings, pulverize, obtain titanium dioxide/Nano composite material of montmorillonite powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 51%, and crystallite dimension is 6.4nm, and rutile content is 49%, crystallite dimension is 8.1nm, the mass ratio of titanium dioxide and imvite (titanium dioxide: imvite) be 0.4: 1.
Embodiment 5: 10 kilograms of diatomite powders are added in the titanium tetrachloride solution of 32.6 liter of 2.3 mol, dipping is 12 hours under the room temperature, obtains titanium dioxide precursor/diatomite slurries.The temperature of control titanium dioxide precursor/diatomite slurries is 35 ℃, stir on one side, the potassium hydroxide solution that adds on one side 1.5 mol in the slurries, when the pH of system value reaches 2.7, filter, wash to the electrical conductivity of filtrate be 180 μ S/cm, obtain the fit filter cake of titanium dioxide hydrates/tripolite compound.Filter cake is added in the titanium tetrachloride solution of 31.25 liter of 0.8 mol, be warming up to 70 ℃, the insulated and stirred reaction is after 8 hours, pH value with the potassium hydroxide solution regulation system of 1.5 mol is 7.2, filter washing, 180 ℃ of dryings, pulverize, obtain titanium dioxide/diatomite nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 57%, and crystallite dimension is 6.7nm, and rutile content is 43%, crystallite dimension is 8.5nm, titanium dioxide and diatomaceous mass ratio (titanium dioxide: diatomite) be 0.8: 1.
Embodiment 6: external except changing the attapulgite powder into sepiolite powder in embodiment 6, other technological parameters are all identical with embodiment 1 with method of operating, obtain titanium dioxide/sepiolite nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 54%, and crystallite dimension is 6.2nm, and rutile content is 46%, crystallite dimension is 8.1nm, the mass ratio of titanium dioxide and sepiolite (titanium dioxide: sepiolite) be 0.6: 1.
Embodiment 7: except the attapulgite powder is changed into the mica powder, other technological parameters are all identical with embodiment 1 with method of operating in embodiment 7, obtain titanium dioxide/mica nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 53%, and crystallite dimension is 6.4nm, and rutile content is 47%, crystallite dimension is 8.2nm, the mass ratio of titanium dioxide and mica (titanium dioxide: mica) be 0.6: 1.
Embodiment 8: except the attapulgite powder is changed into the talcum powder, other technological parameters are all identical with embodiment 1 with method of operating in embodiment 8, obtain titanium dioxide/talcum nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 55%, and crystallite dimension is 6.5nm, and rutile content is 45%, crystallite dimension is 8.4nm, the mass ratio of titanium dioxide and talcum (titanium dioxide: talcum) be 0.6: 1.
Embodiment 9: except the attapulgite powder is changed into the rectorite powder, other technological parameters are all identical with embodiment 1 with method of operating, obtain titanium dioxide/rectorite nano composite material powder in embodiment 9.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 54%, and crystallite dimension is 6.4nm, and rutile content is 46%, crystallite dimension is 8.3nm, the mass ratio of titanium dioxide and rectorite (titanium dioxide: rectorite) be 0.6: 1.
Embodiment 10: except the attapulgite powder is changed into the illite powder, other technological parameters are all identical with embodiment 1 with method of operating in embodiment 10, obtain titanium dioxide/illite nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 53%, and crystallite dimension is 6.3nm, and rutile content is 47%, crystallite dimension is 8.2nm, titanium dioxide and illitic mass ratio (titanium dioxide: illite) be 0.6: 1.
Embodiment 11: external except changing the attapulgite powder into pyrophyllite powder in embodiment 11, other technological parameters are all identical with embodiment 1 with method of operating, obtain titanium dioxide/pyrophillite nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 52%, and crystallite dimension is 6.5nm, and rutile content is 48%, crystallite dimension is 8.3nm, the mass ratio of titanium dioxide and pyrophillite (titanium dioxide: pyrophillite) be 0.6: 1.
Embodiment 12: external except changing the attapulgite powder into swelling perlite powder in embodiment 12, other technological parameters are all identical with embodiment 1 with method of operating, obtain titanium dioxide/expanded perlite nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 55%, and crystallite dimension is 6.3nm, and rutile content is 45%, crystallite dimension is 8.2nm, the mass ratio of titanium dioxide and expanded perlite (titanium dioxide: expanded perlite) be 0.6: 1.
Comparative example 1: 10 kilograms of attapulgite powders are added in the titanium tetrachloride solution of 30 liter of 2.0 mol, the temperature of control mixed serum is 30 ℃, stir on one side, the sodium hydroxide solution that adds on one side 2.0 mol in the slurries, when the pH of system value reaches 2.5, filter, wash to the electrical conductivity of filtrate be 150 μ S/cm, obtain titanium dioxide hydrates/attapulgite clay compounded body filter cake.Filter cake is added in the titanium tetrachloride solution of 30 liter of 0.5 mol, be warming up to 80 ℃, the insulated and stirred reaction is after 4 hours, pH value with the sodium hydroxide solution regulation system of 2.0 mol is 7.0, filters washing, drying is pulverized, and obtains titanium dioxide/attapulgite clay nano composite material powder.Titanium dioxide is the mixed crystal of anatase and rutile in the nano composite material, wherein anatase content is 54%, and crystallite dimension is 6.4nm, and rutile content is 46%, crystallite dimension is 8.1nm, the mass ratio of titanium dioxide and attapulgite (titanium dioxide: attapulgite) be 0.6: 1.
Comparative example 2: 10 kilograms of attapulgite powders are added in the titanium tetrachloride solution of 37.5 liter of 2.0 mol, dipping is 24 hours under the room temperature, obtains titanium dioxide precursor/attapulgite slurry.The temperature of control titanium dioxide precursor/attapulgite slurry is 30 ℃, stir on one side, add the sodium hydroxide solution of 2.0 mol on one side in the slurries, when the pH of system value reaches 2.5, stop to add, be warming up to 80 ℃, the insulated and stirred reaction is after 4 hours, pH value with the sodium hydroxide solution regulation system of 2.0 mol is 7.0, filter washing, drying, pulverize, obtain titanium dioxide/attapulgite composite material powder.Titanium dioxide is undefined structure in the composite, the mass ratio of titanium dioxide and attapulgite (titanium dioxide: attapulgite) be 0.6: 1.
Comparative example 3: 10 kilograms of attapulgite powders are added in the titanium tetrachloride solution of 30 liter of 2.0 mol, dipping is 24 hours under the room temperature, obtains titanium dioxide precursor/attapulgite slurry.The temperature of control titanium dioxide precursor/attapulgite slurry is 30 ℃, stir on one side, the sodium hydroxide solution that adds on one side 2.0 mol in the slurries, when the pH of system value reaches 2.5, filter, wash to the electrical conductivity of filtrate be 150 μ S/cm, obtain titanium dioxide hydrates/attapulgite clay compounded body filter cake.Filter cake is added in the titanium tetrachloride solution of 30 liter of 0.5 mol, be warming up to 40 ℃, the insulated and stirred reaction is after 4 hours, pH value with the sodium hydroxide solution regulation system of 2.0 mol is 7.0, filters washing, drying is pulverized, and obtains titanium dioxide/attapulgite composite material powder.Titanium dioxide is undefined structure in the composite, the mass ratio of titanium dioxide and attapulgite (titanium dioxide: attapulgite) be 0.6: 1.
The photocatalysis performance evaluation of embodiment 13 titanium dioxide/silicate mineral nano composite material
In XPA photochemical reaction instrument (the dynamo-electric factory of Nanjing Xu Jiang), add the nano composite material that 0.2 restraint is equipped with, the reactive red M-2B aqueous solution that to add 500 milliliters of mass concentrations again be 20 mg/litre, open the air that stirs and feed 0.02 liter/minute of flow from the bottom, open uviol lamp (power 15W, wavelength 254nm), every 15 milliliters of sampling in 10 minutes, centrifugation is got supernatant liquor and is tested.Measure solution absorbency by spectrophotometer under its maximum absorption wavelength, degradation rate is calculated as follows:
η is degradation rate (%); A
0, A
tBe respectively degrade preceding, the solution absorbance of t after the time; C
0, C
tBe respectively degrade preceding, the solution concentration of t after the time.
The photocatalysis experimental data of embodiment and comparative example products obtained therefrom is as shown in table 1 below.The reactive red degradation rate is more high to show that the photocatalysis performance of titanium dioxide/silicate mineral nano composite material is more good.Lack 3-60 hour step of dipping among the present invention in the comparative example 1, silicate does not cause the final products photocatalytic activity not high through effectively activating.Lack in the comparative example 2 in the step 2 of the present invention filter and step 3 in add titanium tetrachloride solution again, titanium dioxide fails to carry out low temperature crystallized and growth at silicate mineral, so titanium dioxide is undefined structure in the product, photocatalytic activity is not high.Having changed the temperature of step 3 of the present invention in the comparative example 3, is 40 ℃ only, has influenced titanium dioxide and has carried out low temperature crystallized and growth at silicate mineral, and effect same is undesirable.
The photocatalysis test of table 1 clay/titanic oxide nano compound material
Be enlightenment with above-mentioned foundation desirable embodiment of the present invention, by above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification, must determine its technical scope according to the claim scope.
Claims (5)
1. the preparation method of titanium dioxide/silicate mineral nano composite material comprises the steps:
(1), at first silicate mineral is added titanium tetrachloride solution, the hydrochloric acid that utilizes the titanium tetrachloride solution hydrolysis to produce activates and the dissolved impurity ion silicate mineral;
(2), then add certain alkaline solution the titanium ion in the solution is converted into the titanium dioxide hydrates precipitation, other foreign ions of flush away obtain titanium dioxide hydrates/silicate mineral complex filter cake;
(3), again filter cake is added in the titanium tetrachloride solution, the sour environment that utilizes the titanium tetrachloride solution hydrolysis to produce is realized dissolving, the re-activation of silicate mineral, the low temperature crystallized and growth of nano titanium oxide on silicate mineral of titanium dioxide hydrates, filtration, washing, dry, pulverizing make titanium dioxide/silicate mineral nano composite material at last.
2. the preparation method of the described titanium dioxide of claim 1/silicate mineral nano composite material is characterized in that the mass ratio of titanium dioxide and silicate mineral is 0.2～1:1 in the composite, and the preparation method of this composite comprises the steps:
(1), silicate mineral is added in the titanium tetrachloride solution of 0.5～3.0 mol, flooded under the room temperature 3～60 hours, obtain titanium dioxide precursor/silicate mineral slurries;
(2), the temperature of the titanium dioxide precursor/silicate mineral slurries of regulating step 1 gained is 10～50 ℃, stir on one side, the pH value that adds the alkaline solution regulation system of 0.5～4.0 mol on one side is 1.6～3.0, filter, wash the electrical conductivity≤200 μ S/cm to filtrate, obtain titanium dioxide hydrates/silicate mineral complex filter cake;
(3), the titanium dioxide hydrates/silicate mineral complex filter cake with step 2 gained adds in the titanium tetrachloride solution of 0.2～1.0 mol, be warming up to 60～100 ℃, insulated and stirred reaction 1～12 hour, pH value with the alkaline solution regulation system of 1.0～4.0 mol is 6.5～7.5, obtains titanium dioxide/silicate mineral nano composite material slurries;
(4), with the composite dope filtration of step 3 gained, washing, 60-180 ℃ of drying pulverized, and namely gets titanium dioxide/silicate mineral nano composite material powder.
3. the preparation method of claim 1 or 2 described titanium dioxide/silicate mineral nano composite materials is characterized in that the silicate mineral described in the step 1 is selected from attapulgite, imvite, diatomite, sepiolite, mica, talcum, rectorite, illite, pyrophillite, expanded perlite.
4. the preparation method of the described titanium dioxide of claim 2/silicate mineral nano composite material, it is characterized in that the titanium tetrachloride solution consumption by the quality of titanium dioxide that its complete reaction generates, titanium dioxide is 0.1～0.8:1 with silicate mineral quality ratio in the step 1; In the step 3, initiate titanium tetrachloride solution in the filter cake, the titanium dioxide that changes into is 0.1～0.2:1 with silicate mineral quality ratio.
5. the preparation method of the described titanium dioxide of claim 2/silicate mineral nano composite material is characterized in that the alkaline solution described in the step 2,3 is a kind of in sodium hydroxide solution, potassium hydroxide solution, the ammoniacal liquor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210015970 CN102580713B (en) | 2012-01-18 | 2012-01-18 | Method for preparing titanium dioxide/silicate mineral nano composites |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210015970 CN102580713B (en) | 2012-01-18 | 2012-01-18 | Method for preparing titanium dioxide/silicate mineral nano composites |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102580713A CN102580713A (en) | 2012-07-18 |
| CN102580713B true CN102580713B (en) | 2013-09-18 |
Family
ID=46470266
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210015970 Active CN102580713B (en) | 2012-01-18 | 2012-01-18 | Method for preparing titanium dioxide/silicate mineral nano composites |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102580713B (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102907384B (en) * | 2012-09-25 | 2014-03-12 | 安徽福斯特渔具有限公司 | Bionic bait with swingable fish head |
| CN103212393B (en) * | 2013-04-26 | 2015-09-23 | 长江水利委员会长江科学院 | Nano-TiO 2/ montmorillonite Composite photocatalysis material for water treatment and preparation method thereof |
| CN106082320B (en) * | 2016-06-23 | 2017-07-07 | 吉林大学 | A kind of hydrothermal synthesis method of Erie's ground mass anatase compound |
| CN107384072B (en) * | 2017-07-21 | 2019-10-18 | 南京理工大学 | Infrared-reflection heat-insulation coating and preparation method thereof based on bismuth molybdate compound |
| CN107376882A (en) * | 2017-08-01 | 2017-11-24 | 洛阳理工学院 | A kind of nanometer titanium dioxide composite material circulation utilization method |
| CN108295830B (en) * | 2018-01-18 | 2021-02-05 | 中国建筑材料科学研究总院有限公司 | TiO with 001, 101 crystal face exposed2Sepiolite composite gel and preparation method thereof |
| CN108906014A (en) * | 2018-08-03 | 2018-11-30 | 西南科技大学 | A kind of high temperature resistant visible-light-responsive photocatalyst and preparation method thereof |
| CN109338454A (en) * | 2018-09-26 | 2019-02-15 | 浙江凯色丽科技发展有限公司 | The preparation method of the siliceous titanium dioxide crystal whisker of rutile-type |
| CN109504136B (en) * | 2018-11-21 | 2020-09-18 | 延边大学 | Nano TiO (titanium dioxide)2Interior wall coating of silica complex based on illite and preparation method thereof |
| CN110218084B (en) * | 2019-05-29 | 2021-06-11 | 浙江大学 | Formaldehyde-removing metal anticorrosive coating and coating method thereof |
| CN110724254B (en) * | 2019-10-18 | 2021-02-12 | 常州大学盱眙凹土研发中心 | Rod-shaped amorphous/anatase TiO2Preparation method and application of composite catalyst |
| CN111908502B (en) * | 2020-06-25 | 2023-05-26 | 江阴市友佳珠光云母有限公司 | Production process of colorful ultrathin synthetic mica sheet |
| CN114345316A (en) * | 2022-01-12 | 2022-04-15 | 上海大学 | TiO22Preparation method of magnesium lithium silicate composite photocatalyst |
| CN114469757A (en) * | 2022-01-14 | 2022-05-13 | 常州纳欧新材料科技有限公司 | Preparation method of attapulgite-based ultraviolet blocking material |
| CN115873306B (en) * | 2022-12-14 | 2024-02-06 | 江苏纳欧新材料有限公司 | Preparation method of high-length-diameter-ratio and high-whiteness conductive material |
| CN116618050B (en) * | 2023-04-20 | 2024-01-12 | 陕西科技大学 | Titanium dioxide/ferric silicate heterojunction photo-Fenton catalyst, preparation method and application |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI124294B (en) * | 2007-08-16 | 2014-06-13 | Sachtleben Pigments Oy | Process for the preparation of a highly dispersible microcrystalline titanium dioxide product, the product and its use |
| CN101333345B (en) * | 2008-07-30 | 2011-07-27 | 江苏工业学院 | Method for preparing nanometer titanium dioxide/attapulgite composite material |
| CN101804338B (en) * | 2009-05-19 | 2012-04-18 | 王秀宝 | Process for producing nano titanium dioxide/diatomite composite photocatalytic material |
-
2012
- 2012-01-18 CN CN 201210015970 patent/CN102580713B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN102580713A (en) | 2012-07-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102580713B (en) | Method for preparing titanium dioxide/silicate mineral nano composites | |
| CN102068998B (en) | Preparation and application methods of BiOBr/BiOCl compound photocatalyst | |
| CN101549299B (en) | Non-metallic element multiple doping nano titanium dioxide photocatalyst and preparation method | |
| CN101508464B (en) | Process for preparing anatase type nano-titanium dioxide | |
| CN102698785B (en) | A kind of tripolite loading nitrogen-doped nanometer TiO 2the preparation method of catalysis material | |
| CN102091644B (en) | Method for preparing carbon-nitrogen-chlorine co-doped nano titanium dioxide photocatalysts | |
| CN101791546A (en) | Method for preparing mixed-phase nano-titania hydrosol photocatalyst | |
| CN101429348A (en) | Process for producing nano-titanium dioxide-zinc oxide composite powder | |
| CN101698507B (en) | Method for quickly preparing rutile phase nano titanium dioxide | |
| CN103240073A (en) | Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof | |
| CN104211109A (en) | Highly pure brookite type titanium dioxide nanosheet, and preparation method and application thereof | |
| CN102784647A (en) | Preparation method for (101)-surface nanoFe-TiO2 high-efficiency nitrogen-fixing photocatalyst | |
| CN102765758B (en) | Sol-gel-hydrothermal method for preparing bismuth tungstate and indium-doped bismuth tungstate | |
| CN102389836B (en) | Polyaniline/titanium dioxide/clay nanometer composite photocatalyst and preparation method thereof | |
| CN101698506B (en) | Preparation method of mixed crystal type nanometer titanium dioxide | |
| Qi et al. | Controlled synthesis of BiVO4 with multiple morphologies via an ethylenediamine-assisted hydrothermal method | |
| He et al. | In situ synthesis of the mesoporous C–TiO2 microspheres derived from partial hydrolysis tetrabutyl titanate for enhanced photocatalytic degradation under visible light | |
| CN102274719A (en) | Visible-light-responsive nano composite powder photocatalyst and preparation method thereof | |
| CN103601239A (en) | Preparation method of anatase and brookite mixed crystal TiO2 nanowire | |
| CN110227458B (en) | Copper-doped mesoporous titanium dioxide composite material and application thereof | |
| CN102432064A (en) | Method for synthesizing nanometer titanium dioxide by reverse microemulsion carbon adsorption titanium tetrachloride hydrolytic system | |
| CN104841471A (en) | Method for doping TiO2 and ammonia water modified carrier activated carbon in Fe to prepare Fe-TiO2/N-AC photocatalyst | |
| CN110040774B (en) | Method for preparing nano titanium dioxide by using metatitanic acid | |
| Febiyanto et al. | Facile synthesis of Ag3PO4 photocatalyst with varied ammonia concentration and its photocatalytic activities for dye removal | |
| CN100566826C (en) | A kind of method of preparing photocatalytic material by titanic iron ore ore concentrate wet chemical method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |