CN101722030A - Preparation method of compound photocatalytic water purification material - Google Patents
Preparation method of compound photocatalytic water purification material Download PDFInfo
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- CN101722030A CN101722030A CN200910201048A CN200910201048A CN101722030A CN 101722030 A CN101722030 A CN 101722030A CN 200910201048 A CN200910201048 A CN 200910201048A CN 200910201048 A CN200910201048 A CN 200910201048A CN 101722030 A CN101722030 A CN 101722030A
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Abstract
The invention relates to a preparation method of a compound photocatalytic water purification material, comprising the step of: fixing nanometer titanium dioxide particles of industrial finished products with the best photocatalytic performance on a micron zeolite sieve or surfaces of medical stone particles by a ball milling method to a multifunctional compound material with the photocatalytic performance and the original water purification characteristic of a carrier. The method has the advantages of simple process, lower raw material cost and no pollution to the environment in a production process, and is suitable for industrial production. The prepared compound material has wide application prospect in the field of advanced treatment of drinking water.
Description
Technical field
The present invention relates to a kind of preparation method of compound photocatalytic water purification material, be specifically related to a kind of preparation technology of drinking water treatment new material.
Background technology
Nano titanium oxide is as a kind of semiconductor light-catalyst, its stable chemical performance, be insoluble in acid-base solution and water, nontoxic to human body, under the irradiation of ultraviolet light, can produce highly active hydroxyl radical free radical, and hydroxyl radical free radical can be degraded almost and all organic pollutions of mineralising owing to its superpower oxidation characteristic.But there is the recovery difficulty in nano titanium oxide as photocatalysis, and the deactivated shortcoming of reuniting easily is difficult to direct use.In order to address this problem, nano titanium oxide is loaded on the stable carrier, become a kind of effective solution.A kind of Zeolite-based nano metal oxide composite and preparation method thereof is disclosed as Chinese invention patent ZL 03129239.9.Chinese invention patent application 200510027382.8 discloses a kind of nano titanium oxide/zeolite composite photocatalyst material and preparation method thereof.Chinese invention patent application 200610040680.5 discloses a kind of preparation method who only generates nano-titania particle at outer surface of zeolite.Because nano titanium oxide only is created on the outer surface of zeolite, do not influence the loose structure of zeolite inside, therefore possessed the dual-use function of photocatalysis and ion-exchange.Chinese invention patent 02115438 discloses a kind of preparation method of compound Chinese medicinal stone, and this method is made ferromagnetism medical stone aggregated particles with the sintered body of the mixture of natural medical stone powder and reduced iron powder, and then deposits one or more layers TiO on particle
2+ Ag or copper or platinum or palladium nano-particles light-sensitive catalyst film.The load principle of above patent all is that zeolite molecular sieve or medical stone are immersed in soluble metallic salt or TiO
2In the colloidal sol stoste, then in air roasting to generate the nano particle of different size.The temperature of roasting has not only determined the size and the specific area of the titanium dioxide nanoparticle that generates, and has also determined it to generate anatase phase and rutile ratio mutually of nano titanium oxide simultaneously.Because the photocatalytic activity of nano titanium oxide depends primarily on specific area and anatase phase and rutile ratio mutually, the nano titanium oxide that obtains in order to last method is not in optimal value, its photocatalysis effect is less than commercially available nanometer level titanium dioxide powder material product (this kind material employing air burning method preparation that is used for photocatalysis use, possess and compare above-mentioned two kinds of better stability of patent and photocatalysis performance), the anatase of the industrialized nano titanium dioxide product of photocatalysis effect optimum is 7: 3 with rutile ratio mutually mutually at present, in addition, the primary raw material titanium salt or the TiO of existing patent technology use
2Colloidal sol stoste cost is higher, and its production process can produce pollution to environment.
Zeolite molecular sieve is widely used in fields such as absorption, heterocatalysis, gas separation, ion-exchange as a kind of inorganic poromerics.In recent years, because the pollution of water environment, this inorganic material of zeolite is widely used in water treatment field, soak the way of using steam treatment again as Chinese invention patent 98121578 by soda acid and improve adsorptivity of natural zeolite, heavy metal ion, organic matter, agricultural chemicals, chloroform etc. are had good removal effect.Chinese invention patent 200520039982, zeolite powder is bonded on the solid netted material of porous with binding agent, then with this kind material-paving in two sides, contaminated river course, select to adsorb the ammonia nitrogen of removing in the water by zeolite powder, the while is at the microbiological oxidation ammonia nitrogen of material surface enrichment and growth.Chinese invention patent 200810034170 by modifier and natural zeolite powder are mixed, has been made the former water treatment of suitable different quality, can efficiently remove ammonia nitrogen, organic water treatment agent.U.S. Pat 5223022 discloses a kind of low silica-alumina ratio zeolite of using as ion-exchanger, removes the toxic heavy metal ion in the water that pollutes.U.S. Pat 5298166 discloses with zeolite molecular sieve load metatitanic acid and has received as ion-exchanger, is used for handling the isotopic ion of nuclear fuel waste liquid.
Medical stone as a kind of to biological nontoxic, harmless and possess bioactive complex mineral, except possessing absorption and ion exchange property, also contain 18 kinds of trace elements such as the necessary potassium of human body, sodium, calcium, magnesium, phosphorus macroelement and zinc, iron, selenium, copper, strontium, iodine, fluorine, metasilicic acid.Therefore, medical stone is widely used in the drinking water field.As Chinese utility model patent 88221158 medical stone and clay are made the water tumbler courage, make the drinking-water mineralising, thus the fatigue of elimination, disease preventing and treating.Chinese invention patent 02133039 discloses a kind of manufacture method of Chinese Maifan stone mineralized water, and the mineralising that medical stone is used for running water is handled, and has not only removed the harmful substance in the water, has also added useful material.Though above material possesses excellent organic matter absorption property, ion-exchange performance or water-mineralizing performance, does not possess photocatalytic activity, can not be with the polluter photocatalytic degradation when being adsorbed with organic pollutants.
Summary of the invention
The preparation method who the purpose of this invention is to provide the compound water-purifying material of a kind of photocatalysis, the compound water-purifying material of photocatalysis that obtains with the inventive method had both possessed photocatalysis performance, possessed the original water purification characteristic of carrier again.This material is with a wide range of applications in the drinking water deep process field.
In order to achieve the above object, the present invention is according to the drinking water deep handling principle, the finished industrial product Nano titanium dioxide particle that will have an optimal light catalytic performance is fixed on micron-sized zeolite molecular sieve or medical stone granule: surface by the method for ball milling, thereby obtains this compound photocatalytic water purification material.
Concrete technology is as follows:
Measure nano-titanium dioxide powder earlier: zeolite molecular sieve or medical stone=1%-50%: the 99%-50% mass percent; Then nano-titanium dioxide powder is placed methyl alcohol or ethanolic solution, the dispersant that adds the 0.01%-1% of nano-titanium dioxide powder quality then, process 20-100kHz obtains the oar material after adding zeolite molecular sieve or medical stone mixing after ultrasonic dispersion treatment 5-100 minute, the oar material is placed in the ball mill mechanical ball milling 1-5 hour, rotational speed of ball-mill is 110-220 rev/min, the mixed powder that then will obtain behind the above-mentioned ball milling descended dry 1-3 hour at 80-110 ℃ again, at last in air with 350-500 ℃ of roasting 3-6 hour, promptly get the compound photocatalytic water purification material product.
Above-mentioned dispersant is trimethylolethane or polyacrylamide.
Above-mentioned abrading-ball: slurry=2-10 when the oar material is placed in the ball mill mechanical ball milling: 1 part of weight ratio.，
Above-mentioned nano-titanium dioxide powder is a finished industrial product Nano titanium dioxide particle, and particle diameter is the 1-100 nanometer.
Above-mentioned zeolite molecular sieve or medical stone are micron-sized through natural or synthesis zeolite, medical stone granule: after the processed, and particle diameter is the 1-100 micron.
Described zeolite molecular sieve is selected from 5A zeolite molecular sieve or 13X zeolite molecular sieve.
Advantage of the present invention and effect are:
1. because the present invention is fixed on micron-sized zeolite molecular sieve or medical stone granule: surface with the method for the finished industrial product Nano titanium dioxide particle with photocatalysis performance by ball milling, thereby the compound photocatalytic water purification material that obtains had both possessed photocatalysis performance, possessing the original water purification characteristic of carrier again, is multifunctional composite.
Since the titanium dioxide granule on the artificial or natural zeolite molecular sieve of the present invention, medical stone granule: (powder) combine by ball grinding method, therefore organic pollution possesses absorption property in satisfying water, heavy metal in the water possessed ion-exchange performance, bacterium in the water is possessed absorption and kills performance etc., and to stripping multi mineral gradually in the water and micro-multiple performance.
3. because the present invention is with micron-sized particle with after closing ball milling, adds thermal bake-out and obtain in air, the method technology is easy, and cost of material is lower, can not produce pollution to environment in the production process, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of the water-purifying material that load nano-titanium dioxide 1%, 5%, 10%, 15% forms on 5A zeolite molecular sieve of the present invention and the 5A zeolite molecular sieve.
Fig. 2 be 13X zeolite molecular sieve of the present invention and on the 13X zeolite molecular sieve x-ray diffraction pattern of load nano-titanium dioxide 1%, 5%, 10%, 15% formed water-purifying material.
Fig. 3 is the electromicroscopic photograph before the load of 5A zeolite molecular sieve, and its particle size is the 2-3 micron.
Fig. 4 is the electromicroscopic photograph that forms water-purifying material behind the 5A zeolite molecular sieve load nano-titanium dioxide of the present invention, and the granular size of its load nano-titanium dioxide is the 30-50 nanometer.
Fig. 5 is the electromicroscopic photograph before the load of 13X zeolite molecular sieve.
Fig. 6 is the electromicroscopic photograph that forms water-purifying material behind the 13X zeolite molecular sieve load nano-titanium dioxide of the present invention.
The specific embodiment
Below by embodiment the present invention is further described,
At first, the used method of testing of the water-purifying material feature that obtains of embodiments of the invention method is as follows:
1, X-ray diffraction: the present invention is the composite of zeolite molecular sieve or medical stone and nano titanium oxide composition, provide the strong diffraction maximum of zeolite molecular sieve or medical stone in the x-ray diffraction pattern, and the characteristic diffraction peak of nano titanium oxide, can judge whether successful load of nano titanium oxide with this.
2, a launch environment SEM: can be clear that state and the size of nano titanium oxide in zeolite molecular sieve or the existence of medical stone surface by electron-microscope scanning.
Be the test result of example explanation material of the present invention with 5A and 13X zeolite molecular sieve load Germany P-25 type nano-titanium dioxide powder below.
Embodiment 1
Take by weighing the above-mentioned titanium dioxide powder of 0.5g and place the 100ml ethanolic solution, add the 0.001g trimethylolethane, the ultrasonic dispersion treatment of 100kHz 20 minutes, add the commercially available 5A zeolite molecular sieve of 4.5g, the slurry that after mixing mixing is obtained mechanical ball milling 1 hour on ball mill, the weight ratio of getting abrading-ball and material is 5: 1, and rotational speed of ball-mill is 120 rev/mins.With the mixed powder that obtains behind the above-mentioned ball milling 110 ℃ dry 1 hour down, and then in air with 450 ℃ of roastings 5 hours, get final product goods, be designated as 10wt%TiO
2/ 5A.
This product characterizes and sees also the x-ray diffraction pattern that Fig. 1: a is the 5A zeolite molecular sieve with X-ray diffraction, a launch environment SEM, and b, c, d, e are respectively the x-ray diffraction pattern of the composite that load nano-titanium dioxide 1%, 5%, 10%, 15% formed the inventive method obtains on the 5A zeolite molecular sieve.Nano titanium oxide can be described in the successful load in 5A zeolite molecular sieve surface from Fig. 1, the size of the size of nano titanium oxide and 5A zeolite is respectively 30 nanometers and 3 microns, with consistent before the load.
Among Fig. 1, a is the x-ray diffraction pattern of typical 5A zeolite molecular sieve, and b, c, d, e are respectively the x-ray diffraction pattern of load nano-titanium dioxide 1%, 5%, 10%, 15% formed composite on the 5A zeolite molecular sieve.Among Fig. 2, a is the x-ray diffraction pattern of 13X zeolite molecular sieve, and b, c, d, e are respectively the x-ray diffraction pattern of load nano-titanium dioxide 1%, 5%, 10%, 15% formed composite on the 13X zeolite molecular sieve.Along with the increasing of load capacity, grow illustrates the surperficial successful load of nano titanium oxide at 5A and 13X zeolite molecular sieve gradually from the characteristic peak of nano titanium oxide.The result of electron microscope has further confirmed the firm load of nano titanium oxide on 5A and 13X zeolite molecular sieve surface.From electromicroscopic photograph, the size of graininess nano titanium oxide is about the consistent size before 20-30 nanometer and the load.
Embodiment 2
Take by weighing the 0.75g nano-titanium dioxide powder and place the 150ml ethanolic solution, add the 0.002g trimethylolethane, the ultrasonic dispersion treatment of 50kHz 40 minutes, add the 4.25g13X zeolite molecular sieve, with mixed slurry mechanical ball milling 1.5 hours on ball mill, the weight ratio of getting abrading-ball and material is 8: 1, and rotational speed of ball-mill is 140 rev/mins.With the mixed powder that obtains behind the above-mentioned ball milling 110 ℃ dry 1.5 hours down, and then in air with 400 ℃ of roastings 6 hours, get final product goods, be designated as 15wt%TiO
2/ 13X.
This product characterizes and sees also Fig. 2 with X-ray diffraction, a launch environment SEM: among the figure, a is the x-ray diffraction pattern of 13X zeolite molecular sieve, and b, c, d, e are respectively the x-ray diffraction pattern of load nano-titanium dioxide 1%, 5%, 10%, 15% formed composite on the 13X zeolite molecular sieve.
This product characterizes with X-ray diffraction, a launch environment SEM: nano titanium oxide is in the successful load in 13X zeolite molecular sieve surface, the size of the size of nano titanium oxide and 13X zeolite is respectively 30 nanometers and 3 microns, with consistent before the load.
Embodiment 3
Take by weighing the 1g nano-titanium dioxide powder and place the 200ml ethanolic solution, add the 0.002g trimethylolethane, the ultrasonic dispersion treatment of 20kHz 60 minutes, add the 4g medical stone, with mixed slurry mechanical ball milling 1 hour on ball mill, the weight ratio of getting abrading-ball and material is 2: 1, and rotational speed of ball-mill is 150 rev/mins.With the mixed powder that obtains behind the above-mentioned ball milling 110 ℃ dry 1 hour down, and then in air with 500 ℃ of roastings 3 hours, get final product goods, be designated as 20wt%TiO
2/ medical stone.
This product characterizes with X-ray diffraction, a launch environment SEM: nano titanium oxide is successful load on the medical stone surface, and the size of nano titanium oxide and the size of medical stone are respectively 30 nanometers and 50 microns, with consistent before the load.
Embodiment 4
Take by weighing the 0.5g nano-titanium dioxide powder and place the 100ml methanol solution, add the 0.001g trimethylolethane, the ultrasonic dispersion treatment of 80kHz 20 minutes, add the 4.5g clinoptilolite, with mixed slurry mechanical ball milling 1 hour on ball mill, the weight ratio of getting abrading-ball and material is 5: 1, and rotational speed of ball-mill is 120 rev/mins.With the mixed powder that obtains behind the above-mentioned ball milling 110 ℃ dry 1 hour down, and then in air with 450 ℃ of roastings 5 hours, get final product goods, be designated as 10wt%TiO
2/ clinoptilolite.
This product characterizes with X-ray diffraction, a launch environment SEM: nano titanium oxide is successful load on the clinoptilolite surface, and the size of nano titanium oxide and the size of clinoptilolite are respectively 30 nanometers and 100 microns, with consistent before the load.
Claims (4)
1. the preparation method of a compound photocatalytic water purification material is characterized in that: measure nano-titanium dioxide powder earlier: zeolite molecular sieve or medical stone=1%-50%: the 99%-50% mass percent; Then nano-titanium dioxide powder is placed methyl alcohol or ethanolic solution, the dispersant that adds the 0.01%-1% of nano-titanium dioxide powder quality then, after adding zeolite molecular sieve or medical stone mixing after ultrasonic dispersion treatment 5-100 minute, process 20-100kHz obtains the oar material, the oar material is placed in the ball mill mechanical ball milling 1-5 hour, rotational speed of ball-mill is 110-220 rev/min, the mixed powder that then will obtain behind the above-mentioned ball milling descended dry 1-3 hour at 80-110 ℃ again, at last in air with 350-500 ℃ of roasting 3-6 hour, promptly get the product compound photocatalytic water purification material;
Above-mentioned dispersant is trimethylolethane or polyacrylamide;
Above-mentioned abrading-ball: slurry=2-10 when the oar material is placed in the ball mill mechanical ball milling: 1 part of weight ratio.
2. the preparation method of a kind of compound photocatalytic water purification material according to claim 1, it is characterized in that: described nano-titanium dioxide powder is commercially available finished industrial product Nano titanium dioxide particle, and particle diameter is the 1-100 nanometer.
3. the preparation method of a kind of compound photocatalytic water purification material according to claim 1, it is characterized in that: described zeolite molecular sieve or medical stone are natural or synthesis zeolite, the medical stone granule :s that possesses after the process processed of micron-sized size, and particle diameter is the 1-100 micron.
4. the preparation method of a kind of compound photocatalytic water purification material according to claim 1, it is characterized in that: described zeolite molecular sieve is selected from 5A zeolite molecular sieve or 13X zeolite molecular sieve.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001722A (en) * | 2010-11-04 | 2011-04-06 | 南京大学 | Method for removing phosphate from water by using zirconia-modified mesoporous silicon material |
| EP2508478A1 (en) * | 2011-03-17 | 2012-10-10 | Paltentaler Minerals GmbH & Co KG | Photocatalytically active natural zeolite in alkaline building material systems |
| CN103100380A (en) * | 2013-02-05 | 2013-05-15 | 喻政华 | Titanium dioxide selective catalyst |
| CN104445497A (en) * | 2014-11-13 | 2015-03-25 | 中国科学院广州能源研究所 | Method for recovering nutrient substances from biogas slurry by use of combinational adsorbents |
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| CN105923693A (en) * | 2016-06-21 | 2016-09-07 | 江门市江海区炜洁净水材料有限公司 | Domestic water purifier and preparation method thereof |
| CN106215916A (en) * | 2016-08-11 | 2016-12-14 | 广西南宁胜祺安科技开发有限公司 | A kind of compound titanium dioxide optical catalyst |
| CN106268749A (en) * | 2016-08-11 | 2017-01-04 | 广西南宁胜祺安科技开发有限公司 | A kind of method preparing Novel Titanium dioxide photocatalyst |
| CN106268838A (en) * | 2016-08-11 | 2017-01-04 | 广西南宁胜祺安科技开发有限公司 | A kind of high-activity titanium deoxide composite photo-catalyst |
| CN106278152A (en) * | 2016-08-12 | 2017-01-04 | 陈赛霞 | A kind of preparation method of the heat-resisting cooking device of antibacterial boccaro |
| CN106362717A (en) * | 2016-08-11 | 2017-02-01 | 广西南宁胜祺安科技开发有限公司 | Preparation method for supported titanium dioxide photocatalyst |
| CN108452824A (en) * | 2017-02-20 | 2018-08-28 | 金华职业技术学院 | It is a kind of to prepare load pure rutile phase TiO2The method of the clinoptilolite of nanotube |
| CN108855200A (en) * | 2018-05-30 | 2018-11-23 | 中南大学 | A kind of preparation method of the support type black titanium dioxide of high catalytic activity |
| CN110354825A (en) * | 2019-07-12 | 2019-10-22 | 吉林建筑大学 | A kind of adsorbent for electroplating wastewater adsorption treatment |
| CN113019423A (en) * | 2021-02-03 | 2021-06-25 | 中国船舶重工集团公司第七一八研究所 | Catalyst for oxidizing ammonia gas by ozone, preparation method and application thereof |
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| CN116040731A (en) * | 2023-01-31 | 2023-05-02 | 广东名桂环保有限公司 | Composite water treatment agent and preparation method thereof |
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| CN102001722A (en) * | 2010-11-04 | 2011-04-06 | 南京大学 | Method for removing phosphate from water by using zirconia-modified mesoporous silicon material |
| CN102001722B (en) * | 2010-11-04 | 2012-06-13 | 南京大学 | Method for removing phosphate from water by using zirconia-modified mesoporous silicon material |
| EP2508478A1 (en) * | 2011-03-17 | 2012-10-10 | Paltentaler Minerals GmbH & Co KG | Photocatalytically active natural zeolite in alkaline building material systems |
| CN103100380A (en) * | 2013-02-05 | 2013-05-15 | 喻政华 | Titanium dioxide selective catalyst |
| CN103100380B (en) * | 2013-02-05 | 2014-11-19 | 喻政华 | Titanium dioxide selective catalyst |
| CN104445497A (en) * | 2014-11-13 | 2015-03-25 | 中国科学院广州能源研究所 | Method for recovering nutrient substances from biogas slurry by use of combinational adsorbents |
| CN104971707A (en) * | 2015-06-03 | 2015-10-14 | 河南师范大学 | Loaded natural zeolite/Bi2O2CO3-BiPO4 composite photocatalyst and preparation method thereof |
| CN105923693A (en) * | 2016-06-21 | 2016-09-07 | 江门市江海区炜洁净水材料有限公司 | Domestic water purifier and preparation method thereof |
| CN106268838A (en) * | 2016-08-11 | 2017-01-04 | 广西南宁胜祺安科技开发有限公司 | A kind of high-activity titanium deoxide composite photo-catalyst |
| CN106268749A (en) * | 2016-08-11 | 2017-01-04 | 广西南宁胜祺安科技开发有限公司 | A kind of method preparing Novel Titanium dioxide photocatalyst |
| CN106215916A (en) * | 2016-08-11 | 2016-12-14 | 广西南宁胜祺安科技开发有限公司 | A kind of compound titanium dioxide optical catalyst |
| CN106362717A (en) * | 2016-08-11 | 2017-02-01 | 广西南宁胜祺安科技开发有限公司 | Preparation method for supported titanium dioxide photocatalyst |
| CN106278152A (en) * | 2016-08-12 | 2017-01-04 | 陈赛霞 | A kind of preparation method of the heat-resisting cooking device of antibacterial boccaro |
| CN108452824A (en) * | 2017-02-20 | 2018-08-28 | 金华职业技术学院 | It is a kind of to prepare load pure rutile phase TiO2The method of the clinoptilolite of nanotube |
| CN108855200A (en) * | 2018-05-30 | 2018-11-23 | 中南大学 | A kind of preparation method of the support type black titanium dioxide of high catalytic activity |
| CN110354825A (en) * | 2019-07-12 | 2019-10-22 | 吉林建筑大学 | A kind of adsorbent for electroplating wastewater adsorption treatment |
| CN113797927A (en) * | 2020-06-12 | 2021-12-17 | 赵石永 | Sterilization film, preparation method thereof and application thereof in lighting device |
| CN113019423A (en) * | 2021-02-03 | 2021-06-25 | 中国船舶重工集团公司第七一八研究所 | Catalyst for oxidizing ammonia gas by ozone, preparation method and application thereof |
| CN113019423B (en) * | 2021-02-03 | 2023-02-24 | 中国船舶重工集团公司第七一八研究所 | Catalyst for oxidizing ammonia gas by ozone, preparation method and application thereof |
| CN116040731A (en) * | 2023-01-31 | 2023-05-02 | 广东名桂环保有限公司 | Composite water treatment agent and preparation method thereof |
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