CN102580710A - Nano TiO2 composite water treatment material and preparation method thereof - Google Patents
Nano TiO2 composite water treatment material and preparation method thereof Download PDFInfo
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- CN102580710A CN102580710A CN2012100743698A CN201210074369A CN102580710A CN 102580710 A CN102580710 A CN 102580710A CN 2012100743698 A CN2012100743698 A CN 2012100743698A CN 201210074369 A CN201210074369 A CN 201210074369A CN 102580710 A CN102580710 A CN 102580710A
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Abstract
The invention discloses a nano TiO2 composite water treatment material and a preparation method thereof, and relates to a nano composite water treatment material and a preparation method thereof. The material solves the problem that the nano TiO2 photocatalytic performance of the nano TiO2 composite water treatment material and the original properties of other materials compounded with nano TiO2 are greatly reduced because the conventional nano TiO2 composite water treatment material is obtained by adopting a blending technology; and the invention provides a mature nano TiO2 composite water treatment material preparation method capable of preserving the properties of the nano TiO2 and a composite matrix material. The nano TiO2 composite water treatment material is prepared from a siloxane polymer and TiO2 sol. The preparation method comprises the following steps of: 1, preparing the TiO2 sol; and 2, adding the siloxane polymer into the TiO2 sol, soaking, stirring, cooling, and thus forming a composite polymer by the TiO2 and the siloxane. The nano TiO2 siloxane composite water treatment material can be applied in the field of deep treatment of water.
Description
Technical field
The present invention relates to a kind of nano combined material for water treatment and preparation method thereof.
Background technology
Nano-TiO
2Have the photocatalysis effect, can organic matter degradation in the water be become inorganic matter, therefore be widely used in water treatment field.Because in water treatment procedure, being difficult to of nano material reclaims, so will carry out re-using after compound with other materials.At present, nano-TiO
2The compound level that also only rests on simple blend with other materials.Because the nano-TiO that adopts blending technology to obtain at present
2No matter compound material for water treatment is nano-TiO
2Photocatalysis performance, still and nano-TiO
2The primary characteristic of carrying out compound other materials all significantly reduces.
And the nano-TiO in existing stage
2Groping and experience of the also main dependence experiment of the preparation of compound material for water treatment and research, what a cover was unripe can keep nano-TiO
2And the nano-TiO of compound matrix material characteristic
2Compound material for water treatment preparation method causes nano-TiO
2The design of compound material for water treatment and development results are difficult to unified.
Summary of the invention
The present invention will solve present nano-TiO
2Compound material for water treatment adopts blending technology to obtain, and causes nano-TiO
2The nano-TiO of compound material for water treatment
2Photocatalysis performance, and and nano-TiO
2The problem that the primary characteristic of carrying out compound other materials all significantly reduces; And a kind of maturation is provided can keep nano-TiO
2And the nano-TiO of compound matrix material characteristic
2Compound material for water treatment preparation method.
Nano-TiO of the present invention
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0. 2～0.3.
Above-mentioned nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.2～0.3 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment.
Nano-TiO of the present invention
2Compound material for water treatment is not TiO
2With the simple mixing of siloxane polymer, but submicroscopic organic compound.Itself has certain gap siloxane polymer, forms a large amount of photocatalytic activity centers, simultaneously again with TiO
2Load on certain siloxane polymer material; And, nano-TiO
2Compound material for water treatment exists on very little yardstick and is separated, so nano-TiO of the present invention
2The photocatalysis performance of compound material for water treatment significantly improves.
Nano-TiO of the present invention
2The nano-TiO that the preparation method of compound material for water treatment is prepared
2Compound material for water treatment is keeping nano-TiO
2Photocatalysis performance the time, kept advantages such as siloxane polymer light weight, stable performance, designability.
Because nano-TiO of the present invention
2The preparation method of compound material for water treatment can keep nano-TiO
2And the compound matrix material characteristic, so can design, prepare nano-TiO by pre-determined characteristics
2Compound material for water treatment is broken away from the track method that research, design, preparation to material need be leaned on experience and groped.
Nano-TiO of the present invention
2Compound material for water treatment can be used for process field, and has excellent treatment effect.
Description of drawings
Fig. 1 is the specific embodiment 16 nano-TiOs
2The XRD figure of compound material for water treatment.
Fig. 2 is the nano-TiO of the specific embodiment 16 preparations
2The SEM electron-microscope scanning figure of compound material for water treatment.
Fig. 3 is TiO in the specific embodiment 17
2Photocatalysis water treatment design sketch under colloidal sol and the siloxane polymer Different Weight ratio condition.
The specific embodiment
Technical scheme of the present invention is not limited to the following cited specific embodiment, also comprises the combination in any between each specific embodiment.
The specific embodiment one: this embodiment nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0. 2～0.3.
The specific embodiment two: this embodiment with the difference of the specific embodiment one is: siloxane polymer is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are (9 ︰ 1)～(8 ︰ 2).Other is identical with embodiment one.
The specific embodiment three: this embodiment with the specific embodiment one or two difference is: nano-TiO
2The particle diameter of compound material for water treatment is 1 ~ 2mm.Other is identical with embodiment one or two.
The specific embodiment four: this embodiment nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0.21; Siloxane polymer is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 88 ︰ 12.
The specific embodiment five: this embodiment nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0.25; Siloxane polymer is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 86 ︰ 14.
The specific embodiment six: this embodiment nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0.28; Siloxane polymer is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 82 ︰ 18.
The specific embodiment seven: this embodiment nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0.29; Siloxane polymer is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 81 ︰ 19.
The specific embodiment eight: this embodiment nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0.3; Siloxane polymer is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 80 ︰ 20.
The specific embodiment nine: this embodiment nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.2～0.3 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment.
This embodiment has preparation method's simple possible, and is with low cost, is easy to form industrialization.
The specific embodiment ten: this embodiment with the difference of the specific embodiment nine is: the siloxane polymer in the step 2 is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are (9 ︰ 1)～(8 ︰ 2).Other step and parameter are identical with embodiment nine.
The specific embodiment 11: this embodiment with the specific embodiment nine or ten difference is: in the step 2 siloxane polymer is added TiO
2Dipping and stir and pour in the spherical module room temperature after 2 hours into and cool off naturally in the colloidal sol promptly obtains the nano-TiO that particle diameter is 1 ~ 2mm
2Compound material for water treatment.Other step and parameter are identical with embodiment nine or ten.
The specific embodiment 12: this embodiment nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.28 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment; Wherein, Siloxane polymer is processed by a chlorine trimethyl silane (TMS) and bisphenol A type epoxy resin (EP); With bisphenol A type epoxy resin (EP) and a chlorine trimethyl silane (TMS) mixed in molar ratio by 80 ︰ 20; Under 250 ± 10 ℃ of conditions, add thermal condensation then, divide water again, obtain siloxane polymer.
This embodiment nano-TiO
2Compound material for water treatment has the excellent physical characteristic of siloxane polymer, and impact strength reaches 20.2kJ/m
2, hot strength reaches 67.04MPa, and elongation at break reaches 11.29%, and Tg reaches 167.98 ℃.
The specific embodiment 13: this embodiment nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.24 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment;
Wherein, Siloxane polymer is processed by dimethyldichlorosilane (DMS) and bisphenol A type epoxy resin (EP); With bisphenol A type epoxy resin (EP) and dimethyldichlorosilane (DMS) mixed in molar ratio by 82 ︰ 18; Under 250 ± 10 ℃ of conditions, add thermal condensation then, divide water again, obtain siloxane polymer.
This embodiment nano-TiO
2Compound material for water treatment has the excellent physical characteristic of siloxane polymer, and impact strength reaches 20.4kJ/m
2, hot strength reaches 68.27MPa, and Tg reaches 167.98 ℃.
The specific embodiment 14: this embodiment nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.25 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment;
Wherein, Siloxane polymer is by dimethyldichlorosilane, α, and ω-dichloro dimethyl silicone polymer (DPS) and bisphenol A type epoxy resin (EP) are processed, with bisphenol A type epoxy resin (EP) and dimethyldichlorosilane, α; ω-dichloro dimethyl silicone polymer is by the mixed in molar ratio of 81 ︰, 1 ︰ 18; Under 250 ± 10 ℃ of conditions, add thermal condensation then, divide water again, obtain siloxane polymer.
This embodiment nano-TiO
2Compound material for water treatment has the excellent physical characteristic of siloxane polymer, and impact strength reaches 31.6kJ/m
2, hot strength reaches 68.27MPa, and elongation at break reaches 81.68%, and Tg reaches 174.50 ℃.
The specific embodiment 15: this embodiment nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.25 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment;
Wherein, siloxane polymer is processed by LSI and epoxy resin E-44, with epoxy resin E-44 and the LSI mixed in molar ratio by 88 ︰ 12, under 250 ± 10 ℃ of conditions, adds thermal condensation then, divides water again, obtains siloxane polymer;
LSI is processed by ethyl orthosilicate and epoxychloropropane; By (mol ratio of 80～85) ︰ (5～20) is mixed ethyl orthosilicate and added in the solvent with epoxychloropropane; And the weight ratio of pressing siloxane polymer 0.01% adds catalyst formic acid; Under temperature 25 ℃ ± 2 conditions, react 18h, promptly obtain LSI;
The solvent that uses in the preparation LSI process is oxolane, xylenes or ethanol.
This embodiment nano-TiO
2Compound material for water treatment has the excellent physical characteristic of siloxane polymer, and impact strength reaches 20.1kJ/m
2, hot strength reaches 65.77MPa, and elongation at break reaches 10.87%, and Tg reaches 172.45 ℃.
The specific embodiment 16: this embodiment nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.24 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment;
Wherein, siloxane polymer is processed by LSI and epoxy resin E-51, with epoxy resin E-51 and the LSI mixed in molar ratio by 85 ︰ 15, under 250 ℃ of conditions, adds thermal condensation then, divides water again, obtains siloxane polymer;
LSI is processed by ethyl orthosilicate and epoxychloropropane; Mol ratio by 82 ︰ 8 is mixed ethyl orthosilicate in the adding solvent with epoxychloropropane; And the weight ratio of pressing siloxane polymer 0.01% adds catalyst formic acid, under 25 ℃ of conditions of temperature, reacts 18h, promptly obtains LSI;
The solvent that uses in the preparation LSI process is oxolane, xylenes or ethanol.
This embodiment nano-TiO
2Compound material for water treatment has the excellent physical characteristic of siloxane polymer, and impact strength reaches 22.4kJ/m
2, hot strength reaches 68.78MPa, and elongation at break reaches 12.42%, and Tg reaches 170.32 ℃.
The nano-TiO of this embodiment preparation
2The XRD test of compound material for water treatment:
Material phase analysis carries out on Japan's motor D of science/max-III Type B X-ray diffractometer.Under the accelerating potential of 40KV, adopt CuK α target emanation, with the velocity scanning of 50/min, powder sample, capture range 2 θ: 10
.-65
。。This embodiment nano-TiO
2The XRD figure of compound material for water treatment is as shown in Figure 1.
The nano-TiO of this embodiment preparation
2The SEM electron-microscope scanning of compound material for water treatment:
Adopt S4700 model Hitachi, Ltd scanning electron microscope analysis instrument, and with sample in vacuum 10
-3～10
-5Carry out gold-plated processing 5min under the condition, as backing material the surface topography of laminated film is observed at metallic film; And style carried out energy spectrum analysis.
Fig. 2 is the nano-TiO of this embodiment preparation
2The SEM electron-microscope scanning figure of compound material for water treatment, multiplication factor is 1000 times.From Fig. 2, can observe the siloxane polymer surface and constitute, and have the hole of some yardsticks, can improve photocatalysis performance by particle and cluster of grains aggressiveness.
The specific embodiment 17: this embodiment with the difference of the specific embodiment 16 is: press different siloxane polymer and TiO in the step 2
2Sol weight ratio joins TiO with siloxane polymer
2In the colloidal sol.Other step and parameter and embodiment ten six phases are together.
The water treatment effect:
Filter water afterwards (i.e. filter back water) with the waterworks, Harbin, as being processed water sample.With nano-TiO
2Compound material for water treatment is placed in the container, will be processed water sample again and pour into wherein, and under the irradiation of ultraviolet lamp, the water after the collection photocatalysis is analyzed TiO
2Photocatalysis water treatment effect (as shown in Figure 3) under colloidal sol and the siloxane polymer Different Weight ratio condition.And in the Harbin City water quality monitoring center is TOC (total content of organic carbon) and is analyzed.Adopt TOC to estimate its effect, total organic carbon is to be used for measuring in the organic components quantity of carbon to represent the index that organic matter pollutes.It comprises in the water all organic summations in the dissolubility and suspension organic matter, but irrelevant with organic existence.
There is not composite Ti O
2Siloxane polymer be 20% as the degradation rate of filtrate degraded TOC, and TiO
2Colloidal sol and siloxane polymer weight ratio are that 0.2～0.3 treatment effect is best, and the TOC degradation rate reaches more than 50%.
Claims (6)
1. nano-TiO
2Compound material for water treatment is characterized in that nano-TiO
2Compound material for water treatment is by siloxane polymer and TiO
2Colloidal sol is processed, TiO
2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO
2The weight ratio of colloidal sol is 1 ︰ 0.2～0.3.
2. nano-TiO according to claim 1
2Compound material for water treatment is characterized in that siloxane polymer processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are (9 ︰ 1)～(8 ︰ 2).
3. nano-TiO according to claim 2
2Compound material for water treatment is characterized in that nano-TiO
2The particle diameter of compound material for water treatment is 1 ~ 2mm.
4. nano-TiO according to claim 1
2The preparation method of compound material for water treatment is characterized in that nano-TiO
2The preparation of compound material for water treatment is carried out according to the following steps:
One, preparation TiO
2Colloidal sol;
Two, press siloxane polymer and TiO
2The weight ratio of colloidal sol 1 ︰ 0.2～0.3 joins TiO with siloxane polymer
2Dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO then naturally
2Be carried on siloxane polymer and promptly obtain nano-TiO
2Compound material for water treatment.
5. nano-TiO according to claim 4
2The preparation method of compound material for water treatment is characterized in that the siloxane polymer in the step 2 is processed by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are (9 ︰ 1)～(8 ︰ 2).
6. nano-TiO according to claim 5
2The preparation method of compound material for water treatment is characterized in that in the step 2 siloxane polymer being added TiO
2Dipping and stir and pour in the spherical module room temperature after 2 hours into and cool off naturally in the colloidal sol promptly obtains the nano-TiO that particle diameter is 1 ~ 2mm
2Compound material for water treatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104759261A (en) * | 2014-01-06 | 2015-07-08 | 中国科学院过程工程研究所 | Titanium dioxide nanometer composite material, and preparation methods and use thereof |
| CN108607522A (en) * | 2018-05-21 | 2018-10-02 | 宁波诺丁汉大学 | Titanium dioxide-multiple-wall carbon nanotube-dimethyl silicone polymer composite functional material and its preparation method and application method |
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| CN101543773A (en) * | 2009-05-07 | 2009-09-30 | 哈尔滨工业大学 | Method for preparing TiO2-fly ash photocatalysis material |
| CN101636079A (en) * | 2006-12-11 | 2010-01-27 | 莫门蒂夫性能材料股份有限公司 | The organically-modified silanization ionic surface active agent of anti-hydrolysis |
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| US20050049158A1 (en) * | 2003-08-29 | 2005-03-03 | Cai Ru Xiong | Coating surface |
| CN101636079A (en) * | 2006-12-11 | 2010-01-27 | 莫门蒂夫性能材料股份有限公司 | The organically-modified silanization ionic surface active agent of anti-hydrolysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104759261A (en) * | 2014-01-06 | 2015-07-08 | 中国科学院过程工程研究所 | Titanium dioxide nanometer composite material, and preparation methods and use thereof |
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| CN108607522A (en) * | 2018-05-21 | 2018-10-02 | 宁波诺丁汉大学 | Titanium dioxide-multiple-wall carbon nanotube-dimethyl silicone polymer composite functional material and its preparation method and application method |
| CN108607522B (en) * | 2018-05-21 | 2020-12-22 | 宁波诺丁汉大学 | Titanium dioxide-multi-walled carbon nanotube-polydimethylsiloxane composite functional material and preparation method and application method thereof |
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