CN102580710B - Nano TiO2 composite water treatment material and preparation method thereof - Google Patents

Nano TiO2 composite water treatment material and preparation method thereof Download PDF

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CN102580710B
CN102580710B CN 201210074369 CN201210074369A CN102580710B CN 102580710 B CN102580710 B CN 102580710B CN 201210074369 CN201210074369 CN 201210074369 CN 201210074369 A CN201210074369 A CN 201210074369A CN 102580710 B CN102580710 B CN 102580710B
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tio
siloxane polymer
nano
water treatment
colloidal sol
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CN102580710A (en
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鞠春华
范国栋
石玉明
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Harbin Institute of Technology
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Harbin Institute of Technology
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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

Nano-TiO 2Compound material for water treatment and preparation method thereof
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 photocatalysis effect, organic matter degradation in the water can be become inorganic matter, therefore be widely used in water treatment field.Because being difficult in water treatment procedure 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, or and nano-TiO 2The primary characteristic of carrying out compound other materials all significantly reduces.
And the nano-TiO in existing stage 2Compound Water processes material preparation and research also mainly relies on groping and experience of experiment, and a cover maturation can not keep nano-TiO 2And the nano-TiO of compound matrix material characteristic 2Compound Water is processed material 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 Water is processed material preparation method.
Nano-TiO of the present invention 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, 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 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely 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 composite.Siloxane polymer itself has certain space, 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 is separated in very little yardstick existence, so nano-TiO of the present invention 2The photocatalysis performance of compound material for water treatment significantly improves.
Nano-TiO of the present invention 2Compound Water is processed the prepared nano-TiO of material preparation method 2Compound material for water treatment is keeping nano-TiO 2Photocatalysis performance the time, kept the advantages such as the siloxane polymerization amount is light, stable performance, designability.
Because nano-TiO of the present invention 2Compound Water is processed the material preparation method can keep nano-TiO 2And the compound matrix material characteristic, so can design, prepare by pre-determined characteristics nano-TiO 2Compound material for water treatment is broken away from the track method that research, design, preparation to material need to be leaned on experience and be 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 solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: present embodiment nano-TiO 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, 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: the difference of present embodiment and the specific embodiment one is: siloxane polymer is made 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: present embodiment and the specific embodiment one or twos' 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: present embodiment nano-TiO 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, TiO 2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO 2The weight ratio of colloidal sol is 1 ︰ 0.21; Siloxane polymer is made by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 88 ︰ 12.
The specific embodiment five: present embodiment nano-TiO 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, TiO 2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO 2The weight ratio of colloidal sol is 1 ︰ 0.25; Siloxane polymer is made by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 86 ︰ 14.
The specific embodiment six: present embodiment nano-TiO 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, TiO 2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO 2The weight ratio of colloidal sol is 1 ︰ 0.28; Siloxane polymer is made by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 82 ︰ 18.
The specific embodiment seven: present embodiment nano-TiO 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, TiO 2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO 2The weight ratio of colloidal sol is 1 ︰ 0.29; Siloxane polymer is made by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 81 ︰ 19.
The specific embodiment eight: present embodiment nano-TiO 2Compound material for water treatment is by siloxane polymer and TiO 2Colloidal sol is made, TiO 2Be carried on siloxane polymer; Wherein, siloxane polymer and TiO 2The weight ratio of colloidal sol is 1 ︰ 0.3; Siloxane polymer is made by epoxy resin and chloride organosilicon; Epoxy resin and chloride organosilyl mol ratio are 80 ︰ 20.
The specific embodiment nine: present embodiment nano-TiO 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment.
Present embodiment has preparation method's simple possible, and is with low cost, is easy to form industrialization.
The specific embodiment ten: the difference of present embodiment and the specific embodiment nine is: the siloxane polymer in the step 2 is made 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: present embodiment and the specific embodiment nine or tens' 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 naturally cool off in the colloidal sol namely 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: present embodiment nano-TiO 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment; Wherein, siloxane polymer is made 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, then under 250 ± 10 ℃ of conditions, add thermal condensation, divide again water, obtain siloxane polymer.
The present 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%, Tg and reaches 167.98 ℃.
The specific embodiment 13: present embodiment nano-TiO 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is made 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, then under 250 ± 10 ℃ of conditions, add thermal condensation, divide again water, obtain siloxane polymer.
The present 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: present embodiment nano-TiO 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is by dimethyldichlorosilane, α, ω-dichloro dimethyl silicone polymer (DPS) and bisphenol A type epoxy resin (EP) are made, 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, then under 250 ± 10 ℃ of conditions, add thermal condensation, divide again water, obtain siloxane polymer.
The present 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%, Tg and reaches 174.50 ℃.
The specific embodiment 15: present embodiment nano-TiO 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is made by LSI and epoxy resin E-44, with epoxy resin E-44 and the LSI mixed in molar ratio by 88 ︰ 12, then adds thermal condensation under 250 ± 10 ℃ of conditions, divides water again, obtains siloxane polymer;
LSI is made 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, namely obtain LSI;
The solvent that uses in the preparation LSI process is oxolane, dimethylbenzene or ethanol.
The present 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%, Tg and reaches 172.45 ℃.
The specific embodiment 16: present embodiment nano-TiO 2Compound Water is processed material preparation and 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is made by LSI and epoxy resin E-51, with epoxy resin E-51 and the LSI mixed in molar ratio by 85 ︰ 15, then adds thermal condensation under 250 ℃ of conditions, divides water again, obtains siloxane polymer;
LSI is made 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, reacts 18h under 25 ℃ of conditions of temperature, namely obtains LSI;
The solvent that uses in the preparation LSI process is oxolane, dimethylbenzene or ethanol.
The present 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%, Tg and reaches 170.32 ℃.
The nano-TiO of present embodiment preparation 2The XRD test of compound material for water treatment:
Material phase analysis carries out at Rigaku motor D/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 。。The present embodiment nano-TiO 2The XRD figure of compound material for water treatment as shown in Figure 1.
The nano-TiO of present 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, the surface topography of laminated film is observed as backing material at metallic film; And style carried out energy spectrum analysis.
Fig. 2 is the nano-TiO of present 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 be consisted of by particle and cluster of grains aggressiveness, and have the hole of some yardsticks, can improve photocatalysis performance.
The specific embodiment 17: present embodiment from 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 are identical with embodiment 16.
The water treatment effect:
Filter water afterwards (i.e. water after the filter) with the waterworks, Harbin, as processed water sample.With nano-TiO 2Compound material for water treatment is placed in the container, more processed water sample is poured 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 be TOC (total content of organic carbon) at water quality monitoring center, Harbin City and analyze.Adopt TOC to estimate its effect, total organic carbon is to measure the index that the quantity of carbon in the organic components represents Organic Pollution.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 (3)

1. nano-TiO 2Compound material for water treatment is characterized in that described nano-TiO 2Compound material for water treatment is prepared from by 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is by dimethyldichlorosilane, α, ω-dichloro dimethyl silicone polymer and bisphenol A type epoxy resin are made, with bisphenol A type epoxy resin and dimethyldichlorosilane, α, ω-dichloro dimethyl silicone polymer is pressed the mixed in molar ratio of 81:1:18, then under 250 ± 10 ℃ of conditions, add thermal condensation, divide again water, obtain siloxane polymer.
2. nano-TiO 2Compound material for water treatment is characterized in that described nano-TiO 2Compound material for water treatment is prepared from by 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is made by LSI and epoxy resin E-44, and then the mixed in molar ratio with epoxy resin E-44 and LSI press 88:12 adds thermal condensation under 250 ± 10 ℃ of conditions, divide water again, obtains siloxane polymer;
LSI is made by ethyl orthosilicate and epoxychloropropane, press (80～85): the mol ratio of (5～20) is mixed ethyl orthosilicate and is 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, namely obtain LSI;
The solvent that uses in the preparation LSI process is oxolane, dimethylbenzene or ethanol.
3. nano-TiO 2Compound material for water treatment is characterized in that described nano-TiO 2Compound material for water treatment is prepared from by 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 2Then dipping and stirring 2 hours in the colloidal sol cools off 36h, TiO naturally 2Be carried on siloxane polymer and namely obtain nano-TiO 2Compound material for water treatment;
Wherein, siloxane polymer is made by LSI and epoxy resin E-51, and then the mixed in molar ratio with epoxy resin E-51 and LSI press 85:15 adds thermal condensation under 250 ℃ of conditions, divide water again, obtains siloxane polymer;
LSI is made by ethyl orthosilicate and epoxychloropropane, pressing the mol ratio of 82:8 mixes ethyl orthosilicate in the adding solvent with epoxychloropropane, and the weight ratio of pressing siloxane polymer 0.01% adds catalyst formic acid, reacts 18h under 25 ℃ of conditions of temperature, namely obtains LSI;
The solvent that uses in the preparation LSI process is oxolane, dimethylbenzene or ethanol.
CN 201210074369 2012-03-20 2012-03-20 Nano TiO2 composite water treatment material and preparation method thereof Expired - Fee Related CN102580710B (en)

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CN104759261B (en) * 2014-01-06 2018-03-13 中国科学院过程工程研究所 A kind of titanic oxide nano compound material and its production and use
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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US20050049158A1 (en) * 2003-08-29 2005-03-03 Cai Ru Xiong Coating surface
CN101264455A (en) * 2008-04-17 2008-09-17 北京首创纳米科技有限公司 Preparation of photocatalysis coating supported with titanium dioxide under low temperature
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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Publication number Priority date Publication date Assignee Title
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
CN101264455A (en) * 2008-04-17 2008-09-17 北京首创纳米科技有限公司 Preparation of photocatalysis coating supported with titanium dioxide under low temperature
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