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Nano TiO2 composite water treatment material and preparation method thereof
CN102580710B
China
Description
translated from Chinese
技术领域 technical field
本发明涉及一种纳米复合水处理材料及其制备方法。 The invention relates to a nanocomposite water treatment material and a preparation method thereof.
背景技术 Background technique
纳米TiO2具有光催化效果，可将水中有机物降解成无机物，因此已经被广泛应用于水处理领域。由于纳米材料的在水处理过程中难以回收，所以要与其他材料进行复合后再使用。目前，纳米TiO2与其他材料的复合还仅仅停留在简单共混的水平。由于目前采用共混技术得到的纳米TiO2复合水处理材料无论是纳米TiO2的光催化性能、还是与纳米TiO2进行复合的其他材料的原有特性都大幅降低。 Nano-TiO 2 has a photocatalytic effect and can degrade organic matter in water into inorganic matter, so it has been widely used in the field of water treatment. Since nanomaterials are difficult to recycle in the water treatment process, they must be compounded with other materials before use. At present, the composite of nano-TiO 2 and other materials is only at the level of simple blending. Due to the nano-TiO 2 composite water treatment materials currently obtained by blending technology, both the photocatalytic performance of nano-TiO 2 and the original characteristics of other materials composited with nano-TiO 2 are greatly reduced.
而且现有阶段的纳米TiO2复合水处理材料的制备和研究还主要依靠实验的摸索和经验，并没有一套成熟的可以保留纳米TiO2及复合基体材料特性的纳米TiO2复合水处理材料制备方法，导致纳米TiO2复合水处理材料的设计和研制结果难以统一。 Moreover, the preparation and research of nano-TiO 2 composite water treatment materials at the present stage mainly rely on experimental exploration and experience, and there is no mature nano-TiO 2 composite water treatment material that can retain the properties of nano-TiO 2 and composite matrix materials. method, resulting in nano-TiO 2 composite water treatment materials design and development results are difficult to unify.
发明内容 Contents of the invention
本发明要解决目前纳米TiO2复合水处理材料采用共混技术获得，导致纳米TiO2复合水处理材料的纳米TiO2光催化性能，以及与纳米TiO2进行复合的其他材料的原有特性都大幅降低的问题；并提供一种成熟的可以保留纳米TiO2及复合基体材料特性的纳米TiO2复合水处理材料制备方法。 The present invention solves the problem that the current nano- TiO2 composite water treatment material is obtained by blending technology, resulting in the nano- TiO2 photocatalytic performance of the nano- TiO2 composite water treatment material and the original characteristics of other materials composited with nano- TiO2 . Reduce the problem; and provide a mature method for preparing nano TiO 2 composite water treatment materials that can retain the properties of nano TiO 2 and composite matrix materials.
本发明纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0. 2～0.3。 Nano TiO2 composite water treatment material of the present invention is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on siloxane polymer; Wherein, the weight ratio of siloxane polymer and TiO2 sol is 1:0 . 2～0.3.
上述纳米TiO2复合水处理材料的制备按以下步骤进行： Above-mentioned nanometer TiO The preparation of composite water treatment material is carried out as follows:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶1︰0.2～0.3的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料。 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.2～0.3, add siloxane polymer into TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane Polymer can obtain nanometer TiO 2 composite water treatment material.
本发明的纳米TiO2复合水处理材料不是TiO2和硅氧烷聚合物的简单混合，而是亚微观的有机复合。硅氧烷聚合物本身具有一定的空隙，形成大量的光催化活性中心，同时又将TiO2负载在一定的硅氧烷聚合物材料上；而且，纳米TiO2复合水处理材料在很小的尺度上存在相分离，因此本发明纳米TiO2复合水处理材料的光催化性能大幅提高。 The nano TiO 2 composite water treatment material of the present invention is not a simple mixture of TiO 2 and siloxane polymer, but a submicroscopic organic composite. The siloxane polymer itself has certain gaps, forming a large number of photocatalytic active centers, and at the same time, TiO 2 is loaded on a certain siloxane polymer material; moreover, the nano-TiO 2 composite water treatment material is There is phase separation on the surface, so the photocatalytic performance of the nano-TiO 2 composite water treatment material of the present invention is greatly improved.
本发明纳米TiO2复合水处理材料的制备方法所制备的纳米TiO2复合水处理材料在保持纳米TiO2的光催化性能的同时，保留了硅氧烷聚合物质量轻、性能稳定、可设计性等优点。 The nano- TiO2 composite water treatment material prepared by the preparation method of the nano- TiO2 composite water treatment material of the present invention maintains the photocatalytic performance of the nano -TiO2 while retaining the light weight, stable performance and designability of the siloxane polymer Etc.
因为本发明纳米TiO2复合水处理材料的制备方法可以保留纳米TiO2及复合基体材料特性，所以可按预定性能设计、制备纳米TiO2复合水处理材料，摆脱对材料的研究、设计、制备需要靠经验和摸索的轨迹方法。 Because the preparation method of the nano- TiO2 composite water treatment material of the present invention can retain the characteristics of the nano- TiO2 and the composite matrix material, it can design and prepare the nano- TiO2 composite water-treatment material according to the predetermined performance, and get rid of the need for research, design and preparation of the material The trajectory method based on experience and exploration.
本发明纳米TiO2复合水处理材料可用于处理领域，并具有优异的处理效果。 The nano TiO2 composite water treatment material of the invention can be used in the treatment field and has excellent treatment effect.
附图说明 Description of drawings
图1是具体实施方式十六纳米TiO2复合水处理材料的XRD图。 Fig. 1 is the XRD pattern of the 16nm TiO 2 composite water treatment material according to the specific embodiment.
图2是具体实施方式十六制备的纳米TiO2复合水处理材料的SEM电镜扫描图。 Fig. 2 is the SEM electron microscope scanning picture of the nano-TiO 2 composite water treatment material prepared in Embodiment 16.
图3是具体实施方式十七中TiO2溶胶与硅氧烷聚合物不同重量比值条件下的光催化水处理效果图。 Fig. 3 is a photocatalytic water treatment effect diagram under the condition of different weight ratios of TiO 2 sol and siloxane polymer in the seventeenth embodiment.
具体实施方式 Detailed ways
本发明技术方案不局限于以下所列举具体实施方式，还包括各具体实施方式间的任意组合。 The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
具体实施方式一：本实施方式纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0. 2～0.3。 Embodiment 1: In this embodiment, the nano- TiO2 composite water treatment material is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on the siloxane polymer; wherein, the siloxane polymer and TiO2 sol The weight ratio is 1:0.2～0.3.
具体实施方式二：本实施方式与具体实施方式一的不同点是：硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为（9︰1）～（8︰2）。其它与实施方式一相同。 Specific embodiment two: the difference between this embodiment and specific embodiment one is: the siloxane polymer is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin and chlorine-containing silicone is (9: 1) ~ (8: 2). Others are the same as the first embodiment.
具体实施方式三：本实施方式与具体实施方式一或二的不同点是：纳米TiO2复合水处理材料的粒径为1~2mm。其它与实施方式一或二相同。 Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the particle size of the nano-TiO 2 composite water treatment material is 1-2 mm. Others are the same as the first or second embodiment.
具体实施方式四：本实施方式纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0.21；硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为88︰12。 Specific Embodiment Four: In this embodiment, the nano- TiO2 composite water treatment material is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on the siloxane polymer; wherein, the siloxane polymer and TiO2 sol The weight ratio is 1:0.21; the siloxane polymer is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin and chlorine-containing silicone is 88:12.
具体实施方式五：本实施方式纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0.25；硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为86︰14。 Specific embodiment five: In this embodiment, the nano- TiO2 composite water treatment material is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on the siloxane polymer; wherein, the siloxane polymer and TiO2 sol The weight ratio is 1:0.25; the siloxane polymer is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin and chlorine-containing silicone is 86:14.
具体实施方式六：本实施方式纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0.28；硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为82︰18。 Specific embodiment six: In this embodiment, the nano- TiO2 composite water treatment material is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on the siloxane polymer; wherein, the siloxane polymer and TiO2 sol The weight ratio is 1:0.28; the siloxane polymer is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin to chlorine-containing silicone is 82:18.
具体实施方式七：本实施方式纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0.29；硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为81︰19。 Specific embodiment seven: In this embodiment, the nano- TiO2 composite water treatment material is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on the siloxane polymer; wherein, the siloxane polymer and TiO2 sol The weight ratio is 1:0.29; the siloxane polymer is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin and chlorine-containing silicone is 81:19.
具体实施方式八：本实施方式纳米TiO2复合水处理材料由硅氧烷聚合物和TiO2溶胶制成，TiO2负载于硅氧烷聚合物；其中，硅氧烷聚合物与TiO2溶胶的重量比为1︰0.3；硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为80︰20。 Embodiment 8: In this embodiment, the nano- TiO2 composite water treatment material is made of siloxane polymer and TiO2 sol, and TiO2 is loaded on the siloxane polymer; wherein, the siloxane polymer and TiO2 sol The weight ratio is 1:0.3; the siloxane polymer is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin and chlorine-containing silicone is 80:20.
具体实施方式九：本实施方式纳米TiO2复合水处理材料的制备按以下步骤进行： Specific embodiment nine: the present embodiment nanometer TiO The preparation of composite water treatment material is carried out according to the following steps:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶1︰0.2～0.3的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料。 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.2～0.3, add siloxane polymer into TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane Polymer can obtain nanometer TiO 2 composite water treatment material.
本实施方式具有制备方法简单可行，成本低廉，易于形成产业化。 This embodiment has the advantages of simple and feasible preparation method, low cost and easy industrialization.
具体实施方式十：本实施方式与具体实施方式九的不同点是：步骤二中的硅氧烷聚合物由环氧树脂与含氯有机硅制成；环氧树脂与含氯有机硅的摩尔比为（9︰1）～（8︰2）。其它步骤及参数与实施方式九相同。 Embodiment 10: The difference between this embodiment and Embodiment 9 is: the siloxane polymer in step 2 is made of epoxy resin and chlorine-containing silicone; the molar ratio of epoxy resin to chlorine-containing silicone It is (9:1) ~ (8:2). Other steps and parameters are the same as those in Embodiment 9.
具体实施方式十一：本实施方式与具体实施方式九或十的不同点是：步骤二中将硅氧烷聚合物加入TiO2溶胶中浸渍并搅拌2小时后倒入球型模具中室温自然冷却，即得到粒径为1~2mm的纳米TiO2复合水处理材料。其它步骤及参数与实施方式九或十相同。
Embodiment 11: The difference between this embodiment and
具体实施方式十二：本实施方式纳米TiO2复合水处理材料的制备按以下步骤进行： Embodiment 12: In this embodiment, the nano- TiO2 composite water treatment material is prepared according to the following steps:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶 1︰0.28的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料；其中，硅氧烷聚合物由一氯三甲基硅烷(TMS) 和双酚A型环氧树脂(EP)制成，将双酚A型环氧树脂(EP) 和一氯三甲基硅烷(TMS)按80︰20的摩尔比混合，然后在250±10℃条件下加热缩合，再分水，得到硅氧烷聚合物。 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.28, add siloxane polymer to TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane polymer Promptly obtain nanometer TiO Composite water treatment material; Wherein, siloxane polymer is made by monochlorotrimethylsilane (TMS) and bisphenol A type epoxy resin (EP), bisphenol A type epoxy resin (EP) EP) and chlorotrimethylsilane (TMS) are mixed at a molar ratio of 80:20, then heated and condensed at 250±10°C, and then separated from water to obtain a siloxane polymer.
本实施方式纳米TiO2复合水处理材料具有硅氧烷聚合物的优异物理特性，冲击强度达到20.2kJ/m2，拉伸强度达67.04MPa，断裂伸长率达11.29%，Tg达167.98℃。 The nano-TiO 2 composite water treatment material in this embodiment has excellent physical properties of siloxane polymers, with impact strength up to 20.2kJ/m 2 , tensile strength up to 67.04MPa, elongation at break up to 11.29%, and Tg up to 167.98°C.
具体实施方式十三：本实施方式纳米TiO2复合水处理材料的制备按以下步骤进行： Specific Embodiment Thirteen: In this embodiment, the nano- TiO2 composite water treatment material is prepared according to the following steps:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶 1︰0.24的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料； 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.24, add siloxane polymer to TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane polymer Promptly obtain the nanometer TiO 2 composite water treatment material;
其中，硅氧烷聚合物由二甲基二氯硅烷(DMS) 和双酚A型环氧树脂(EP)制成，将双酚A型环氧树脂(EP) 和二甲基二氯硅烷(DMS)按82︰18的摩尔比混合，然后在250±10℃条件下加热缩合，再分水，得到硅氧烷聚合物。 Among them, the siloxane polymer is made of dimethyldichlorosilane (DMS) and bisphenol A epoxy resin (EP), and bisphenol A epoxy resin (EP) and dimethyldichlorosilane ( DMS) were mixed at a molar ratio of 82:18, then heated and condensed at 250±10°C, and then separated from water to obtain a siloxane polymer.
本实施方式纳米TiO2复合水处理材料具有硅氧烷聚合物的优异物理特性，冲击强度达到20.4kJ/m2，拉伸强度达68.27MPa，Tg达167.98℃。 The nano-TiO 2 composite water treatment material in this embodiment has the excellent physical properties of siloxane polymer, the impact strength reaches 20.4kJ/m 2 , the tensile strength reaches 68.27MPa, and the Tg reaches 167.98°C.
具体实施方式十四：本实施方式纳米TiO2复合水处理材料的制备按以下步骤进行： Embodiment 14: In this embodiment, the nano- TiO2 composite water treatment material is prepared according to the following steps:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶 1︰0.25的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料； 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.25, add siloxane polymer to TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane polymer Promptly obtain the nanometer TiO 2 composite water treatment material;
其中，硅氧烷聚合物由二甲基二氯硅烷、α,ω-二氯聚二甲基硅氧烷(DPS)和双酚A型环氧树脂(EP)制成，将双酚A型环氧树脂(EP) 和二甲基二氯硅烷、α,ω-二氯聚二甲基硅氧烷按81︰1︰18的摩尔比混合，然后在250±10℃条件下加热缩合，再分水，得到硅氧烷聚合物。 Among them, the siloxane polymer is made of dimethyldichlorosilane, α, ω-dichloropolydimethylsiloxane (DPS) and bisphenol A epoxy resin (EP), and the bisphenol A type Epoxy resin (EP) is mixed with dimethyldichlorosilane and α, ω-dichloropolydimethylsiloxane at a molar ratio of 81:1:18, then heated and condensed at 250±10°C, and then Separate water to obtain siloxane polymer.
本实施方式纳米TiO2复合水处理材料具有硅氧烷聚合物的优异物理特性，冲击强度达到31.6kJ/m2，拉伸强度达68.27MPa，断裂伸长率达81.68%，Tg达174.50℃。 The nano-TiO 2 composite water treatment material in this embodiment has excellent physical properties of siloxane polymers, with an impact strength of 31.6kJ/m 2 , a tensile strength of 68.27MPa, an elongation at break of 81.68%, and a Tg of 174.50°C.
具体实施方式十五：本实施方式纳米TiO2复合水处理材料的制备按以下步骤进行： Embodiment 15: In this embodiment, the nano- TiO2 composite water treatment material is prepared according to the following steps:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶 1︰0.25的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料； 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.25, add siloxane polymer to TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane polymer Promptly obtain the nanometer TiO 2 composite water treatment material;
其中，硅氧烷聚合物由LSI和环氧树脂E-44制成，将环氧树脂E-44和LSI按88︰12的摩尔比混合，然后在250±10℃条件下加热缩合，再分水，得到硅氧烷聚合物； Among them, the siloxane polymer is made of LSI and epoxy resin E-44, and the epoxy resin E-44 and LSI are mixed according to the molar ratio of 88:12, and then heated and condensed at 250±10°C, and then separated water to obtain silicone polymers;
LSI由正硅酸乙酯与环氧氯丙烷制成，按（80～85）︰（5～20）的摩尔比将正硅酸乙酯与环氧氯丙烷混合加入溶剂中，并按硅氧烷聚合物0.01%的重量比加入催化剂甲酸，在温度25℃±2条件下反应18h，即得到LSI； LSI is made of tetraethyl orthosilicate and epichlorohydrin. Mix tetraethyl orthosilicate and epichlorohydrin into the solvent according to the molar ratio of (80-85): (5-20), and 0.01% by weight of the alkane polymer is added to the catalyst formic acid, and reacted for 18 hours at a temperature of 25 ° C ± 2 to obtain LSI;
制备LSI过程中使用的溶剂为四氢呋喃、二甲苯或乙醇。 The solvent used in the preparation of LSI is tetrahydrofuran, xylene or ethanol.
本实施方式纳米TiO2复合水处理材料具有硅氧烷聚合物的优异物理特性，冲击强度达到20.1kJ/m2，拉伸强度达65.77MPa，断裂伸长率达10.87%，Tg达172.45℃。 The nano-TiO 2 composite water treatment material in this embodiment has excellent physical properties of siloxane polymers, with impact strength up to 20.1kJ/m 2 , tensile strength up to 65.77MPa, elongation at break up to 10.87%, and Tg up to 172.45°C.
具体实施方式十六：本实施方式纳米TiO2复合水处理材料的制备按以下步骤进行： Specific Embodiment Sixteen: In this embodiment, nano- TiO2 composite water treatment material is prepared according to the following steps:
一、制备TiO2溶胶； 1. Preparation of TiO 2 sol;
二、按硅氧烷聚合物与TiO2溶胶 1︰0.24的重量比将硅氧烷聚合物加入到TiO2溶胶中浸渍并搅拌2小时，然后自然冷却36h，TiO2负载于硅氧烷聚合物即得到纳米TiO2复合水处理材料； 2. According to the weight ratio of siloxane polymer to TiO 2 sol 1:0.24, add siloxane polymer to TiO 2 sol, impregnate and stir for 2 hours, then cool naturally for 36 hours, and TiO 2 is loaded on siloxane polymer Promptly obtain the nanometer TiO 2 composite water treatment material;
其中，硅氧烷聚合物由LSI和环氧树脂E-51制成，将环氧树脂E-51和LSI按85︰15的摩尔比混合，然后在250℃条件下加热缩合，再分水，得到硅氧烷聚合物； Among them, the siloxane polymer is made of LSI and epoxy resin E-51. The epoxy resin E-51 and LSI are mixed in a molar ratio of 85:15, and then heated and condensed at 250°C, and then water is separated. to obtain a siloxane polymer;
LSI由正硅酸乙酯与环氧氯丙烷制成，按82︰8的摩尔比将正硅酸乙酯与环氧氯丙烷混合加入溶剂中，并按硅氧烷聚合物0.01%的重量比加入催化剂甲酸，在温度25℃条件下反应18h，即得到LSI； LSI is made of tetraethyl orthosilicate and epichlorohydrin. Mix tetraethyl orthosilicate and epichlorohydrin into the solvent at a molar ratio of 82:8, and add 0.01% by weight of siloxane polymer Add catalyst formic acid and react for 18 hours at a temperature of 25°C to obtain LSI;
制备LSI过程中使用的溶剂为四氢呋喃、二甲苯或乙醇。 The solvent used in the preparation of LSI is tetrahydrofuran, xylene or ethanol.
本实施方式纳米TiO2复合水处理材料具有硅氧烷聚合物的优异物理特性，冲击强度达到22.4kJ/m2，拉伸强度达68.78MPa，断裂伸长率达12.42%，Tg达170.32℃。 The nano-TiO 2 composite water treatment material in this embodiment has excellent physical properties of siloxane polymers, with impact strength up to 22.4kJ/m 2 , tensile strength up to 68.78MPa, elongation at break up to 12.42%, and Tg up to 170.32°C.
本实施方式制备的纳米TiO2复合水处理材料的XRD试验： The nano TiO prepared by the present embodiment The XRD test of the composite water treatment material:
物相分析在日本理学电机D/max-ⅢB型X射线衍射仪上进行。在40KV的加速电压下，采用CuKα靶辐射，以50/min的速度扫描，粉末样品，收集范围2θ：10。-65。。本实施方式纳米TiO2复合水处理材料的XRD图如图1所示。 Phase analysis was carried out on a Rigaku D/max-ⅢB X-ray diffractometer. Under the acceleration voltage of 40KV, the CuKα target is used to radiate, and the scanning speed is 50/min. The powder sample is collected in the range of 2θ:10 . -65 . . The XRD pattern of the nano-TiO 2 composite water treatment material in this embodiment is shown in FIG. 1 .
本实施方式制备的纳米TiO2复合水处理材料的SEM电镜扫描： The nanometer TiO that present embodiment prepares The SEM scanning electron microscope of composite water treatment material:
采用S4700型号日立公司扫描电镜分析仪器，并将试样在真空10-3～10-5条件下进行镀金处理5min，在金属薄膜作为衬底材料对复合薄膜的表面形貌进行观测；并对式样进行能谱分析。
Using the S4700 model Hitachi scanning electron microscope analysis instrument, the sample was gold-plated for 5 minutes under the condition of
图2是本实施方式制备的纳米TiO2复合水处理材料的SEM电镜扫描图，放大倍数是1000倍。从图2中可以观察到硅氧烷聚合物表面由颗粒和颗粒团聚体构成，并且具有一些尺度的孔洞，可提高光催化性能。 Fig. 2 is a SEM electron microscope scanning image of the nano-TiO 2 composite water treatment material prepared in this embodiment, and the magnification is 1000 times. From Figure 2, it can be observed that the surface of the siloxane polymer is composed of particles and particle aggregates, and has holes of some scales, which can improve the photocatalytic performance.
具体实施方式十七：本实施方式与具体实施方式十六的不同点是：步骤二中按不同的硅氧烷聚合物与TiO2溶胶重量比将硅氧烷聚合物加入到TiO2溶胶中。其它步骤及参数与实施方式十六相同。 Embodiment 17: The difference between this embodiment and Embodiment 16 is that in step 2, the siloxane polymer is added to the TiO 2 sol according to the weight ratio of the siloxane polymer to the TiO 2 sol. Other steps and parameters are the same as those in Embodiment 16.
水处理效果： Water treatment effect:
用哈尔滨自来水厂过滤之后的水（即滤后水），作为被处理水样。将纳米TiO2复合水处理材料放在容器里，再将被处理水样倒入其中，在紫外光灯的照射下，收集光催化后的水，分析TiO2溶胶与硅氧烷聚合物不同重量比值条件下的光催化水处理效果（如图3所示）。并在哈尔滨市水质监测中心做TOC( 总有机碳含量)分析。采用TOC来评价其效果，总有机碳是用来测定有机物成分中碳的数量来表示有机物污染的指标。它包括水中溶解性和悬浮性有机物中所有有机物的总和，但与有机物的存在状态无关。 The water filtered by the Harbin Waterworks (i.e. filtered water) was used as the treated water sample. Put the nano-TiO 2 composite water treatment material in the container, then pour the treated water sample into it, collect the photocatalyzed water under the irradiation of ultraviolet light, and analyze the different weights of TiO 2 sol and siloxane polymer Photocatalytic water treatment effect under ratio conditions (as shown in Figure 3). And do TOC (Total Organic Carbon Content) analysis in Harbin Water Quality Monitoring Center. TOC is used to evaluate its effect, and total organic carbon is an index used to measure the amount of carbon in organic matter components to indicate organic matter pollution. It includes the sum of all organic matter in dissolved and suspended organic matter in water, but has nothing to do with the existing state of organic matter.
没有复合TiO2的硅氧烷聚合物作为滤料降解TOC的降解率为20%，而TiO2溶胶与硅氧烷聚合物重量比值为0.2～0.3的处理效果最好，TOC降解率达到50%以上。 The siloxane polymer without compound TiO 2 is used as a filter material to degrade TOC, and the degradation rate of TOC is 20%, while the treatment effect is the best when the weight ratio of TiO 2 sol to siloxane polymer is 0.2-0.3, and the TOC degradation rate reaches 50%. above.