WO2019051734A1 - 一种TiO2毛细管整体柱的制备方法 - Google Patents

一种TiO2毛细管整体柱的制备方法 Download PDF

Info

Publication number
WO2019051734A1
WO2019051734A1 PCT/CN2017/101791 CN2017101791W WO2019051734A1 WO 2019051734 A1 WO2019051734 A1 WO 2019051734A1 CN 2017101791 W CN2017101791 W CN 2017101791W WO 2019051734 A1 WO2019051734 A1 WO 2019051734A1
Authority
WO
WIPO (PCT)
Prior art keywords
parts
same
water
preparation
capillary
Prior art date
Application number
PCT/CN2017/101791
Other languages
English (en)
French (fr)
Inventor
季春柳
Original Assignee
季春柳
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 季春柳 filed Critical 季春柳
Publication of WO2019051734A1 publication Critical patent/WO2019051734A1/zh

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof

Definitions

  • the invention particularly relates to a method for preparing a TiO 2 capillary monolithic column.
  • Photocatalysis can directly use solar energy as a light source to drive the reaction, which is an ideal environmental pollution control technology.
  • semiconductor TiO 2 is widely used in photocatalytic degradation of organic pollutants, solar cells, gas sensors and photolysis of water to produce hydrogen.
  • the carrier can be generally classified into metal, glass, ceramic, etc., and these carriers are mostly made of SiO 2 , such as glass and silica gel, and also molecular sieve, stainless steel, titanium plate and activated carbon.
  • SiO 2 such as glass and silica gel
  • molecular sieve such as stainless steel
  • titanium plate and activated carbon titanium plate and activated carbon.
  • a physical coating film is relatively common, such as a immersion pulling method, a rotary coating method, and a gravity casting method, but the film is easily peeled off due to a weak physical effect. It is difficult to recycle.
  • the invention discloses a preparation method of a TiO 2 capillary monolithic column, comprising the steps of: taking a capillary having a length of 30 cm and an inner diameter of 500 ⁇ m, injecting a 1 mol/L NaOH solution into a syringe, sealing the two ends with a rubber stopper, and activating the 2-4 h in a water bath at 45-55 ° C; Rinse the pH to 6.5-7.5 with deionized water, then rinse off the water on the inner wall with absolute ethanol, dry at 110-120 ° C for 1-2 h; 20-30 parts of absolute ethanol, 0.5-1.5 parts of glacial acetic acid and 1 - 3 parts of TBOT mixed uniformly to obtain solution A, 15-25 parts of absolute ethanol, 30-40 parts of water and 3-7 parts of PEG are mixed uniformly to obtain solution B; under magnetic stirring, solution A is added dropwise to solution B, and drops After the addition is completed, the mixture is stirred for 20-40 min, injected into the activated
  • the preparation method it is activated under a water bath at 50 ° C for 3 h.
  • the pH is washed to 7 by deionized water.
  • the preparation method it is dried at 115 ° C for 1.5 h.
  • the rubber stopper is capped and placed in a 45 ° C water bath for 4 h.
  • the temperature is raised to 480 ° C for 10 h at 10 ° C / min.
  • the method provided by the invention has simple operation, and the prepared TiO 2 capillary monolithic column has good catalytic effect, and after repeated use for many times, the film peels off less, and secondary pollution to the environment is avoided.
  • the invention discloses a preparation method of a TiO 2 capillary monolithic column, comprising the steps of: taking a capillary having a length of 30 cm and an inner diameter of 500 ⁇ m, injecting a 1 mol/L NaOH solution into a syringe, sealing the two ends with a rubber stopper, and activating for 3 hours under a water bath at 50 ° C, deionized water Rinse the pH to 7, then rinse off the water on the inner wall with absolute ethanol, and dry at 115 ° C for 1.5 h; mix 25 parts of absolute ethanol, 1 part of glacial acetic acid and 2 parts of TBOT to obtain a solution A, 20 parts of absolute ethanol.
  • solution B 35 parts of water and 5 parts of PEG are mixed uniformly to obtain solution B; under magnetic stirring, solution A is added dropwise to solution B, and after stirring, stirring is continued for 30 minutes, and it is injected into the activated capillary column, and sealed with a rubber stopper. After the end, it was placed in a 45 ° C water bath for 4 h, and then the unreacted sol was blown out with a syringe, dried in a 115 ° C drying oven for 4 h, then placed in a muffle furnace for calcination, and heated to 480 ° C at 10 ° C / min. 6h, cooled to room temperature; each raw material is part by weight.
  • a preparation method of a TiO 2 capillary monolithic column comprises the following steps: taking a capillary having a length of 30 cm and an inner diameter of 500 ⁇ m, injecting a 1 mol/L NaOH solution into a syringe, sealing the two ends with a rubber stopper, and activating the water bath at 45 ° C for 2 hours, deionized water Rinse the pH to 6.5, then rinse off the water on the inner wall with absolute ethanol, and dry at 110 ° C for 1 h; mix 20 parts of absolute ethanol, 0.5 parts of glacial acetic acid and 1 part of TBOT to obtain a solution A, 15 parts of absolute ethanol, 30 parts of water and 3 parts of PEG were mixed to obtain solution B.
  • solution A was added dropwise to solution B. After the addition was completed, stirring was continued for 20 minutes, and the mixture was poured into an activated capillary column and capped with a rubber stopper. After being placed in a 40 ° C water bath for 3 h, the unreacted sol was blown out with a syringe, dried in a drying oven at 110 ° C for 3 h, then placed in a muffle furnace for calcination, and heated at 10 ° C / min to 460 ° C for 5 h. It is obtained by cooling to room temperature; each raw material is part by weight.
  • a preparation method of a TiO 2 capillary monolithic column comprises the following steps: taking a capillary having a length of 30 cm and an inner diameter of 500 ⁇ m, injecting a 1 mol/L NaOH solution into a syringe, sealing the two ends with a rubber stopper, and activating the water bath at 55 ° C for 4 hours, deionized water Rinse the pH to 7.5, then rinse off the water on the inner wall with absolute ethanol, and dry at 120 ° C for 2 h; mix 30 parts of absolute ethanol, 1.5 parts of glacial acetic acid and 3 parts of TBOT to obtain a solution A, 25 parts of absolute ethanol, 40 parts of water and 7 parts of PEG were mixed to obtain solution B; under the stirring of force, solution A was added dropwise to solution B, and after stirring, stirring was continued for 40 minutes, and it was injected into the activated capillary column and capped with a rubber stopper.
  • the unreacted sol was blown out with a syringe, dried in a drying oven at 120 ° C for 5 h, then placed in a muffle furnace for calcination, and heated at 10 ° C / min to 500 ° C for 7 h. It is obtained by cooling to room temperature; each raw material is part by weight.
  • the method provided by the invention has simple operation, and the prepared TiO 2 capillary monolithic column has good catalytic effect, and after repeated use for many times, the film peels off less, and secondary pollution to the environment is avoided.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

一种TiO 2毛细管整体柱的制备方法，步骤如下：取长30cm、内径500μm的毛细管，注入NaOH溶液，封闭两端，水浴活化，去离子水冲洗，无水乙醇去除水，110-120℃下干燥；将20-30份无水乙醇、0.5-1.5份冰醋酸和1-3份TBOT混匀得溶液A，15-25份无水乙醇、30-40份水和3-7份PEG混匀得溶液B；磁力搅拌下将A滴加到B中，继续搅拌，注入毛细管柱中，封端后放入40-50℃水浴中3-5h，干燥，再放入马弗炉中以10℃/min升温到460-500℃保温5-7h，冷却即得。该方法操作简单，制得的薄膜催化效果好。

Description

一种TiO2毛细管整体柱的制备方法 技术领域
本发明具体涉及一种TiO2毛细管整体柱的制备方法。
背景技术
随着全球工业化的发展，环境污染问题日益严重，尤其是水和空气中的有机物污染是目前最难解决的问题之一。光催化可直接利用太阳能作为光源来驱动反应，是一种理想的环境污染治理技术。半导体TiO2作为一种重要的光催化剂，广泛应用于光催化降解有机污染物、太阳能电池、气敏传感器和光解水制氢等领域。
在当前的TiO2光催化体系中，粉体和薄膜是研究最多的两种形态。粉体虽然比表面积高、量子产率大、光催化效率高，但反应后易团聚、难以分离和回收，极大地限制了其在工业方面的应用。近年来，以溶胶-凝胶法为基础的TiO2薄膜制备方法成为光催化剂的研究热点。考虑到薄膜容易碎裂，需要将其负载在稳定性高且能够与之有较强的物理或化学键合作用的载体上。载体一般可分为金属类、玻璃类和陶瓷类等，这些载体多以SiO2为原料，如玻璃和硅胶，另外还有分子筛、不锈钢、钛板和活性炭等。目前在以溶胶-凝胶法为基础制备二氧化钛薄膜的方法中，物理涂膜较为普遍，如浸渍提拉法、旋转涂膜法和重力铸造法等，但由于物理作用较弱，薄膜容易脱落，难以循环使用。
发明内容
本发明的目的在于提供一种TiO2毛细管整体柱的制备方法。
本发明通过下面技术方案实现：
一种TiO2毛细管整体柱的制备方法，包括如下步骤：取长30cm、内径500μm的毛细管，用注射器注入1mol/L的NaOH溶液，橡皮塞封闭两端，45-55℃水浴下活化2-4h，去离子水冲洗PH至6.5-7.5，再用无水乙醇冲洗掉内壁上的水，110-120℃下干燥1-2h；将20-30份无水乙醇、0.5-1.5份冰醋酸和1-3份TBOT混合均匀得溶液A，15-25份无水乙醇、30-40份水和3-7份PEG混合均匀得溶液B；磁力搅拌下，将溶液A滴加到溶液B中，滴加完毕后继续搅拌20-40min，将其注入活化好的毛细管柱中，用橡皮塞封端后放入40-50℃水浴中反应3-5h，再用注射器吹出未反应完的溶胶，放入110-120℃干燥箱中干燥3-5h，再放入马弗炉中煅烧，以10℃/min升温到460-500℃保温5-7h，冷却至室温即得；各原料均为重量份。
优选地，所述的制备方法中，50℃水浴下活化3h。
优选地，所述的制备方法中，去离子水冲洗PH至7。
优选地，所述的制备方法中，115℃下干燥1.5h。
优选地，所述的制备方法中，橡皮塞封端后放入45℃水浴中反应4h。
优选地，所述的制备方法中，以10℃/min升温到480℃保温6h。
本发明技术效果：
本发明提供的方法操作简单，制得的TiO2毛细管整体柱催化效果好，循环使用多次后，薄膜脱落较少，避免了对环境的二次污染。
具体实施方式
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种TiO2毛细管整体柱的制备方法，包括如下步骤：取长30cm、内径500μm的毛细管，用注射器注入1mol/L的NaOH溶液，橡皮塞封闭两端，50℃水浴下活化3h，去离子水冲洗PH至7，再用无水乙醇冲洗掉内壁上的水，115℃下干燥1.5h；将25份无水乙醇、1份冰醋酸和2份TBOT混合均匀得溶液A，20份无水乙醇、35份水和5份PEG混合均匀得溶液B；磁力搅拌下，将溶液A滴加到溶液B中，滴加完毕后继续搅拌30min，将其注入活化好的毛细管柱中，用橡皮塞封端后放入45℃水浴中反应4h，再用注射器吹出未反应完的溶胶，放入115℃干燥箱中干燥4h，再放入马弗炉中煅烧，以10℃/min升温到480℃保温6h，冷却至室温即得；各原料均为重量份。
实施例2
一种TiO2毛细管整体柱的制备方法，包括如下步骤：取长30cm、内径500μm的毛细管，用注射器注入1mol/L的NaOH溶液，橡皮塞封闭两端，45℃水浴下活化2h，去离子水冲洗PH至6.5，再用无水乙醇冲洗掉内壁上的水，110℃下干燥1h；将20份无水乙醇、0.5份冰醋酸和1份TBOT混合均匀得溶液A，15份无水乙醇、30份水和3份PEG混合均匀得溶液B；磁力搅拌下，将溶液A滴加到溶液B中，滴加完毕后继续搅拌20min，将其注入活化好的毛细管柱中，用橡皮塞封端后放入40℃水浴中反应3h，再用注射器吹出未反应完的溶胶，放入110℃干燥箱中干燥3h，再放入马弗炉中煅烧，以10℃/min升温到460℃保温5h，冷却至室温即得；各原料均为重量份。
实施例3
一种TiO2毛细管整体柱的制备方法，包括如下步骤：取长30cm、内径500μm的毛细管，用注射器注入1mol/L的NaOH溶液，橡皮塞封闭两端，55℃水浴下活化4h，去离子水冲洗PH至7.5，再用无水乙醇冲洗掉内壁上的水，120℃下干燥2h；将30份无水乙醇、1.5份冰醋酸和3份TBOT混合均匀得溶液A，25份无水乙醇、40份水和7份PEG混合均匀得溶液B；磁力搅拌下，将溶液A滴加到溶液B中，滴加完毕后继续搅拌40min，将其注入活化好 的毛细管柱中，用橡皮塞封端后放入50℃水浴中反应5h，再用注射器吹出未反应完的溶胶，放入120℃干燥箱中干燥5h，再放入马弗炉中煅烧，以10℃/min升温到500℃保温7h，冷却至室温即得；各原料均为重量份。
本发明提供的方法操作简单，制得的TiO2毛细管整体柱催化效果好，循环使用多次后，薄膜脱落较少，避免了对环境的二次污染。

Claims (6)

  1. 一种TiO2毛细管整体柱的制备方法，其特征在于包括如下步骤：取长30cm、内径500μm的毛细管，用注射器注入1mol/L的NaOH溶液，橡皮塞封闭两端，45-55℃水浴下活化2-4h，去离子水冲洗PH至6.5-7.5，再用无水乙醇冲洗掉内壁上的水，110-120℃下干燥1-2h；将20-30份无水乙醇、0.5-1.5份冰醋酸和1-3份TBOT混合均匀得溶液A，15-25份无水乙醇、30-40份水和3-7份PEG混合均匀得溶液B；磁力搅拌下，将溶液A滴加到溶液B中，滴加完毕后继续搅拌20-40min，将其注入活化好的毛细管柱中，用橡皮塞封端后放入40-50℃水浴中反应3-5h，再用注射器吹出未反应完的溶胶，放入110-120℃干燥箱中干燥3-5h，再放入马弗炉中煅烧，以10℃/min升温到460-500℃保温5-7h，冷却至室温即得；各原料均为重量份。
  2. 根据权利要求1所述的制备方法，其特征在于：50℃水浴下活化3h。
  3. 根据权利要求1所述的制备方法，其特征在于：去离子水冲洗PH至7。
  4. 根据权利要求1所述的制备方法，其特征在于：115℃下干燥1.5h。
  5. 根据权利要求1所述的制备方法，其特征在于：橡皮塞封端后放入45℃水浴中反应4h。
  6. 根据权利要求1所述的制备方法，其特征在于：以10℃/min升温到480℃保温6h。
PCT/CN2017/101791 2017-09-14 2017-09-15 一种TiO2毛细管整体柱的制备方法 WO2019051734A1 (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201710825559 2017-09-14
CN201710825559.1 2017-09-14

Publications (1)

Publication Number Publication Date
WO2019051734A1 true WO2019051734A1 (zh) 2019-03-21

Family

ID=65723160

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2017/101791 WO2019051734A1 (zh) 2017-09-14 2017-09-15 一种TiO2毛细管整体柱的制备方法

Country Status (1)

Country Link
WO (1) WO2019051734A1 (zh)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101318128A (zh) * 2008-07-23 2008-12-10 天津大学 锐钛矿结构的高光催化活性纳米TiO2的制备方法
CN101503211A (zh) * 2008-02-04 2009-08-12 中国科学院合肥物质科学研究院 二氧化钛纳米孔阵列薄膜及其制备方法
CN101513609A (zh) * 2009-03-27 2009-08-26 苏州科技学院 一种用于水处理的光催化剂及其制备和应用
WO2010036520A1 (en) * 2008-09-26 2010-04-01 Wisconsin Alumni Research Foundation Mesoporous metal oxide materials for phosphoproteomics
CN104528821A (zh) * 2014-12-29 2015-04-22 柳州邦诚科技有限公司 纳米二氧化钛的制备方法
CN104645960A (zh) * 2013-11-20 2015-05-27 李志刚 复合二氧化钛碳纳米管的制备方法
CN106238027A (zh) * 2016-07-02 2016-12-21 北京化工大学 纳米TiO2毛细管柱的制备方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101503211A (zh) * 2008-02-04 2009-08-12 中国科学院合肥物质科学研究院 二氧化钛纳米孔阵列薄膜及其制备方法
CN101318128A (zh) * 2008-07-23 2008-12-10 天津大学 锐钛矿结构的高光催化活性纳米TiO2的制备方法
WO2010036520A1 (en) * 2008-09-26 2010-04-01 Wisconsin Alumni Research Foundation Mesoporous metal oxide materials for phosphoproteomics
CN101513609A (zh) * 2009-03-27 2009-08-26 苏州科技学院 一种用于水处理的光催化剂及其制备和应用
CN104645960A (zh) * 2013-11-20 2015-05-27 李志刚 复合二氧化钛碳纳米管的制备方法
CN104528821A (zh) * 2014-12-29 2015-04-22 柳州邦诚科技有限公司 纳米二氧化钛的制备方法
CN106238027A (zh) * 2016-07-02 2016-12-21 北京化工大学 纳米TiO2毛细管柱的制备方法

Similar Documents

Publication Publication Date Title
CN103086613B (zh) 一种增透自洁镀膜玻璃的制备方法
CN101973582B (zh) 一种制备密度可调的TiO2纳米棒阵列的方法
CN107837817A (zh) 一种碳点/氮化碳/二氧化钛复合材料及其制备方法和应用
CN106745226A (zh) 基于低共熔溶剂合成的微纳二氧化钛和制备方法及应用
CN102019176B (zh) 一种用玄武岩纤维负载的TiO2光催化膜的制备方法
CN110026173A (zh) 纳米ZnO/TiO2复合光催化剂及其制备方法和应用
CN105905940B (zh) 一种钛酸镍/二氧化钛复合纳米材料的制备方法
CN104402197A (zh) 一种低含水量石英玻璃体材料制备方法
CN104722326A (zh) 一种CuS/g-C3N4纳米球花复合物催化剂的制备方法
CN104310466B (zh) 一种基于凝胶球前驱体的中空二氧化钛微球及其制备方法
CN104785232A (zh) 陶瓷负载高活性纳米二氧化钛薄膜的低温制备方法
WO2020147777A1 (zh) 一种选择性吸光材料的新用途及新型光热系统
CN104998629A (zh) 一种核-壳结构SiO2-TiO2复合纳米材料及其制备方法和应用
CN110292920A (zh) 锆掺杂二氧化铈多孔小球的制备方法
WO2019051734A1 (zh) 一种TiO2毛细管整体柱的制备方法
CN113101932A (zh) 微波-紫外光催化剂的制备方法及应用
CN104211071A (zh) 一种CdS@SiO2纳米复合材料的合成方法
CN108285174B (zh) 一种WO3-ZrO2光催化污水处理膜的制备方法
CN107020072A (zh) 一种高粘附高分散的二氧化钛光催化薄膜的制备方法
CN103332870A (zh) 一种纳米二氧化钛薄膜的制备方法
CN106316151A (zh) 一种纳米TiO2薄膜电极的制备方法
CN103816856B (zh) 用于降解水中微量有机污染物的材料及其制备方法和应用
CN103230791B (zh) 一种异质结结构纳米光催化材料的制备方法
CN103521270A (zh) 磺化煤负载二氧化钛光催化剂及其制备方法
CN101856609B (zh) 海绵钛负载TiO2光催化剂及其制备方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17925330

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 17925330

Country of ref document: EP

Kind code of ref document: A1

32PN Ep: public notification in the ep bulletin as address of the adressee cannot be established

Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 112(1) EPC (EPO FORM 1205A DATED 29/09/2020).

122 Ep: pct application non-entry in european phase

Ref document number: 17925330

Country of ref document: EP

Kind code of ref document: A1