CN113231106A - Preparation method for loading titanium dioxide nanoflowers on polyester fibers - Google Patents
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- CN113231106A CN113231106A CN202110508925.7A CN202110508925A CN113231106A CN 113231106 A CN113231106 A CN 113231106A CN 202110508925 A CN202110508925 A CN 202110508925A CN 113231106 A CN113231106 A CN 113231106A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000000835 fiber Substances 0.000 title claims abstract description 53
- 229920000728 polyester Polymers 0.000 title claims abstract description 51
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 48
- 239000002057 nanoflower Substances 0.000 title claims abstract description 39
- 238000011068 loading method Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000004108 freeze drying Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000013078 crystal Substances 0.000 abstract description 8
- 238000005406 washing Methods 0.000 abstract description 8
- 238000007710 freezing Methods 0.000 abstract description 6
- 230000008014 freezing Effects 0.000 abstract description 6
- 230000006698 induction Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method for loading titanium dioxide nanoflowers on polyester fibers, which comprises the following steps: 1) mixing 0.1-5 parts (by weight) of polyethylene-polypropylene glycol and 10-50ml of water, and stirring to obtain a solution 1; 2) adding 0.1-3 parts (by weight) of n-butyl titanate into the solution 1, and stirring to obtain a solution 2; 3) adding 10-300 parts (by weight) of polyester fiber into the solution 2, and stirring to obtain a solution 3; 4) carrying out hydrothermal treatment on the solution 3 at the temperature of 110-140 ℃; 5) after cooling, carrying out freeze drying treatment on the solution to obtain mixed solution loaded with titanium dioxide nanoflower polyester fibers; and carrying out centrifugal separation on the mixed solution, and washing to obtain the titanium dioxide nanoflower-loaded polyester fiber. According to the invention, through a freeze drying method in a polyethylene-polypropylene glycol (F-127) specific induction system, titanium dioxide crystal grains are fixed on the surface of the polyester fiber due to solution freezing, and finally the high-dispersity titanium dioxide nanoflower-loaded polyester fiber is obtained.
Description
Technical Field
The invention relates to a preparation method for loading titanium dioxide nanoflowers on polyester fibers.
Background
Titanium dioxide is a common semiconductor photocatalytic material. Under the irradiation of light, the light energy can be converted into chemical energy, and most organic matters including refractory organic matters can be successfully decomposed in a short time. In addition, the paint also has the characteristics of high stability, light corrosion resistance, no toxicity and the like, and does not produce secondary pollution in the treatment process, so that the paint is more and more spotlighted in the fields of antibiosis, deodorization, oil stain decomposition, mildew and algae prevention, air purification and the like.
Since titanium dioxide is a nanoparticle powder, it is necessary to support it on a carrier for practical use. The fibers have a large specific surface and are good carriers. However, in the current loading process, the thermal drying process of the solution which does not contain particles is usually carried out, so that the nano material is agglomerated on the surface of the fiber, the large specific surface area of the original nano material is lost, and finally the integral catalytic activity is sharply reduced.
On the other hand, freeze drying, also called sublimation drying, is a drying method in which a material is frozen below the freezing point of water, placed in a container under high vacuum (10-40 Pa), and the moisture in the material is directly sublimated from solid ice into water vapor by heat supply. Freeze drying utilizes the principle of ice crystal sublimation to sublimate water of frozen materials from ice solids into steam directly without ice melting in a high vacuum environment, so the freeze drying is also called as freeze sublimation drying.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method for loading titanium dioxide nanoflowers on polyester fibers.
The purpose is realized by the following technical scheme:
a preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps:
1) mixing 0.1-5 parts (by weight) of polyethylene-polypropylene glycol and 10-50ml of water, and stirring to obtain a solution 1;
2) adding 0.1-3 parts (by weight) of n-butyl titanate into the solution 1, and stirring to obtain a solution 2;
3) adding 10-300 parts (by weight) of polyester fiber into the solution 2, and stirring to obtain a solution 3;
4) carrying out hydrothermal treatment on the solution 3 at the temperature of 110-140 ℃;
5) and after cooling, carrying out freeze drying treatment on the solution to obtain the mixed solution loaded with the titanium dioxide nanoflower polyester fibers.
Further, the hydrothermal treatment of step 4) is carried out in an autoclave.
Further, carrying out centrifugal separation on the mixed solution obtained in the step 5), and washing the product with ethanol and deionized water to obtain the titanium dioxide nanoflower-loaded polyester fiber.
Further, the control conditions of the freeze-drying treatment in the step 5) are as follows: temperature minus 50-minus 70 ℃, water capturing capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa.
The invention has the beneficial effects that:
1. according to the invention, through a freeze drying method in a polyethylene-polypropylene glycol (F-127) specific induction system, a titanium dioxide crystal grain solution is frozen to be below the freezing point of water, so that titanium dioxide crystal grains are fixed on the surface of polyester fibers due to the freezing of the solution. And then, under the high-vacuum environment, the water content of the frozen titanium dioxide crystal grain solution can be directly sublimated into steam from ice solid without melting ice, so that the problem of agglomeration caused by volume reduction of the solution due to hot drying and evaporation of the solution is avoided, and finally the polyester fiber loaded with the titanium dioxide nanoflowers with high dispersibility is obtained.
2. The titanium dioxide nanoflower structure widens the active surface of catalytic reaction, improves the activity and can save raw materials; the preparation process is relatively simple, the conditions are easy to control, and the method is easy for large-scale industrial production.
Drawings
FIG. 1 is a scanning electron microscope image of polyester fiber loaded with titanium dioxide nanoflower, wherein the size of the drawing is 20 μm.
FIG. 2 is a scanning electron microscope image of the polyester fiber loaded with the titanium dioxide nanoflower, wherein the size of the scale is 2 μm.
FIG. 3 is a scanning electron microscope image of titanium dioxide nanoflowers on polyester fibers, wherein the size of the drawing is 1 μm.
Detailed Description
The present invention will be further described with reference to the following specific examples and accompanying drawings so that those skilled in the art can better understand the technical solutions of the present invention.
Example 1
A preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps: 1) 0.1 part (by weight) of polyethylene-polypropylene glycol and 10ml of water are mixed and stirred for 3 hours to obtain a solution 1;
2) adding 0.1 part (weight ratio) of n-butyl titanate into the solution 1, and stirring for 5 minutes to obtain a solution 2;
3) adding 10 parts (by weight) of polyester fiber into the solution 2, and stirring for 5 minutes to obtain a solution 3, wherein the polyester fiber is commercially available;
4) placing the solution 3 in an autoclave, and treating for 12 hours under the hydrothermal condition of 110 ℃;
5) after cooling, carrying out freeze drying treatment on the solution to obtain a mixed solution loaded with titanium dioxide nanoflower polyester fibers, wherein the control conditions of the freeze drying treatment are that the temperature is 50 ℃ below zero, and the water catching capacity is as follows: 3-4kg/24h, vacuum degree: less than or equal to 5 pa;
and after the mixed solution is subjected to centrifugal separation, washing the resultant with ethanol and deionized water for 3 times to obtain the polyester fiber loaded with the titanium dioxide nanoflowers.
According to the invention, through a freeze drying method in a polyethylene-polypropylene glycol (F-127) specific induction system, a titanium dioxide crystal grain solution is frozen to be below the freezing point of water, so that titanium dioxide crystal grains are fixed on the surface of polyester fibers due to the freezing of the solution. And then, under the high-vacuum environment, the water content of the frozen titanium dioxide crystal grain solution can be directly sublimated into steam from ice solid without melting ice, so that the problem of agglomeration caused by volume reduction of the solution due to hot drying and evaporation of the solution is avoided, and finally the polyester fiber loaded with the titanium dioxide nanoflowers with high dispersibility is obtained.
Referring to fig. 1, a scanning electron microscope image of the polyester fiber loaded with the titanium dioxide nanoflower prepared in the embodiment is shown, and the size of the drawing is 20 μm.
Fig. 2 is a scanning electron microscope image of the polyester fiber loaded with the titanium dioxide nanoflower prepared in the embodiment, and the scale size in the image is 2 μm.
Referring to fig. 3, a scanning electron microscope image of the titanium dioxide nanoflower on the polyester fiber prepared in the embodiment is shown, and the size of the drawing is 1 μm.
Example 2
A preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps:
1) mixing 5 parts by weight of polyethylene-polypropylene glycol and 50ml of water, and stirring for 5 hours to obtain a solution 1;
2) adding 3 parts (by weight) of n-butyl titanate into the solution 1, and stirring for 30 minutes to obtain a solution 2;
3) adding 300 parts (by weight) of polyester fiber into the solution 2, and stirring for 15 minutes to obtain a solution 3;
4) placing the solution 3 in an autoclave, and treating for 48 hours under the hydrothermal condition of 140 ℃;
5) after cooling, the solution is subjected to freeze drying treatment, wherein the control conditions of the freeze drying treatment are as follows: temperature 70 ℃ below zero, water capturing capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa;
and after the mixed solution is subjected to centrifugal separation, washing the resultant with ethanol and deionized water for 3 times to obtain the polyester fiber loaded with the titanium dioxide nanoflowers.
Example 3
A preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps:
1) mixing 3 parts by weight of polyethylene-polypropylene glycol and 30ml of water, and stirring for 4 hours to obtain a solution 1;
2) adding 2 parts (by weight) of n-butyl titanate into the solution 1, and stirring for 15 minutes to obtain a solution 2;
3) adding 150 parts (by weight) of polyester fiber into the solution 2, and stirring for 10 minutes to obtain a solution 3;
4) placing the solution 3 in an autoclave, and treating for 30 hours under the hydrothermal condition of 125 ℃;
5) after cooling, the solution 3 is subjected to freeze-drying treatment under the following control conditions: 60 ℃ below zero, water capture capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa;
and after the mixed solution is subjected to centrifugal separation, washing the resultant with ethanol and deionized water for 3 times to obtain the polyester fiber loaded with the titanium dioxide nanoflowers.
Example 4
A preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps:
1) 0.1 part (by weight) of polyethylene-polypropylene glycol and 50ml of water are mixed and stirred for 3 hours to obtain a solution 1;
2) adding 3 parts (by weight) of n-butyl titanate into the solution 1, and stirring for 5 minutes to obtain a solution 2;
3) adding 10 parts (by weight) of polyester fiber into the solution 2, and stirring for 5 minutes to obtain a solution 3;
4) placing the solution 3 in an autoclave, and treating for 48 hours under the hydrothermal condition of 140 ℃;
5) after cooling, the solution 3 is subjected to freeze-drying treatment under the following control conditions: temperature minus 50 ℃, water capturing capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa;
and after the mixed solution is subjected to centrifugal separation, washing the resultant with ethanol and deionized water for 3 times to obtain the polyester fiber loaded with the titanium dioxide nanoflowers.
Example 5
A preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps:
1) mixing 5 parts by weight of polyethylene-polypropylene glycol and 10ml of water, and stirring for 5 hours to obtain a solution 1;
2) adding 0.1 part (weight ratio) of n-butyl titanate into the solution 1, and stirring for 5 minutes to obtain a solution 2;
3) adding 300 parts (by weight) of polyester fiber into the solution 2, and stirring for 15 minutes to obtain a solution 3;
4) placing the solution 3 in an autoclave, and treating for 12-48 hours under the hydrothermal condition of 110 ℃;
5) after cooling, the solution is subjected to freeze drying treatment, wherein the control conditions of the freeze drying treatment are as follows: temperature 70 ℃ below zero, water capturing capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa;
and after the mixed solution is subjected to centrifugal separation, washing the resultant with ethanol and deionized water for 3 times to obtain the polyester fiber loaded with the titanium dioxide nanoflowers.
Example 6
A preparation method for loading titanium dioxide nanoflowers on polyester fibers comprises the following steps:
1) 5 parts by weight of polyethylene-polypropylene glycol and 10ml of ultrapure water were mixed and stirred for 5 hours to obtain a solution 1;
2) adding 3 parts (by weight) of n-butyl titanate into the solution 1, and stirring for 5 minutes to obtain a solution 2;
3) adding 300 parts (by weight) of polyester fiber into the solution 2, and stirring for 5 minutes to obtain a solution 3;
4) placing the solution 3 in an autoclave, and treating for 12 hours under the hydrothermal condition of 140 ℃;
5) after cooling, the solution is subjected to freeze drying treatment, wherein the control conditions of the freeze drying treatment are as follows: temperature minus 50 ℃, water capturing capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa;
and after the mixed solution is subjected to centrifugal separation, washing the resultant with ethanol and deionized water for 3 times to obtain the polyester fiber loaded with the titanium dioxide nanoflowers.
Claims (4)
1. A preparation method for loading titanium dioxide nanoflowers on polyester fibers is characterized by comprising the following steps:
1) mixing 0.1-5 parts (by weight) of polyethylene-polypropylene glycol and 10-50ml of water, and stirring to obtain a solution 1;
2) adding 0.1-3 parts (by weight) of n-butyl titanate into the solution 1, and stirring to obtain a solution 2;
3) adding 10-300 parts (by weight) of polyester fiber into the solution 2, and stirring to obtain a solution 3;
4) carrying out hydrothermal treatment on the solution 3 at the temperature of 110-140 ℃;
5) and after cooling, carrying out freeze drying treatment on the solution to obtain the mixed solution loaded with the titanium dioxide nanoflower polyester fibers.
2. The method for preparing titanium dioxide nanoflower-loaded polyester fiber by freeze-drying as claimed in claim 1, wherein the hydrothermal treatment of step 4) is performed in an autoclave.
3. The method for preparing titanium dioxide nanoflower-loaded polyester fibers through freeze drying as claimed in claim 2, wherein the mixed solution obtained in step 5) is subjected to centrifugal separation, and the resultant is washed with ethanol and deionized water to obtain the titanium dioxide nanoflower-loaded polyester fibers.
4. The method for preparing titanium dioxide nanoflower-loaded polyester fiber by freeze-drying as claimed in claim 5, wherein the control conditions of the freeze-drying treatment in step 5) are as follows: temperature minus 50-minus 70 ℃, water capturing capacity: 3-4kg/24h, vacuum degree: less than or equal to 5 pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110508925.7A CN113231106A (en) | 2021-05-11 | 2021-05-11 | Preparation method for loading titanium dioxide nanoflowers on polyester fibers |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110508925.7A CN113231106A (en) | 2021-05-11 | 2021-05-11 | Preparation method for loading titanium dioxide nanoflowers on polyester fibers |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001432A (en) * | 2014-04-30 | 2014-08-27 | 上海应用技术学院 | Titanium dioxide/polyvinylidene fluoride composite mesoporous membrane, and preparation method and application thereof |
| WO2014141992A1 (en) * | 2013-03-15 | 2014-09-18 | 株式会社ダイセル | Titanium oxide liquid dispersion, titanium oxide liquid coating, and photocatalyst coating film |
| CN105401404A (en) * | 2015-11-10 | 2016-03-16 | 盐城工学院 | Fabric for treating printing and dyeing wastewater and preparation method of fabric |
| CN105833858A (en) * | 2016-04-28 | 2016-08-10 | 北京科技大学 | Preparation method for two-dimensional carbon film cladding sea urchin-shaped titanium dioxide composite material |
| CN106334585A (en) * | 2016-10-17 | 2017-01-18 | 盐城工学院 | Fabric for treating printing and dyeing wastewater and preparation method thereof |
| CN108435259A (en) * | 2018-03-26 | 2018-08-24 | 江苏奥净嘉环保科技有限公司 | A kind of preparation method of doped nano titanium dioxide polyaniline composite photocatalyst |
| US10987659B1 (en) * | 2020-11-05 | 2021-04-27 | King Abdulaziz University | Synthesis of TiO2/Co3O4 core-shell photocatalysts |
-
2021
- 2021-05-11 CN CN202110508925.7A patent/CN113231106A/en active Pending
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| CN104001432A (en) * | 2014-04-30 | 2014-08-27 | 上海应用技术学院 | Titanium dioxide/polyvinylidene fluoride composite mesoporous membrane, and preparation method and application thereof |
| CN105401404A (en) * | 2015-11-10 | 2016-03-16 | 盐城工学院 | Fabric for treating printing and dyeing wastewater and preparation method of fabric |
| CN105833858A (en) * | 2016-04-28 | 2016-08-10 | 北京科技大学 | Preparation method for two-dimensional carbon film cladding sea urchin-shaped titanium dioxide composite material |
| CN106334585A (en) * | 2016-10-17 | 2017-01-18 | 盐城工学院 | Fabric for treating printing and dyeing wastewater and preparation method thereof |
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Non-Patent Citations (2)
| Title |
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| 王炎: "介孔TiO2的模板法合成及结构修饰研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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