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CN109853223A - A kind of TiO2The preparation method of-rGo composite self-cleaning fabric - Google Patents

A kind of TiO2The preparation method of-rGo composite self-cleaning fabric Download PDF

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Publication number
CN109853223A
CN109853223A CN201811651063.8A CN201811651063A CN109853223A CN 109853223 A CN109853223 A CN 109853223A CN 201811651063 A CN201811651063 A CN 201811651063A CN 109853223 A CN109853223 A CN 109853223A
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Prior art keywords
titanium dioxide
graphene oxide
tio
preparation
cleaning fabric
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CN201811651063.8A
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Chinese (zh)
Inventor
谢燕
方曼
姜雨淋
朱裕平
纪耀
康彦琳
沈雪婷
高大伟
王春霞
祁珍明
王丽丽
钱玉
陈郯
牛力恒
东汤春
章学如
朱河山
贝新宇
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Yangcheng Institute of Technology
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Yangcheng Institute of Technology
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Abstract

The invention discloses a kind of TiO2The preparation method of-rGo composite self-cleaning fabric, includes the following steps: step 1, prepares titanium dioxide-redox graphene dispersion liquid;Step 2, after fabric being cleaned out, ultraviolet light irradiation handles 20 ~ 40 min;Step 3, step 2 treated fabric is immersed containing in step 1 gained titanium dioxide-redox graphene dispersion liquid finishing fluid, 20 ~ 40 min of ultrasound, then 50 ~ 120 s of setting treatment to get.The composite self-cleaning fabric self-cleaning effect that the present invention obtains is excellent, and process is simple, it is easy to accomplish industrialization is suitable for promoting the use of.

Description

A kind of TiO2The preparation method of-rGo composite self-cleaning fabric
Technical field
The invention belongs to function fabric technical fields, and in particular to a kind of TiO2The preparation side of-rGo composite self-cleaning fabric Method.
Background technique
Titanium dioxide (TiO2) wide due to having with chemical stability height and the characteristics such as environmental-friendly in photocatalysis field General application value.Under the conditions of existing for the Guang Heshui, TiO2To the pernicious gas in air such as nitrogen oxides, formaldehyde, toluene There is very strong killing effect Deng with very strong degradation and to bacterium.Meanwhile TiO2With very strong ultraviolet radiation absorption Ability can substantially reduce invasion of the ultraviolet light to high molecular material, reduce the generation of living radical, and protection materials are not ultraviolet Line is degraded.Therefore, TiO2The performances such as the excellent automatically cleaning of fabric, antibacterium and antiultraviolet can be assigned.
Graphene or redox graphene (GO) Yin have good electric conductivity and chemical stability, in conjunction with special list Atomic layer planar structure and its high-specific surface area, frequently as nano particle carrier material and be widely used.Aoxidize stone Black alkene is the important presoma for preparing redox graphene.
Currently, the research about TiO2 and redox graphene compound is concentrated mainly on TiO2 nano particle and reduction The simple physical of graphene oxide mixes, and since TiO2 nano particle is easy to reunite on redox graphene, it hinders Direct effect between the two, reduces the synergistic effect between redox graphene and TiO2 nano particle significantly.
Summary of the invention
For the deficiency of existing issue, the object of the present invention is to provide a kind of TiO2The preparation of-rGo composite self-cleaning fabric Method.
The technical solution used to solve the technical problems of the present invention is that:
A kind of TiO2The preparation method of-rGo composite self-cleaning fabric, includes the following steps:
Step 1, titanium dioxide-redox graphene dispersion liquid is prepared;
Step 2, after fabric being cleaned out, ultraviolet light irradiation handles 20~40min;
Step 3, step 2 treated fabric is immersed and is dispersed containing step 1 gained titanium dioxide-redox graphene In the finishing fluid of liquid, 20~40min of ultrasound, then 50~120s of setting treatment to get.
Wherein, the step 1 comprises the following specific steps that:
(1) graphite oxide olefinic substance is dispersed in water, ultrasound obtains graphene oxide dispersion;
(2) titanium dioxide is added in graphene oxide dispersion made from step (1), is stirred, ultrasound is centrifuged, and is done It is dry, obtain graphene oxide-loaded titania powder solid product;
(3) titania powder solid product graphene oxide-loaded made from step (2) is added into water, then plus Enter reducing agent, move into reaction kettle, 140~180 DEG C, hydro-thermal reaction 12~for 24 hours, then through washing, centrifugation, it is dry after, obtain two Titanium oxide-redox graphene composite material;
(4) water is added to titanium dioxide made from step (3)-redox graphene composite material, ultrasonic disperse obtains two Titanium oxide-redox graphene dispersion liquid.
As the optimal technical scheme of the application, in the step (1), the concentration of graphene oxide dispersion is 0.05%-0.5%.
As the optimal technical scheme of the application, in the step (2), titanium dioxide is metal-doped titanium dioxide, non- The binary doped titanium dioxide of metal-doped titanium dioxide, metal-non-metal, metal-non-metal-metal ternary doping titanium dioxide Titanium.
Preferably, in the step (2), metal-doped titanium dioxide be Sb is titania-doped, Sb is titania-doped, La is titania-doped, Zr is titania-doped or Fe is titania-doped.
Preferably, in the step (2), nonmetal doping titanium dioxide is that N is titania-doped or S adulterates titanium dioxide Titanium.
Preferably, in the step (2), the binary doped titanium dioxide of metal-non-metal be Sb-N it is titania-doped, La-N is titania-doped, Fe-N is titania-doped, Fe-S is one or both of titania-doped.
Preferably, in the step (2), metal-non-metal-metal ternary doping titanium dioxide is Sb-N-Zr doping two Titanium oxide or La-N-Fe are titania-doped.
As the optimal technical scheme of the application, in the step (3), reducing agent is ammonium hydroxide;Ammonium hydroxide additional amount and oxidation Graphene-supported titania powder solid product mass ratio is 1~4:1, titanium dioxide-graphene oxide composite material Mass concentration is 1~10%.
As the optimal technical scheme of the application, oxygen reduction fossil in titanium dioxide-redox graphene composite material The mass ratio of black alkene and titanium dioxide is 1-5:5-1.
As the optimal technical scheme of the application, in the finishing fluid of the step 3, titanium dioxide-redox graphene The additional amount of dispersion liquid is the 1~5% of finishing fluid gross mass.
As the optimal technical scheme of the application, the temperature of the setting treatment is 140~160 DEG C, pre- before setting treatment Drying, the temperature of prebake are 70~90 DEG C, and the time is 40~80min.
Beneficial effect
TiO provided by the invention2The preparation method of-rGo composite self-cleaning fabric has following compared with prior art The utility model has the advantages that
(1) redox graphene is added during the preparation process, as TiO2Carrier, promote TiO2Dispersibility with One property;
(2) TiO in finishing fluid of the present invention2Close interfacial contact is formd with redox graphene, promotes photoproduction electricity The separation of son-hole, improves TiO2Photocatalytic activity, further increase the automatically cleaning efficiency of fabric;
(3) titanium dioxide selection metal, nonmetal doping titanium dioxide or the metal-non-metal binary that the present invention selects Titania-doped, test discovery self-cleaning effect is substantially better than titanium dioxide;
(4) find that self-cleaning fabrics first carry out ultraviolet irradiation processing before arrangement in preparation process of the present invention, for knitting The automatically cleaning efficiency of object is obviously improved.
Specific embodiment
The present invention is described in further details with reference to embodiments.Production is not specified in agents useful for same or instrument and equipment Manufacturer, it is accordingly to be regarded as the conventional products that can be bought by market.
Embodiment 1:
A kind of preparation method of TiO2-rGo composite self-cleaning fabric, includes the following steps:
Step 1, titanium dioxide-redox graphene dispersion liquid is prepared;
Step 2, after fabric being cleaned out, ultraviolet light irradiation handles 20min;
Step 3, step 2 treated fabric is immersed and is dispersed containing step 1 gained titanium dioxide-redox graphene In the finishing fluid of liquid, titanium dioxide-redox graphene dispersion liquid additional amount is the 1% of finishing fluid gross mass, ultrasound 20min, then setting treatment 50s, the temperature of setting treatment are 140 DEG C, and prebake before setting treatment, the temperature of prebake is 70 DEG C, time 80min.To obtain the final product.
Wherein, the step 1 comprises the following specific steps that:
(1) graphite oxide olefinic substance is dispersed in water, ultrasound obtains graphene oxide dispersion, wherein graphite oxide The concentration of alkene dispersion liquid is 0.05%;
(2) it is added to Sb is titania-doped in graphene oxide dispersion made from step (1), stirs, ultrasound, from The heart, it is dry, obtain graphene oxide-loaded titania powder solid product;
(3) titania powder solid product graphene oxide-loaded made from step (2) is added into water, then plus Enter ammonium hydroxide, ammonium hydroxide additional amount is that graphene oxide-loaded titania powder solid product mass ratio is 1:4, moves into reaction Kettle, 140 DEG C of hydro-thermal reaction 12h obtain titanium dioxide-redox graphene composite wood then after washing, centrifugation, drying Expect, wherein the mass ratio 1:1 of reduction-oxidation graphene oxide and titanium dioxide;
(4) water is added to titanium dioxide made from step (3)-redox graphene composite material, mass concentration is 1%, ultrasonic disperse obtains titanium dioxide-redox graphene dispersion liquid.
Embodiment 2
A kind of preparation method of TiO2-rGo composite self-cleaning fabric, includes the following steps:
Step 1, titanium dioxide-redox graphene dispersion liquid is prepared;
Step 2, after fabric being cleaned out, ultraviolet light irradiation handles 40min;
Step 3, step 2 treated fabric is immersed and is dispersed containing step 1 gained titanium dioxide-redox graphene In the finishing fluid of liquid, titanium dioxide-redox graphene dispersion liquid additional amount is the 5% of finishing fluid gross mass, ultrasound 40min, then setting treatment 120s, the temperature of setting treatment are 160 DEG C, and prebake before setting treatment, the temperature of prebake is 90 DEG C, time 40min.
To obtain the final product.
Wherein, the step 1 comprises the following specific steps that:
(1) graphite oxide olefinic substance is dispersed in water, ultrasound obtains graphene oxide dispersion, wherein graphite oxide The concentration of alkene dispersion liquid is 0.5%;
(2) it is added to La-N is titania-doped in graphene oxide dispersion made from step (1), stirs, ultrasound, Centrifugation, it is dry, obtain graphene oxide-loaded titania powder solid product;
(3) titania powder solid product graphene oxide-loaded made from step (2) is added into water, then plus Enter ammonium hydroxide, ammonium hydroxide additional amount and graphene oxide-loaded titania powder solid product mass ratio are 1~1, move into reaction Kettle, 180 DEG C, hydro-thermal reaction for 24 hours, then after washing, centrifugation, drying, obtains titanium dioxide-redox graphene composite wood Material, wherein the mass ratio of redox graphene and titanium dioxide is 5:1;
(4) water is added to titanium dioxide made from step (3)-redox graphene composite material, mass concentration is 10%, ultrasonic disperse obtains titanium dioxide-redox graphene dispersion liquid.
Embodiment 3
A kind of preparation method of TiO2-rGo composite self-cleaning fabric, includes the following steps:
Step 1, titanium dioxide-redox graphene dispersion liquid is prepared;
Step 2, after fabric being cleaned out, ultraviolet light irradiation handles 30min;
Step 3, step 2 treated fabric is immersed and is dispersed containing step 1 gained titanium dioxide-redox graphene In the finishing fluid of liquid, titanium dioxide-redox graphene dispersion liquid additional amount is the 1~5% of finishing fluid gross mass, ultrasound 25min, then setting treatment 100s, the temperature of setting treatment are 150 DEG C, and prebake before setting treatment, the temperature of prebake is 85 DEG C, time 60min.To obtain the final product.
Wherein, the step 1 comprises the following specific steps that:
(1) graphite oxide olefinic substance is dispersed in water, ultrasound, obtains graphene oxide dispersion, graphene oxide point The concentration of dispersion liquid is 0.2%;
(2) the titania-doped titanium dioxide of Sb-N-Zr is added to graphene oxide dispersion made from step (1) In, stirring, ultrasound is centrifuged, and it is dry, obtain graphene oxide-loaded titania powder solid product;
(3) titania powder solid product graphene oxide-loaded made from step (2) is added into water, then plus Enter ammonium hydroxide, ammonium hydroxide additional amount and graphene oxide-loaded titania powder solid product mass ratio are 2:1, move into reaction Kettle, 140~180 DEG C, hydro-thermal reaction 12~for 24 hours, then after washing, centrifugation, drying, obtain titanium dioxide-oxygen reduction fossil Black alkene composite material, the mass ratio of redox graphene and titanium dioxide is 1:5 in composite material;
(4) water is added to titanium dioxide made from step (3)-redox graphene composite material, mass concentration is 5%, ultrasonic disperse obtains titanium dioxide-redox graphene dispersion liquid.
As the optimal technical scheme of the application, the temperature of the setting treatment is 140~160 DEG C, pre- before setting treatment Drying, the temperature of prebake are 70~90 DEG C, and the time is 40~80min.
Embodiment 4
Except titanium dioxide is that N is titania-doped, other raw materials and method are the same as embodiment 3.
Embodiment 5
Except titanium dioxide is that W is titania-doped, other raw materials and method are the same as embodiment 2.
Embodiment 6
Except titanium dioxide is that Sb-N is titania-doped, other raw materials and method are the same as embodiment 1.
Embodiment 7
Except titanium dioxide is that La is titania-doped, other raw materials and method are the same as embodiment 3.
Comparative example 1
Titanium dioxide-redox graphene dispersion liquid is not added in finishing fluid, other raw materials and method are the same as embodiment 3.
Comparative example 2
It is not added with redox graphene in finishing fluid, only adds titanium dioxide, other raw materials and method are the same as embodiment 3.
Performance test
As can be seen from the above table, the degradation effect of PARA FORMALDEHYDE PRILLS(91,95) of the present invention is significant, and the removal rate of methane is 90% or more.
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with the attached claims be protection Range.

Claims (8)

1.一种TiO2-rGo复合自清洁织物的制备方法,其特征在于,包括如下步骤:1. a preparation method of TiO 2 -rGo composite self-cleaning fabric, is characterized in that, comprises the steps: 步骤1,制备二氧化钛-还原氧化石墨烯分散液;Step 1, preparing titanium dioxide-reduced graphene oxide dispersion; 步骤2,将织物清理干净后,紫外光辐照处理20~40 min;Step 2, after the fabric is cleaned, irradiated with ultraviolet light for 20-40 min; 步骤3,将步骤2处理后的织物浸入含有步骤1所得二氧化钛-还原氧化石墨烯分散液的整理液中,超声20~40 min,再定型处理50~120 s,即得。In step 3, the fabric treated in step 2 is immersed in the finishing solution containing the titanium dioxide-reduced graphene oxide dispersion obtained in step 1, ultrasonicated for 20-40 min, and then shaped for 50-120 s. 2.根据权利要求1所述的TiO2-rGo复合自清洁织物的制备方法,其特征在于,所述步骤1包括如下具体步骤:2. The preparation method of TiO 2 -rGo composite self-cleaning fabric according to claim 1, wherein the step 1 comprises the following specific steps: (1)将氧化石墨烯物质分散在水中,超声,得到氧化石墨烯分散液;(1) Dispersing the graphene oxide material in water, ultrasonically, to obtain a graphene oxide dispersion; (2)将二氧化钛加入到步骤(1)制得的氧化石墨烯分散液中,搅拌,超声,离心,干燥,得到氧化石墨烯负载的二氧化钛粉末固体产物;(2) adding titanium dioxide to the graphene oxide dispersion liquid obtained in step (1), stirring, ultrasonicating, centrifuging, and drying to obtain a graphene oxide-supported titanium dioxide powder solid product; (3)将步骤(2)制得的氧化石墨烯负载的二氧化钛粉末固体产物加入至水中,再加入还原剂,移入反应釜,140~180℃,水热反应12~24 h,然后经水洗、离心、干燥后,得到二氧化钛-还原氧化石墨烯复合材料;(3) The graphene oxide-supported titanium dioxide powder solid product obtained in step (2) is added to water, then a reducing agent is added, and then transferred to a reactor, 140~180 ° C, hydrothermal reaction for 12~24 h, and then washed with water, After centrifugation and drying, the titanium dioxide-reduced graphene oxide composite material is obtained; (4)向步骤(3)制得的二氧化钛-还原氧化石墨烯复合材料加入水,超声分散,得二氧化钛-还原氧化石墨烯分散液。(4) adding water to the titanium dioxide-reduced graphene oxide composite material obtained in step (3), and ultrasonically dispersing to obtain a titanium dioxide-reduced graphene oxide dispersion liquid. 3.根据权利要求2所述的TiO2-rGo复合自清洁织物的制备方法,其特征在于,所述步骤(1)中,氧化石墨烯分散液的浓度为0.05%-0.5%。3 . The method for preparing a TiO 2 -rGo composite self-cleaning fabric according to claim 2, wherein in the step (1), the concentration of the graphene oxide dispersion liquid is 0.05%-0.5%. 4.根据权利要求2所述的TiO2-rGo复合自清洁织物的制备方法,其特征在于,所述步骤(2)中,二氧化钛为N掺杂二氧化钛、Sb掺杂二氧化钛、La掺杂二氧化钛或Sb-N掺杂二氧化钛、La-N掺杂二氧化钛中的一种或两种。4 . The preparation method of TiO 2 -rGo composite self-cleaning fabric according to claim 2, wherein in the step (2), the titanium dioxide is N-doped titanium dioxide, Sb-doped titanium dioxide, La-doped titanium dioxide or One or both of Sb-N-doped titanium dioxide and La-N-doped titanium dioxide. 5.根据权利要求2所述的TiO2-rGo复合自清洁织物的制备方法,其特征在于,所述步骤(3)中,还原剂为氨水;氨水加入量与氧化石墨烯负载的二氧化钛粉末固体产物质量比为1~4:1,所述步骤(4)中,二氧化钛-还原氧化石墨烯复合材料的质量浓度为1~10%。5. The preparation method of TiO 2 -rGo composite self-cleaning fabric according to claim 2, wherein in the step (3), the reducing agent is ammonia water; the addition amount of ammonia water and the titanium dioxide powder solid supported by graphene oxide The product mass ratio is 1-4:1, and in the step (4), the mass concentration of the titanium dioxide-reduced graphene oxide composite material is 1-10%. 6.根据权利要求2所述的TiO2-rGo复合自清洁织物的制备方法,其特征在于,二氧化钛-还原氧化石墨烯复合材料中还原氧化石墨烯和二氧化钛的质量比为1-5:5-1。6. the preparation method of TiO 2 -rGo composite self-cleaning fabric according to claim 2, is characterized in that, in the titanium dioxide-reduced graphene oxide composite material, the mass ratio of reduced graphene oxide and titanium dioxide is 1-5: 5- 1. 7.根据权利要求1所述的TiO2-rGo复合自清洁织物的制备方法,其特征在于,所述步骤3的整理液中,二氧化钛-还原氧化石墨烯分散液的加入量为整理液总质量的1~5%。7. the preparation method of TiO 2 -rGo composite self-cleaning fabric according to claim 1, is characterized in that, in the finishing liquid of described step 3, the add-on of titanium dioxide-reduced graphene oxide dispersion liquid is finishing liquid gross mass 1~5% of . 8. 根据权利要求1所述的TiO2-rGO复合自清洁织物的制备方法,其特征在于,所述定型处理的温度为140~160 ℃,定型处理前预烘干,预烘干的温度为70~90 ℃,时间为40~80min。8. the preparation method of TiO 2 -rGO composite self-cleaning fabric according to claim 1, is characterized in that, the temperature of described shaping treatment is 140~160 ℃, pre-drying before shaping treatment, the temperature of pre-drying is 70~90 ℃, the time is 40~80min.
CN201811651063.8A 2018-12-31 2018-12-31 A kind of TiO2The preparation method of-rGo composite self-cleaning fabric Pending CN109853223A (en)

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