Journal of Textile Research ›› 2023, Vol. 44 ›› Issue (11): 167-175.doi: 10.13475/j.fzxb.20221103501

• Dyeing and Finishing & Chemicals • Previous Articles     Next Articles

Preparation of porous TiO2 particles and their adsorption for ionic dyes

HUANG Biao1, ZHENG Li'na1, QIN Yan1, CHENG Yujun2, LI Chengcai1, ZHU Hailin3, LIU Guojin1()   

  1. 1. Zhejiang Provincial Key Laboratory of Fiber Materials and Manufacturing Technology, Zhejiang Sci-Tech University, Hangzhou, Zhejiang 310018, China
    2. Shaoxing Quality and Technical Supervision and Testing Institute, Shaoxing, Zhejiang 312000, China
    3. Zhejiang Provincial Innovation Center of Advanced Textile Technology, Shaoxing, Zhejiang 312000, China
  • Received:2022-11-11 Revised:2023-08-08 Online:2023-11-15 Published:2023-12-25

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Abstract:

Objective The utilization rate of dyes is unable to reach 100% in practical situations, which inevitably leads to residual dyes in the water discharged after dyeing, causing serious water pollution. Therefore, it is necessary to develop a water treatment technology that can effectively treat dye wastewater. Aiming at the treatment of ionic dyes in printing and dyeing wastewater, porous titana (TiO2) particles were used as adsorbent to adsorb dyes.

Method In addition to the characteristics of stable chemical properties, low price, easy availability, and no toxicity, TiO2 particles also have the unique characteristic of photocatalysis. Therefore, TiO2 particles are often adopted to adsorb and catalyze dyes in wastewater. Through photocatalysis, the dye can be degraded, so that the TiO2 particles can be reused. With tetrabutyl orthotitanate as titanium source, porous TiO2 particles with different potentials were prepared by hydrothermal method using different templates, and then the crystal form of TiO2 particles was controlled by high-temperature calcination. The potential, morphology and crystal form of TiO2 were analyzed by solid surface Zeta potential test, field emission scanning electron microscopy(FETEM), transmission electron microscopy(TEM) and X-ray diffraction (XRD). The dye concentration and adsorbent dosage were optimized by adsorption test, and the reuse performance of TiO2 particles was explored.

Results Positively charged TiO2 particles (G-TiO2) adsorb anionic dyes only other than cationic dyes at all, while the negatively charged TiO2 particles (Y-TiO2) only adsorb cationic dyes other than anionic dyes (Fig. 3 and Fig. 4). The adsorption mechanism follows the electrostatic adsorption mechanism. G-TiO2 has a porous spherical structure formed by the aggregation of numerous particles, about 93% of which are microspheres with a particle size of 200-500 nm. Y-TiO2 is in the state of fine particle aggregation, and about 91% of which are microspheres with a particle size of 50-100 nm (Fig. 6 and Fig. 7). The crystal forms of the two kinds of TiO2 particles after calcination are anatase, which have photocatalytic properties (Fig. 9). Under the same experimental conditions, the adsorption rate of 100 mg/L Congo Red dye by 100 mg G-TiO2 can reach 99.5%, and that of 20 mg/L Methylene Blue dye by 100 mg Y-TiO2 can reach 93.5% (Fig. 11). In the cycle experiment, the adsorption rate of Congo Red dye by G-TiO2 decreased by about 12.6% after four cycles, while that of Methylene Blue dye by Y-TiO2 decreased by about 17% after five cycles (Fig. 13).

Conclusion Two kinds of porous TiO2 particles adsorbents were prepared by changing the type of template in the hydrothermal reaction. The adsorbents not only retain the capillary adsorption of conventional porous TiO2 particles on dyes, but also increase the electrostatic adsorption, which can realize the rapid adsorption of ionic dyes in printing and dyeing wastewater. The adsorbents can be chemically modified subsequently to have improved photocatalytic performance, and can also be loaded on polymer films or nonwovens for specific applications. This study will provide strategic support for the treatment of ionic dye wastewater.

Key words: printing and dyeing wastewater, ionic dye, adsorption treatment, porous, titania microsphere, reuse

CLC Number: 

  • TS179

Fig. 1

Standard curve of Congo Red dye"

Fig. 2

Standard curve of Methylene Blue dye"

Fig. 3

Adsorption rates of adsorbents for different dyes"

Fig. 4

Zeta potential before and after dye adsorption by adsorbents at different pH values"

Fig. 5

Adsorption mechanism of ionic dyes by adsorbents"

Fig. 6

Surface morphologies of adsorbents"

Fig. 7

Particle size distributions of adsorbents"

Fig. 8

Nitrogen gas adsorption/desorption isotherm (a) and pore size distribution (b) of adsorbents"

Tab. 1

Specific surface area, maximum pore size and pore volume of adsorbents"

样品名称 比表面积/
(m2·g-1)		 最可几孔径/
nm		 孔体积/
(mL·g-1)
G-TiO2 74.139 9±0.556 1 16.238 4 0.310 0
Y-TiO2 365.571 6±0.363 8 6.026 9 0.271 5

Fig. 9

Crystal forms of adsorbents before and after calcination"

Fig. 10

Adsorption rates of adsorbents for dyes with different concentrations. (a)Adsorption rate of G-TiO2 for Congo Red dye; (b)Adsorption rate of Y-TiO2 for Methylene Blue dye"

Fig. 11

Adsorption rates of adsorbents for dyes with different dosages. (a) Adsorption rate of G-TiO2 for Congo Red dye; (b)Adsorption rate of Y-TiO2 for Methylene Blue dye"

Fig. 12

Adsorption experiments of dyes by adsorbents. (a) Color changes before and after G-TiO2 adsorption of Congo Red dye; (b) Color changes before and after Y-TiO2 adsorption of Methylene Blue dye"

Fig. 13

Changes of adsorption rates and mass of adsorbent's at different cycles. (a) Adsorption rates of Congo Red dye by G-TiO2 and changes of G-TiO2 mass; (b) Adsorption rates of Methylene Blue dye by Y-TiO2 and changes of Y-TiO2 mass"

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