CN110180520A - A kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material and preparation method thereof - Google Patents

A kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material and preparation method thereof Download PDF

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Publication number
CN110180520A
CN110180520A CN201910379551.6A CN201910379551A CN110180520A CN 110180520 A CN110180520 A CN 110180520A CN 201910379551 A CN201910379551 A CN 201910379551A CN 110180520 A CN110180520 A CN 110180520A
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carbon fiber
carbon
tio
catalysis material
mesoporous carbon
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Inventor
杨艳玲
陈华军
和茹梅
孙瑜
毕雅欣
邹鑫鑫
侯小江
叶晓慧
张荔
朱建锋
冯雷
陈志刚
锁国权
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063Titanium; Oxides or hydroxides thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/58Fabrics or filaments
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Health & Medical Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Toxicology (AREA)
  • Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material includes the following steps: that ethylene glycol is dissolved in acetone by (1), obtains solution A;(2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;(3) butyl titanate is added into suspension B, suspension C is obtained after ultrasonic disperse is uniform;(4) suspension C is transferred to autoclave, and carbon fiber is immersed suspension C, and solvent thermal reaction occurs under magnetic stirring and generates solvent hot D for reactant;(5) solvent hot D through supersound washing and is dried into obtain mesoporous carbon TiO2/ carbon fiber catalysis material.The present invention prepares a kind of recyclable mesoporous carbon@TiO by solvent thermal reaction2/ carbon fiber catalysis material, method is simple and easy, solves the problems, such as that powder photocatalyst is separated and recycled in actual use, opens new approach for light-catalysed industrial applications.

Description

A kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material and preparation method thereof
Technical field
The present invention relates to catalysis materials to synthesize field, and in particular to a kind of recyclable mesoporous carbon@TiO2/ carbon fiber light Catalysis material and preparation method thereof.
Background technique
TiO2Base semiconductor catalysis material shows excellent photocatalysis performance in solar energy photocatalytic field, receives Universal concern is widely used in photocatalysis hydrogen production, CO2Reduction and contaminant degradation field.
But powder TiO2Photochemical catalyst is difficult to separate and recover in actual use, meanwhile, powder TiO2Photocatalysis Agent also brings bigger difficulty to the design of photo catalysis reactor, and the presence of these problems significantly limits TiO2Base semiconductor The industrial applications of catalysis material.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material Preparation method, include the following steps:
(1) ethylene glycol is dissolved in acetone, obtains solution A;
(2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
(3) butyl titanate is added into suspension B, suspension C is obtained after ultrasonic disperse is uniform;
(4) suspension C is transferred to autoclave, and carbon fiber is immersed suspension C, and reactant occurs molten under magnetic stirring Agent thermal response generates solvent hot D;
(5) solvent hot D through supersound washing and is dried into obtain mesoporous carbon TiO2/ carbon fiber catalysis material.
A kind of above-mentioned recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, in step (1): third Ketone and quality of glycol ratio are 2:1 ~ 3:1.
A kind of above-mentioned recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, in step (2): being situated between Hole carbon ball partial size is 200 ~ 400nm.
A kind of above-mentioned recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, which is characterized in that In step (3): butyl titanate and mesoporous carbon spheres mass ratio are 5:1 ~ 20:1.
A kind of above-mentioned recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, in step (4): molten Agent thermal response temperature is 150 ~ 180 DEG C, and the reaction time is 12 ~ 18h, and carbon fiber compactedness is 20 ~ 40%.
A kind of above-mentioned recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, in step (5): logical Supersound washing removal impurity is crossed, mesoporous carbon@TiO is obtained after drying2/ carbon fiber catalysis material.
Technical solution of the present invention obtains following beneficial technical effect:
The present invention prepares a kind of recyclable mesoporous carbon@TiO by solvent thermal reaction2/ carbon fiber catalysis material, method are simple It is easy.
Mesoporous carbon@TiO2/ carbon fiber catalysis material solve powder photocatalyst separate in actual use and The problem of recycling opens new approach for light-catalysed industrial applications.
Detailed description of the invention
Fig. 1 carbon fiber SEM photograph.
Fig. 2 mesoporous carbon@TiO2/ carbon fiber catalysis material SEM photograph.
Fig. 3 mesoporous carbon@TiO2/ carbon fiber catalysis material photomacrograph.
Specific embodiment
Preferred embodiment detailed description is given below in scheme in the present invention to clearly illustrate.
Embodiment 1
A kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, comprising the following steps:
1) ethylene glycol and acetone are uniformly mixed to obtain solution A by 2:1 mass ratio;
2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
3) butyl titanate is added into suspension B, butyl titanate and mesoporous carbon spheres mass ratio are 5:1, and ultrasonic disperse is uniform Suspension C is obtained afterwards;
4) suspension C is transferred to magnetic agitation autoclave, and carbon fiber is immersed suspension C, and carbon fiber compactedness is 20%.Above-mentioned reactant obtains solvent hot D in 150 DEG C of reaction 18h.
5) by product D supersound washing 5s, mesoporous carbon@TiO is obtained afterwards for 24 hours in 80 DEG C of drying2/ carbon fiber catalysis material.
Embodiment 2
A kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, comprising the following steps:
1) ethylene glycol and acetone are uniformly mixed to obtain solution A by 2:1 mass ratio;
2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
3) butyl titanate is added into suspension B, butyl titanate and mesoporous carbon spheres mass ratio are 10:1, and ultrasonic disperse is uniform Suspension C is obtained afterwards;
4) suspension C is transferred to magnetic agitation autoclave, and carbon fiber is immersed suspension C, and carbon fiber compactedness is 30%.Above-mentioned reactant obtains solvent hot D in 160 DEG C of reaction 16h.
5) by product D supersound washing 8s, mesoporous carbon@TiO is obtained after 90 DEG C of drying 18h2/ carbon fiber catalysis material.
Embodiment 3
A kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, comprising the following steps:
1) ethylene glycol and acetone are uniformly mixed to obtain solution A by 3:1 mass ratio;
2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
3) butyl titanate is added into suspension B, butyl titanate and mesoporous carbon spheres mass ratio are 5:1, and ultrasonic disperse is uniform Suspension C is obtained afterwards;
4) suspension C is transferred to magnetic agitation autoclave, and carbon fiber is immersed suspension C, and carbon fiber compactedness is 20%.Above-mentioned reactant obtains solvent hot D in 180 DEG C of reaction 12h.
5) by product D supersound washing 10s, mesoporous carbon@TiO is obtained after 110 DEG C of drying 12h2/ carbon fiber catalysis material.
Embodiment 4
A kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, comprising the following steps:
1) ethylene glycol and acetone are uniformly mixed to obtain solution A by 2:1 mass ratio;
2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
3) butyl titanate is added into suspension B, butyl titanate and mesoporous carbon spheres mass ratio are 20:1, and ultrasonic disperse is uniform Suspension C is obtained afterwards;
4) suspension C is transferred to magnetic agitation autoclave, and carbon fiber is immersed suspension C, and carbon fiber compactedness is 40%.Above-mentioned reactant obtains solvent hot D in 160 DEG C of reaction 15h.
5) by product D supersound washing 8s, mesoporous carbon@TiO is obtained after 100 DEG C of drying 20h2/ carbon fiber catalysis material.
Embodiment 5
A kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, comprising the following steps:
1) ethylene glycol and acetone are uniformly mixed to obtain solution A by 3:1 mass ratio;
2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
3) butyl titanate is added into suspension B, butyl titanate and mesoporous carbon spheres mass ratio are 5:1, and ultrasonic disperse is uniform Suspension C is obtained afterwards;
4) suspension C is transferred to magnetic agitation autoclave, and carbon fiber is immersed suspension C, and carbon fiber compactedness is 25%.Above-mentioned reactant obtains solvent hot D in 170 DEG C of reaction 16h.
5) by product D supersound washing 7s, mesoporous carbon@TiO is obtained after 110 DEG C of drying 15h2/ carbon fiber catalysis material.
Above-described embodiment is only intended to clearly illustrate the invention example, and not specific to the invention The restriction of embodiment.For those of ordinary skill in the art, it can also be made on the basis of the above description Its various forms of variation or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all in essence of the invention Protection of any obvious changes or variations extended out within mind and principle still in the invention claim Among range.

Claims (8)

1. a kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material, which is characterized in that in carbon fiber surface with mesoporous Carbon@TiO2Nano material.
2. a kind of recyclable mesoporous carbon@TiO2The preparation method of/carbon fiber catalysis material, which is characterized in that including walking as follows It is rapid:
Carbon fiber is immersed in the dispersion liquid for being dispersed with mesoporous carbon spheres, butyl titanate, carries out solvent thermal reaction, obtain one kind Recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material.
3. a kind of recyclable mesoporous carbon@TiO according to claim 22The preparation method of/carbon fiber catalysis material, It is characterized in that, the solvent is the mixed solvent that quality of glycol ratio is 2:1 ~ 3:1.
4. a kind of recyclable mesoporous carbon@TiO according to claim 22The preparation method of/carbon fiber catalysis material, It is characterized in that, butyl titanate and carbon ball mass ratio are 5:1 ~ 20:1.
5. a kind of recyclable mesoporous carbon@TiO according to claim 22The preparation method of/carbon fiber catalysis material, It is characterized in that, mesoporous carbon spheres partial size is 200 ~ 400nm.
6. a kind of recyclable mesoporous carbon@TiO according to claim 22The preparation method of/carbon fiber catalysis material, It is characterized in that, solvent thermal reaction temperature is 150 ~ 180 DEG C, and the reaction time is 12 ~ 18h, and carbon fiber compactedness is 20 ~ 40%.
7. a kind of recyclable mesoporous carbon@TiO according to claim 22The preparation method of/carbon fiber catalysis material, It is characterized in that, impurity is removed by supersound washing after the completion of solvent thermal reaction, mesoporous carbon@TiO is obtained after drying2/ carbon fiber light is urged Change material.
8. a kind of recyclable mesoporous carbon@TiO according to claim 22The preparation method of/carbon fiber catalysis material, It is characterized in that, includes the following steps:
1) ethylene glycol is dissolved in acetone, obtains solution A;
2) mesoporous carbon spheres are added in solution A, ultrasonic disperse is uniform to obtain suspension B;
3) butyl titanate is added into suspension B, suspension C is obtained after ultrasonic disperse is uniform;
4) suspension C is transferred to autoclave, and carbon fiber is immersed suspension C, and reactant occurs molten under magnetic stirring Agent thermal response generates solvent hot D;
5) solvent hot D through supersound washing and is dried into obtain mesoporous carbon TiO2/ carbon fiber catalysis material.
CN201910379551.6A 2019-05-08 2019-05-08 A kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material and preparation method thereof Pending CN110180520A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113522262A (en) * 2021-07-15 2021-10-22 陕西科技大学 Recyclable flexible titanium dioxide/pyrolytic carbon/carbon fiber felt composite photocatalytic material and preparation method and application thereof
CN114100598A (en) * 2021-11-29 2022-03-01 洛阳理工学院 Assembling method of Van der Waals heterojunction photocatalysis and photoelectrocatalysis material from bottom to top
PL244171B1 (en) * 2021-10-29 2023-12-11 Univ West Pomeranian Szczecin Tech Method of selective reduction of carbon dioxide to carbon monoxide

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113522262A (en) * 2021-07-15 2021-10-22 陕西科技大学 Recyclable flexible titanium dioxide/pyrolytic carbon/carbon fiber felt composite photocatalytic material and preparation method and application thereof
PL244171B1 (en) * 2021-10-29 2023-12-11 Univ West Pomeranian Szczecin Tech Method of selective reduction of carbon dioxide to carbon monoxide
CN114100598A (en) * 2021-11-29 2022-03-01 洛阳理工学院 Assembling method of Van der Waals heterojunction photocatalysis and photoelectrocatalysis material from bottom to top

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