CN115121291A - Photocatalytic compound and preparation method thereof - Google Patents

Photocatalytic compound and preparation method thereof Download PDF

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CN115121291A
CN115121291A CN202210954744.1A CN202210954744A CN115121291A CN 115121291 A CN115121291 A CN 115121291A CN 202210954744 A CN202210954744 A CN 202210954744A CN 115121291 A CN115121291 A CN 115121291A
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carrier
spinning
polyacrylonitrile
tio
solution
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易媛
王文广
简思源
李恒超
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Guangdong University of Technology
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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
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
    • B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
    • B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
    • B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
    • 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
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0205—Impregnation in several steps
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341—Irradiation 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
    • B01J37/342—Irradiation 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 electric, magnetic or electromagnetic fields, e.g. for magnetic separation

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Optics & Photonics (AREA)
  • Health & Medical Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Toxicology (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a photocatalytic compound and a preparation method thereof, wherein the photocatalytic compound comprises a carrier and Ag 3 PO 4 ；Ag 3 PO 4 Supported on a carrier comprising TiO 2 The polyacrylonitrile spun fiber of (1); the preparation method comprises the following steps: spinning: spinning with the spinning solution to obtain a carrier; the spinning solution comprises TiO 2 And polyacrylonitrile; the support being a support comprising TiO 2 The polyacrylonitrile spun fiber of (a); and (3) dipping: preparing an impregnation liquid, and impregnating the carrier in the impregnation liquid; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; transferring the carrier fromTaking out the impregnation solution, and then dropwise adding NaH 2 PO 4 Solution, drying the carrier after reaction, Ag 3 PO 4 Loading on a carrier to obtain a photocatalytic compound; the photocatalytic compound has good stability, and Ag 3 PO 4 Tio intimately bonded to spun fibres 2 Effectively stabilize Ag 3 PO 4 Not easy to fall off, high catalysis efficiency and good durability.

Description

Photocatalytic compound and preparation method thereof
Technical Field
The invention relates to a photocatalytic compound and a preparation method thereof, belonging to the technical field of functional reagents.
Background
With the rapid development of the world industrial process, environmental pollution is becoming one of the important problems to be solved urgently. It was discovered since 1967 that single crystal TiO was irradiated with ultraviolet light 2 The electrode can decompose water to generate hydrogen and oxygen, so that a new era of semiconductor photocatalysis and photoelectrocatalysis is opened. The photocatalytic material is a great research hotspot of researchers, and the application of the semiconductor photocatalyst in the purification of organic pollutants is widely concerned in the last decades. Among the numerous photocatalytic materials, titanium dioxide (TiO) 2 ) The photocatalyst is popular with people due to the advantages of high photocatalytic activity, strong oxidizing ability, good light stability, environmental protection, no toxicity, low cost and the like, and is the most researched semiconductor photocatalyst at present. But titanium dioxide (TiO) 2 ) The band gap of the light emitting diode is wide and can only respond under ultraviolet light, so that the light emitting diode has limitation in practical application. Therefore, it has become a necessary trend to find a visible light-responsive photocatalyst having low cost, environmental friendliness and good performance, and it has a profound significance to develop a catalyst having high photocatalytic activity under visible light.
In recent years, a series of Ag-based photocatalysts such as Ag 2 CO 3 And Ag 3 PO 4 And the like show excellent photocatalytic activity when organic pollutants are degraded under the irradiation of visible light. Silver phosphate, as a typical visible light photocatalytic material, has the advantages of high activity and wide photoresponse range, but also has the problem of photo-corrosion. Most of the currently researched photocatalysts exist in a powder state, are difficult to recycle, have poor cycle performance and stability in practical application, and hinder large-scale application of the photocatalysts in the field of photocatalysis.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, a first object of the present invention is to provide a photocatalytic compoundThe compound and the photocatalytic compound have good stability, and Ag 3 PO 4 Tio intimately bonded to spun fibres 2 Effectively stabilize Ag 3 PO 4 Not easy to fall off, high catalysis efficiency and good durability.
The second purpose of the invention is to provide a preparation method of the photocatalytic composite, which can be carried out at room temperature without subsequent calcination treatment, thereby greatly reducing the damage probability to the material.
The first purpose of the invention can be achieved by adopting the following technical scheme: a photocatalytic composite comprises a carrier and Ag 3 PO 4 ；Ag 3 PO 4 Supported on a carrier comprising TiO 2 The polyacrylonitrile spun fiber.
Further, the raw material for preparing the carrier includes TiO 2 Polyacrylonitrile and DMF; TiO 2 2 The mass ratio of the polyacrylonitrile to the polyacrylonitrile is 1 (2-10).
Further, the mass ratio of polyacrylonitrile to DMF is (0.6-2.5): 10.
The second purpose of the invention can be achieved by adopting the following technical scheme: a method of preparing a photocatalytic composite, comprising:
spinning: spinning with the spinning solution to obtain a carrier; the spinning solution comprises TiO 2 And polyacrylonitrile; the support being a support comprising TiO 2 The polyacrylonitrile spun fiber of (a);
and (3) impregnation: preparing an impregnation liquid, and impregnating the carrier in the impregnation liquid; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; taking the carrier out of the impregnation liquid, and then dropwise adding NaH 2 PO 4 Solution, drying the carrier after reaction, Ag 3 PO 4 And loading on a carrier to obtain the photocatalytic compound.
Further, in the spinning step, the preparation method of the spinning solution comprises the following steps: adding TiO into the mixture 2 Adding the powder into N, N-dimethylformamide, stirring, adding polyacrylonitrile powder, and continuously stirring for 10-18h to obtain the spinning solution.
Further, in the spinning step, the spinning solution is spun by an electrostatic spinning machine, an electrode plate connected with the negative electrode is covered by aluminum foil, and the receiving efficiency is 1-4.25g of the spinning solution/h.
Further, in the dipping step, AgNO in the dipping solution 3 The concentration of the N-dimethylformamide is 50-80g/L, and the solvent is N, N-dimethylformamide and deionized water.
Further, the volume ratio of the N, N-dimethylformamide to the deionized water was 1: 3.
Further, in the impregnation step, NaH 2 PO 4 The concentration of the solution is 30-60 g/L.
Further, in the impregnation step, the carrier is washed, frozen and dried after the reaction, and Ag is obtained 3 PO 4 Loading on a carrier to obtain the photocatalytic compound.
Compared with the prior art, the invention has the beneficial effects that:
1. the photocatalytic compound has good stability and Ag 3 PO 4 Tio intimately bonded to spun fibres 2 Effectively stabilize Ag 3 PO 4 The catalyst is not easy to fall off, and has high catalytic efficiency and good durability;
2. the photocatalytic compound takes polyacrylonitrile spinning fiber as a carrier, and the nano-linear microstructure has an ultra-large specific surface area and a loading site and can provide abundant reaction sites in catalytic reaction;
3. the photocatalytic compound takes the spinning fiber as a carrier, provides stable load bearing in the process of preparing the compound, is very simple and convenient to soak and take out in liquid, has simple reaction conditions and convenient recovery, solves the problem that the traditional catalyst powder is difficult to separate and recover, and has good industrial application prospect;
4. the photocatalytic compound has good hydrophilicity, is beneficial to being applied to wastewater purification, can adsorb organic matters in wastewater on the compound, promotes charge transmission in the photocatalytic reaction process, and has high mass transfer efficiency;
5. the photocatalytic composite of the present invention is made of TiO 2 Composite Ag 3 PO 4 As a catalytic substance, can effectively promote lightSeparation of electron-generating holes, improvement of photocatalytic activity, TiO 2 And Ag 3 PO 4 Form a heterojunction by recombination and inhibit Ag 3 PO 4 The photo-corrosion of the material improves the photocatalytic cycle stability of the material;
6. the preparation method of the photocatalytic compound is carried out at room temperature, and calcination treatment is not needed subsequently, so that the damage probability to the material is greatly reduced;
7. the preparation method of the photocatalytic compound adopts an immersion method to ensure that silver ions are fully adsorbed on the surface of the spinning fiber, thereby being beneficial to subsequent deposition of sufficient Ag 3 PO 4 。
Drawings
FIG. 1 is a scanning electron micrograph of a photocatalytic composite;
FIG. 2 is a degradation curve of rhodamine B photocatalytic degradation in example 1.
Detailed Description
The invention will be further described with reference to the accompanying drawings and the detailed description below:
a photocatalytic composite contains carrier and Ag 3 PO 4 ；Ag 3 PO 4 Supported on a carrier comprising TiO 2 The polyacrylonitrile spun fiber of (a); the raw material for preparing the carrier comprises TiO 2 Polyacrylonitrile and DMF; TiO 2 2 The mass ratio of the polyacrylonitrile to the polyacrylonitrile is 1 (2-10); the mass ratio of polyacrylonitrile to DMF is (0.6-2.5): 10.
A method of preparing a photocatalytic composite, comprising:
spinning: spinning the spinning solution by using an electrostatic spinning machine, covering a polar plate connected with a negative electrode by using an aluminum foil, and obtaining a carrier with the receiving efficiency of 1-4.25g of spinning solution/h; the spinning solution comprises TiO 2 And polyacrylonitrile; the support being a support comprising TiO 2 The polyacrylonitrile spun fiber of (1); the preparation method of the spinning solution comprises the following steps: adding TiO into the mixture 2 Adding the powder into N, N-dimethylformamide, stirring, adding polyacrylonitrile powder, and continuously stirring for 10-18h to obtain a spinning solution;
and (3) impregnation: preparing an impregnation liquid, and impregnating the carrier in the impregnation liquid; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; taking the carrier out of the impregnation liquid, and then dropwise adding NaH 2 PO 4 Dissolving, washing the carrier with deionized water, freezing at 0 deg.C or below, vacuum drying in freeze drier, and collecting Ag 3 PO 4 Loading on a carrier to obtain a photocatalytic compound; AgNO in impregnating solution 3 The concentration of the N, N-dimethylformamide is 50-80g/L, and the solvent is N, N-dimethylformamide and deionized water; the volume ratio of the N, N-dimethylformamide to the deionized water is 1: 3; NaH 2 PO 4 The concentration of the solution is 30-60 g/L.
The obtained photocatalytic composite comprises a carrier and Ag 3 PO 4 ；Ag 3 PO 4 Supported on a carrier comprising TiO 2 The scanning electron microscope image of the polyacrylonitrile spinning fiber and the photocatalytic compound is shown in figure 1.
Example 1:
a method of preparing a photocatalytic composite, comprising:
spinning: spinning the spinning solution by using an electrostatic spinning machine, covering a polar plate connected with a negative electrode by using an aluminum foil, wherein the receiving efficiency is 2.196g of the spinning solution/h, and spinning for 6h to obtain a carrier; the spinning solution comprises TiO 2 And polyacrylonitrile; the support being a support comprising TiO 2 The polyacrylonitrile spun fiber of (a); the preparation method of the spinning solution comprises the following steps: adding TiO into the mixture 2 (P25) adding 0.3g of powder into 12mL of N, N-Dimethylformamide (DMF), stirring, adding 1.5g of polyacrylonitrile (PA N) powder, and continuously stirring for 16h to obtain a spinning solution;
and (3) dipping: preparing an impregnation solution, and impregnating the carrier in the impregnation solution for 5 hours; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; taking the carrier out of the impregnation liquid, and then dropwise adding NaH 2 PO 4 Dissolving, washing the carrier with deionized water, freezing at 0 deg.C or below, vacuum drying in freeze drier, and collecting Ag 3 PO 4 Loading on a carrier to obtain a photocatalytic compound; AgNO in impregnating solution 3 The concentration of the N, N-dimethylformamide is 60g/L, and the solvent is 16mL of N, N-dimethylformamide and deionized water; the volume ratio of the N, N-dimethylformamide to the deionized water is 1: 3; NaH 2 PO 4 The concentration of the solution is 50 g-L。
The degradation test of the photocatalytic compound is carried out, and the degradation curve of photocatalytic degradation of rhodamine B is shown in figure 2.
Example 2:
a method of preparing a photocatalytic composite, comprising:
spinning: spinning the spinning solution by using an electrostatic spinning machine, covering a polar plate connected with a negative electrode by using an aluminum foil, wherein the receiving efficiency is 2.13g of spinning solution/h, and spinning for 6h to obtain a carrier; the spinning solution comprises TiO 2 And polyacrylonitrile; the support being a support comprising TiO 2 The polyacrylonitrile spun fiber of (a); the preparation method of the spinning solution comprises the following steps: adding TiO into the mixture 2 (P25) adding 0.2g of powder into 12mL of N, N-Dimethylformamide (DMF), stirring, adding 1.2g of polyacrylonitrile (PA N) powder, and continuously stirring for 16h to obtain a spinning solution;
and (3) impregnation: preparing an impregnation solution, and impregnating the carrier in the impregnation solution for 5 hours; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; taking the carrier out of the impregnation liquid, and then dropwise adding NaH 2 PO 4 Dissolving, washing the carrier with deionized water, freezing at 0 deg.C or below, vacuum drying in freeze drier, and collecting Ag 3 PO 4 Loading on a carrier to obtain a photocatalytic compound; AgNO in impregnating solution 3 The concentration of the N, N-dimethylformamide is 70g/L, and the solvent is 16mL of N, N-dimethylformamide and deionized water; the volume ratio of the N, N-dimethylformamide to the deionized water is 1: 3; NaH (sodium hydroxide) 2 PO 4 The concentration of the solution was 40 g/L.
Example 3:
a method of preparing a photocatalytic composite, comprising:
spinning: spinning the spinning solution by using an electrostatic spinning machine, covering a polar plate connected with a negative electrode by using an aluminum foil, wherein the receiving efficiency is 2.579g of spinning solution/h, and spinning for 6h to obtain a carrier; the spinning solution comprises TiO 2 And polyacrylonitrile; the support being a support comprising TiO 2 The polyacrylonitrile spun fiber of (a); the preparation method of the spinning solution comprises the following steps: adding TiO into the mixture 2 (P25) adding 0.4g of powder into 14mL of N, N-Dimethylformamide (DMF), stirring, adding 1.8g of polyacrylonitrile (PA N) powder, and continuously stirring for 16h to obtain a spinning solution;
and (3) dipping: preparing an impregnation solution, and impregnating the carrier in the impregnation solution for 5 hours; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; taking the carrier out of the impregnation liquid, and then dropwise adding NaH 2 PO 4 Dissolving, washing the carrier with deionized water, freezing at 0 deg.C or below, vacuum drying in freeze drier, and collecting Ag 3 PO 4 Loading on a carrier to obtain a photocatalytic compound; AgNO in impregnating solution 3 The concentration of the N, N-dimethylformamide is 70g/L, and the solvent is 16mL of N, N-dimethylformamide and deionized water; the volume ratio of the N, N-dimethylformamide to the deionized water is 1: 3; NaH (sodium hydroxide) 2 PO 4 The concentration of the solution was 35 g/L.
Various other changes and modifications to the above-described embodiments and concepts will become apparent to those skilled in the art from the above description, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.

Claims (10)

1. A photocatalytic composite comprising a carrier and Ag 3 PO 4 (ii) a The Ag is 3 PO 4 Supported on a carrier comprising TiO 2 The polyacrylonitrile spun fiber.
2. The photocatalytic composite of claim 1, wherein the raw material for preparing the support comprises TiO 2 Polyacrylonitrile and DMF; the TiO is 2 The mass ratio of polyacrylonitrile to polyacrylonitrile is 1 (2-10).
3. The photocatalytic composite as claimed in claim 2, wherein the mass ratio of polyacrylonitrile to DMF is (0.6-2.5): 10.
4. A method for preparing a photocatalytic composite, comprising:
spinning: spinning with the spinning solution to obtain a carrier; the spinning solution comprises TiO 2 And polyacrylonitrile; the carrier is TiO-containing 2 Polyacrylonitrile spinning fiber；
And (3) dipping: preparing an impregnation liquid, and impregnating the carrier in the impregnation liquid; the impregnating solution comprises AgNO 3 And N, N dimethylformamide; taking the carrier out of the impregnation liquid, and then dropwise adding NaH 2 PO 4 Solution, drying the carrier after reaction, Ag 3 PO 4 And loading on a carrier to obtain the photocatalytic compound.
5. The method for preparing a photocatalytic composite as set forth in claim 4, wherein the spinning solution is prepared by: adding TiO into the mixture 2 Adding the powder into N, N-dimethylformamide, stirring, adding polyacrylonitrile powder, and continuously stirring for 10-18h to obtain the spinning solution.
6. The method of claim 4, wherein the spinning solution is spun using an electrostatic spinning machine, and the plate connected to the negative electrode is covered with aluminum foil at a receiving efficiency of 1 to 4.25g spinning solution/h.
7. The method of claim 4, wherein in the impregnating step, the AgNO in the impregnating solution is 3 The concentration of (A) is 50-80g/L, and the solvent is N, N dimethylformamide and deionized water.
8. The method of claim 7, wherein the volume ratio of the N, N-dimethylformamide to the deionized water is 1: 3.
9. The method of claim 4, wherein in the step of impregnating, the NaH is added to the solution 2 PO 4 The concentration of the solution is 30-60 g/L.
10. The method of claim 4, wherein the impregnation step comprises washing, freezing and drying the support after the reaction, and the Ag is 3 PO 4 And loading on a carrier to obtain the photocatalytic compound.
CN202210954744.1A 2022-08-10 2022-08-10 Photocatalytic compound and preparation method thereof Pending CN115121291A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104383947A (en) * 2014-11-11 2015-03-04 浙江理工大学 Silver phosphate/titanium dioxide nanocomposite and preparation method thereof
CN105056980A (en) * 2015-09-01 2015-11-18 中国计量学院 Ag3PO4/TiO2 nanotube array composite photocatalyst and preparation method thereof
CN108251970A (en) * 2018-01-23 2018-07-06 苏州大学 TiO2The preparation method of/PAN nanofiber membrane
CN112973744A (en) * 2021-02-03 2021-06-18 华北电力大学 Novel photoelectric catalyst and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104383947A (en) * 2014-11-11 2015-03-04 浙江理工大学 Silver phosphate/titanium dioxide nanocomposite and preparation method thereof
CN105056980A (en) * 2015-09-01 2015-11-18 中国计量学院 Ag3PO4/TiO2 nanotube array composite photocatalyst and preparation method thereof
CN108251970A (en) * 2018-01-23 2018-07-06 苏州大学 TiO2The preparation method of/PAN nanofiber membrane
CN112973744A (en) * 2021-02-03 2021-06-18 华北电力大学 Novel photoelectric catalyst and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈超等: "静电纺丝制备TiO2/PAN纳米纤维毡及其性能研究" *

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Application publication date: 20220930