CN114100693A - Nano CuO/Cu2O-cotton fabric composite material and preparation method and application thereof - Google Patents

Nano CuO/Cu2O-cotton fabric composite material and preparation method and application thereof Download PDF

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Publication number
CN114100693A
CN114100693A CN202111145262.3A CN202111145262A CN114100693A CN 114100693 A CN114100693 A CN 114100693A CN 202111145262 A CN202111145262 A CN 202111145262A CN 114100693 A CN114100693 A CN 114100693A
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cuo
cotton fabric
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composite material
cuso
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苏秀平
陈爽爽
徐巧
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Shaoxing University Yuanpei College
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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
    • B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Toxicology (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
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Abstract

The invention relates to the technical field of photocatalytic materials, and discloses nano CuO/Cu2An O-cotton fabric composite material, a preparation method and application thereof. The composite material is Cu2O hybridized CuO nano particle modified cotton fabric, Cu2The O hybridized CuO nano particle structure is Cu2O coated CuO particles and Cu2The O-hybridized CuO nano-particles are attached to the surface of cotton fiber and used for degrading organic dye under visible light. The invention has high catalytic efficiency under visible light; CuO/Cu loaded on cotton fabric2The firmness of the O nano particles is high; low cost and repeated use.

Description

Nano CuO/Cu2O-cotton fabric composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to nano CuO/Cu2An O-cotton fabric composite material, a preparation method and application thereof.
Background
The cotton fabric is an ideal environment-friendly material, has the characteristics of being green, sustainable, low in price and the like, and is easily polluted by organic pollutants and bacteria. The cotton fabric can be derived from plants, bacteria and marine shellfish, and has the advantages of degradability, flexibility, hydrophilicity, abundant surface groups and the like. The cotton fabric can be used as an interface bridge between an inorganic nano material and a high polymer material, is an ideal choice for the interface chemistry of composite materials, and develops the photocatalytic degradation of organic pollutants and antibacterial performanceThe textile cloth has wide application prospect. Meanwhile, sewage treatment is an important subject of the current society, and the development of a high-efficiency photocatalyst capable of sterilizing and degrading organic matters is very key, so that the catalyst can be used in the field of photocatalytic degradation for treating water pollution. At present, most of mature technologies are titanium dioxide, the titanium dioxide only has a photocatalysis effect after being irradiated by ultraviolet light, the ultraviolet light is easy to generate light pollution, and the development of a clean visible light high-efficiency illumination self-cleaning technology is a green and environment-friendly trend. Cu is abundant in nature, has low price compared with Ti, and is suitable for mass synthesis. Cuprous oxide can play the role of sterilization and microorganism degradation under the action of illumination, and the cuprous oxide has the function of promoting the visible light catalysis efficiency of cuprous oxide nanoparticles and the mutual synergistic effect. The cotton cloth can enrich the pollutants, and is beneficial to the light treatment and decomposition after the pollutants are enriched, so that the cotton fabric is loaded with nano CuO/Cu2O is a new photocatalyst development direction. However, the CuO/Cu is loaded on the cotton fabric2The firmness of the O nanoparticles is low, and the catalytic efficiency still needs to be improved.
The grant number CN106978715B discloses a textile cloth composite material with photocatalysis and antibacterial properties, which is a composite material of sheet AgBr/ZnO/BiOBr loaded on textile cloth, and is formed by attaching BiOBr nano sheets to the surfaces of textile cloth fibers, wherein ZnO and AgBr nano particles are loaded on the BiOBr nano sheets. However, the raw material is relatively expensive silver.
Disclosure of Invention
In order to solve the technical problem, the invention provides nano CuO/Cu2O-cotton fabric composite material, preparation method and application thereof, and has high catalytic efficiency under visible light, and CuO/Cu loaded on cotton fabric2The O nano particles have the characteristics of high firmness and low cost, and can be repeatedly used.
The specific technical scheme of the invention is as follows: nano CuO/Cu2The O-cotton fabric composite material is Cu2O hybridized CuO nano particle modified cotton fabric, Cu2The O hybridized CuO nano particle structure is Cu2O coated CuO particles and Cu2O-hybridized CuO nanoparticlesThe particles adhere to the surface of the cotton fibers.
Under the heating condition, copper ions in the reaction system are easier to generate copper oxide firstly, and part of bivalent copper ions in the copper oxide are reduced into cuprous oxide nano particles under the action of a reducing agent and are attached to the surfaces of the cupric oxide nano particles to form the hybrid particles of the cupric oxide and the cuprous oxide. The cotton cloth is loaded with the multi-type valence hybrid nano-particles, namely Cu is formed2O/CuO nanoparticle composite, Cu2The O @ CuO nano particles are attached to the surface of the cotton fiber, and the surface of the cotton fiber attached with cuprous oxide hybridized copper oxide nano particles plays a role in concerted catalysis and increasing the catalytic efficiency. The organic dye on the surface of the fabric is repeatedly adsorbed and degraded under the illumination of visible light, and the fabric has a stable photocatalytic self-cleaning effect.
The invention also discloses the nano CuO/Cu2The preparation method of the O-cotton fabric composite material comprises the following steps:
(1) cotton fabric pretreatment: soaking in alkali liquor, cleaning, and drying;
(2) nano CuO/Cu2O-cotton fabric composite material: placing cotton fabric in CuSO4Adding a protective agent into the solution, adjusting the pH value to 11.5-12.5, then adding a reducing agent, reacting at 55-65 ℃, cleaning and drying after the reaction is finished to obtain the nano CuO/Cu2An O-cotton fabric composite; the mass ratio of the cotton fabric to the copper sulfate in the solution is 1: 0.008-0.024.
The method firstly uses alkali liquor to pretreat the cotton fabric, activates the surface of the fiber and provides conditions for Cu ion adsorption. Then adding a protective agent, wherein the existence of the protective agent can improve the pre-factor of the catalytic reaction and promote the reduction of copper ions. The cupric sulfate solution generates copper hydroxide floccule under the alkaline condition, and when the oxidation-reduction reaction does not occur, under the heating condition of the reaction system, copper ions are easier to be firstly generated into cupric oxide, and the divalent copper ions in the other part of cuprous oxide are reduced into cuprous oxide nano-particles under the action of a reducing agent. Attached to the surface of the copper oxide particles to form hybrid particles of copper oxide and cuprous oxide. Adjusting the pH value of the solution, adding a reducing agent, and adding part of Cu2+Reduction to Cu+. In the present invention, Cu2O is synthesized in situ on cotton fabric, and the cotton fabric is used as a bridge to lead Cu2The O is dispersed very uniformly and is not easy to fall off, and the composite material is easy to reuse by using cotton fabric as a base material. The composite material has the advantages of simple preparation method, high speed, low energy consumption, high efficiency, no toxicity and the like.
Preferably, the alkali liquor is 1.5-2.5mmol/L NaOH solution, and the soaking time is 1.5-2.5 h.
Preferably, in the step (1), the cleaning method is deionized water rinsing.
Preferably, in the step (2), the CuSO4The concentration of the solution is 80-120 mmol/L.
Preferably, in the step (2), the protective agent is lactose, and the addition amount of lactose is calculated according to the ratio of the amount of the substance: CuSO40.9-1.1: 1.
preferably, in the step (2), the reducing agent is NH2OH·HCl，NH2OH & HCl concentration of 0.8-1.2mol/L, NH in terms of mass ratio2OH & HCl addition amount: CuSO4Is 5-10: 1.
preferably, in the step (2), the reaction time is 1.5-2.5h at the temperature of 55-65 ℃; the cleaning method comprises the steps of washing with ethanol, rinsing with deionized water, cleaning, and transferring to a vacuum oven for drying for 10-12 h.
The invention also discloses the nano CuO/Cu2The O-cotton fabric composite material is used for degrading organic dye under visible light.
Compared with the prior art, the invention has the beneficial effects that:
1. the catalytic efficiency is high under visible light;
2. CuO/Cu loaded on cotton fabric2The firmness of the O nano particles is high;
3. low cost and repeated use.
Drawings
FIG. 1 shows cotton fabric loaded with nano CuO/Cu2The comparison of the front and back of O nano-particles, (a) is cotton fabric before sample preparation, and (b) is prepared nano CuO/Cu2O-cotton fabric composite material；
FIG. 2 is an XRD pattern of example 1 of the present invention;
FIG. 3 is a graph of photodegradation rate for example 1 of the present invention;
FIG. 4 is a diagram of a photocatalytic cycle in example 1 of the present invention;
FIG. 5 is a graph showing the degradation rate of the dyes in examples of the present invention and comparative examples for 2 hours.
Detailed Description
The present invention will be further described with reference to the following examples. The devices, reagents and methods referred to in the present invention are those known in the art unless otherwise specified.
Example 1
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric and soaking in 10mL of CuSO with the concentration of 100mmol/L4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 0.8mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In this process, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction is finished, taking out a sample, slightly washing the sample with ethanol for three times, and then transferring the sample to a vacuum oven to dry for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
Example 2 (copper sulfate addition more than example 1)
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric and soaking in 10mL of CuSO with the concentration of 150mmol/L4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 0.8mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In this process, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction, the sample was taken out and gently washed with ethanolThirdly, transferring the mixture to a vacuum oven for drying for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
Example 3 (copper sulfate addition amount is smaller than that in example 1)
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric and soaking in 10mL of CuSO with the concentration of 80mmol/L4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 0.8mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In this process, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction is finished, taking out a sample, slightly washing the sample with ethanol for three times, and then transferring the sample to a vacuum oven to dry for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
Example 4 (reducing agent addition amount is smaller than that in example 1)
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric and soaking in 10mL of CuSO with the concentration of 150mmol/L4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 0.5mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In this process, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction is finished, taking out a sample, slightly washing the sample with ethanol for three times, and then transferring the sample to a vacuum oven to dry for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
Example 5 (more reducing agent than in example 1)
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric, soaking in 10mL of 150mmol/L CuSO4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 1.0mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In this process, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction is finished, taking out a sample, slightly washing the sample with ethanol for three times, and then transferring the sample to a vacuum oven to dry for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
Comparative example 1
The surface of the cotton fabric is not loaded with CuO or Cu2O。
Comparative example 2
The surface of the cotton fabric only loads Cu2O。
Comparative example 3 (copper sulfate addition amount is insufficient)
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric and soaking in 10mL of CuSO with the concentration of 10mmol/L4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 0.8mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In this process, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction is finished, taking out a sample, slightly washing the sample with ethanol for three times, and then transferring the sample to a vacuum oven to dry for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
COMPARATIVE EXAMPLE 4 (excess copper sulfate addition)
(1) Cotton fabric pretreatment: soaking cotton cloth in 2 mmol/L sodium hydroxide solution for 2 hr, washing with deionized water, and drying;
(2) weighing 1g of cotton fabric and soaking in 10mL of CuSO with the concentration of 200mmol/L4To the solution, 34mg of lactose was added as a protective agent, followed by 1mol/L sodium hydroxide solution to adjust the pH to 12, and then 10mL of a solution having a concentration of: 0.8mol/L reducing agent NH2OH & HCl was stirred at 60 ℃ for 2 h. In the process ofIn, Cu2+Is reduced by a reducing agent NH2And (4) reducing OH & HCl. After the reaction is finished, taking out a sample, slightly washing the sample with ethanol for three times, and then transferring the sample to a vacuum oven to dry for 12 hours to obtain the nano CuO/Cu2An O-cotton fabric composite material.
Performance testing
SEM observation, XRD test, photodegradation rate test and cycle number test were carried out on the sample of example 1.
As can be seen from FIG. 1 (b), the sample cotton fabric prepared in example 1 had a large amount of nano CuO/Cu adhered to the surface thereof2O nanoparticles, whereas fig. 1 (a) produces a clean front surface. As can be seen from fig. 2, the sample obtained by XRD diffraction observation can observe characteristic peaks of cellulose I at 2 θ =15.03 °, 16.7 ° and 22.8 °; in addition, diffraction peaks characteristic of crystal planes of CuO ("1" ̅ 11), (111), ("2" ̅ 02), (202), ("1" ̅ 13), (022), (220) appear at 35.8 °, 38.9 °, 48.7 °, 58.2 °, 61.5 °, 66.2 ° and 68.1 ° of 2 θ, respectively, and diffraction peaks characteristic of crystal planes of 29.36 °, 36.45, 42.38 °, 61.57 °, 73.69 ° and 77.65 ° of 2 θ, and Cu corresponding to crystal planes of 110, 111, 200, 220, 311 and 222, respectively2And (4) O crystals. Indicating that the surface deposits of the cotton fabrics are CuO and Cu2And O crystal phase. C in FIG. 30The initial concentration of the dye and the residual concentration of the dye after catalytic degradation are C, and the result shows that the sample has a higher catalytic degradation rate. As can be seen in fig. 4, the samples still have a higher catalytic drop after 6 cycles.
The embodiment 1-5 and the comparative example 1-4 are irradiated on a visible light source 350w xenon lamp, the degraded dye solution is taken after 2 hours to test the degradation rate, the embodiment 5 with the highest degradation efficiency can be obtained, and the scheme generates the nano-Cu2The O hybridized CuO has a better proportion and obtains the best catalytic synergistic effect. Examples 1 and 3 due to CuSO4Less Cu produced2The amount of O is relatively small, and thus the degradation efficiency is lower than that of example 2; example 4 the degradation efficiency was low due to insufficient reducing agent, more CuO was produced and Cu having a stronger reducibility was formed2The amount of O nano particles is less; example 5 the degradation efficiency was the highest because the amounts of reducing agent and copper sulfate were relatively the highest and therefore the reduction yield was higherMuch Cu2O and CuO hybrid materials. Comparative example 1 has no catalytic function nano-particles on the surface, basically has no catalytic degradation capability, and comparative example 2 has Cu on the surface2O but no CuO concerted catalysis did not form composite particles, and thus the degradation efficiency was lower than examples 1-5, and comparative example 3 had lower degradation efficiency because the number of composite particles formed was smaller than that of examples. Comparative example 4 is insufficient in the amount of the reducing agent due to the higher copper sulfate, and a part of the unreduced copper ions are largely generated into CuO at a high temperature, which is disadvantageous to the catalytic action of the cuprous oxide catalytic active sites, so that the catalytic degradation efficiency is lower than that of examples 2 and 5. As shown in fig. 5.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (9)

1. Nano CuO/Cu2The O-cotton fabric composite material is characterized in that the composite material is Cu2O hybridized CuO nano particle modified cotton fabric, Cu2The O hybridized CuO nano particle structure is Cu2O coated CuO particles and Cu2O-hybridized CuO nanoparticles were attached to the surface of cotton fibers.
2. The CuO/Cu nanoparticles as claimed in claim 12The preparation method of the O-cotton fabric composite material is characterized by comprising the following steps of:
(1) cotton fabric pretreatment: soaking in alkali liquor, cleaning, and drying;
(2) nano CuO/Cu2O-cotton fabric composite material: placing cotton fabric in CuSO4Adding a protective agent into the solution, adjusting the pH value to 11.5-12.5, then adding a reducing agent, reacting at the temperature of 55-65 ℃, cleaning and drying after the reaction is finished to obtain CuO/Cu2An O-cotton fabric composite; the mass ratio of the cotton fabric to the copper sulfate in the solution is 1: 0.015-0.017.
3. The preparation method of claim 2, wherein in the step (1), the alkali liquor is 1.5-2.5mmol/L NaOH solution, and the soaking time is 1.5-2.5 h.
4. The method according to claim 2, wherein in the step (1), the washing method is a deionized water rinse.
5. The method according to claim 2, wherein in the step (2), the CuSO is used as the CuSO4The concentration of the solution is 80-120 mmol/L.
6. The preparation method according to claim 2, wherein in the step (2), the protective agent is lactose, and the addition amount of lactose is recorded in terms of mass ratio: CuSO40.9-1.1: 1.
7. the method according to claim 2, wherein in the step (2), the reducing agent is NH2OH·HCl，NH2OH & HCl concentration of 0.8-1.2mol/L, NH in terms of mass ratio2OH & HCl addition amount: CuSO4Is 5-10: 1.
8. the method according to claim 2, wherein in the step (2), the reaction time is 1.5 to 2.5 hours at a temperature of 55 to 65 ℃; the cleaning method comprises the steps of washing with ethanol, rinsing with deionized water, cleaning, and transferring to a vacuum oven for drying for 10-12 h.
9. The nano CuO/Cu as claimed in claim 12The O-cotton fabric composite material is used for degrading organic dye under visible light.
CN202111145262.3A 2021-09-28 2021-09-28 Nano CuO/Cu2O-cotton fabric composite material and preparation method and application thereof Withdrawn CN114100693A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114870897A (en) * 2022-05-11 2022-08-09 常州大学 Preparation method and application of multifunctional photocatalytic bactericidal cotton fabric responding under visible light
CN115888821A (en) * 2022-11-21 2023-04-04 苏州大学 Composite cotton fabric, preparation method thereof and application thereof in degrading organic pollutants under offset double light sources

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114870897A (en) * 2022-05-11 2022-08-09 常州大学 Preparation method and application of multifunctional photocatalytic bactericidal cotton fabric responding under visible light
CN114870897B (en) * 2022-05-11 2024-03-15 常州大学 Preparation method and application of multifunctional photocatalytic sterilization cotton fabric responding under visible light
CN115888821A (en) * 2022-11-21 2023-04-04 苏州大学 Composite cotton fabric, preparation method thereof and application thereof in degrading organic pollutants under offset double light sources

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