CN114377706A - MXene/TiO loaded by glass fiber ball bundle2Aerogel composite material and preparation method thereof - Google Patents
MXene/TiO loaded by glass fiber ball bundle2Aerogel composite material and preparation method thereof Download PDFInfo
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- CN114377706A CN114377706A CN202210000519.4A CN202210000519A CN114377706A CN 114377706 A CN114377706 A CN 114377706A CN 202210000519 A CN202210000519 A CN 202210000519A CN 114377706 A CN114377706 A CN 114377706A
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- glass fiber
- mxene
- fiber ball
- tio
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- 239000003365 glass fiber Substances 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000004964 aerogel Substances 0.000 claims abstract description 24
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002699 waste material Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 12
- 239000011240 wet gel Substances 0.000 claims abstract description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000007710 freezing Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 7
- 238000004381 surface treatment Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 3
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 3
- 229960005055 sodium ascorbate Drugs 0.000 claims description 3
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 229920002873 Polyethylenimine Polymers 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 125000003916 ethylene diamine group Chemical group 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims 1
- 229960001124 trientine Drugs 0.000 claims 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 239000004408 titanium dioxide Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 230000001699 photocatalysis Effects 0.000 description 8
- 239000011941 photocatalyst Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 transition metal carbides Chemical class 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910009819 Ti3C2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010793 electronic waste Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/51—
-
- B01J35/58—
-
- 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
-
- 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
Abstract
The invention discloses a glass fiber ball bundle loaded MXene/TiO2Aerogel composite materials and methods of making the same. Firstly, preparing a glass fiber ball bundle by using waste PCB (printed Circuit Board) nonmetal powder and carrying out surface active treatment on the glass fiber ball bundle; adding MXene powder into anhydrous ethanol solution of tetrabutyl titanate to prepare MXene alcohol dispersion solution by ultrasonic treatmentAdding glass fiber ball beam, stirring, adding deionized water, adjusting pH, adding organic solution, transferring to a reaction kettle, and heating to obtain glass fiber ball beam loaded MXene/TiO2Wet gel; finally, after sieving, freezing and drying treatment are carried out to obtain the MXene/TiO loaded by the glass fiber ball bundle2An aerogel composite. The composite material obtained by the invention can be used for adsorption and catalytic degradation of organic pollutants; can coordinate and modify titanium dioxide and greatly expand TiO2Photocatalytic range.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a composite materialMXene/TiO loaded by glass fiber ball bundle2Aerogel composite materials and methods of making the same.
Background
Printed Circuit Boards (PCBs) are widely used in various electronic devices as basic components of the electronic industry, and the number of discarded PCBs is remarkably increasing with the generation of a large amount of electronic waste. Conventional PCB materials contain precious metals such as gold, silver, and platinum, metals having recycling values such as copper, aluminum, lead, and zinc, and a large amount of non-metallic materials such as plastics, ceramics, glass fibers, and flame retardants, as well as various harmful substances, and their recycling and disposal techniques are receiving wide attention at home and abroad. The mechanical physical recovery is a widely adopted technology at present, and mainly recovers valuable metals in waste PCBs, and residual non-metal powder is difficult to be effectively utilized due to a special three-dimensional structure.
MXene is a class of 2D inorganic compound materials consisting of several atomic layers of transition metal carbides, nitrides or carbonitrides. MXene has an intrinsic nanoscale lamellar structure, metal components and surface functional groups with adjustable height, a huge specific surface area, good hydrophilicity and excellent conductivity, so that MXene has huge potential in the aspects of environment and energy catalysis. Wherein, in the field of catalysis, Ti3C2TxThe photocatalyst has been applied to photocatalysis such as ORR, OER, HER, etc., water decomposition hydrogen production, photocatalytic degradation of organic pollutants in water, and the like, can be a catalyst or a carrier, and proves the great potential of the photocatalyst in the field of photocatalysts.
TiO2As a semiconductor photocatalyst, the photocatalyst has the advantages of strong oxidation capability, stable physical and chemical properties, no toxicity, low price and the like, and is always at the core position of research in the field of environmental purification. However, TiO2Because the material can only utilize ultraviolet light, the efficiency of the material per se in the aspect of solar energy utilization is low, and the photoproduction electron-hole are easy to recombine, which is the key for restricting the practical application of the material.
Chinese patent CN107399928B discloses a method for preparing glass fiber ball bundles by using waste PCB non-metal powder.
Disclosure of Invention
The invention aims to provide a glass fiber ball bundle loaded MXene/TiO2Aerogel composite materials and methods of making the same. The invention takes waste PCB non-metal powder as raw material to prepare glass fiber ball bundle used as carrier, and MXene/TiO is loaded in the ball bundle2Aerogel, supported MXene/TiO2The aerogel is used as a photocatalyst, so that the problem that the MXene material is not easy to fix is solved, and the stability of the composite material is improved; and also utilizes MXene and TiO2Synergistic effect of (2), reduction of TiO2The forbidden band width of the catalyst can shift the photocatalysis to red, and the organic pollutants can be degraded by light under visible light (sunlight irradiation), thereby greatly expanding TiO2The range of application of (a); the invention takes the waste as the raw material, takes the decomposition of organic waste as the aim, realizes the aim of treating waste by waste,
in order to achieve the purpose, the invention provides MXene/TiO loaded by glass fiber ball bundles2A method of preparing an aerogel composite comprising the steps of:
step 1, preparing glass fiber ball bundles by using waste PCB (printed Circuit Board) nonmetal powder, and performing surface treatment by using a silane coupling agent;
step 2, slowly adding 3-4 g of MAX phase into 60-80 mL of HF solution with the mass fraction of 25% -40%, stirring for 24-48 h at the temperature of 40-60 ℃, cooling, centrifuging, washing and precipitating with deionized water until the pH value is 5-7, and drying to obtain MXene powder;
step 3, adding tetrabutyl titanate into absolute ethyl alcohol, stirring for 2-6 hours, adding MXene powder prepared in the step 2, performing ultrasonic treatment for 30-90 minutes, adding the glass fiber ball bundle prepared in the step 1, stirring, adding a proper amount of deionized water, adjusting the pH value to 1-3 with acid, adding an organic solution, transferring the organic solution into a reaction kettle, heating, cooling and sieving to obtain the MXene/TiO loaded on the glass fiber ball bundle2Wet gel;
step 4, loading MXene/TiO on glass fiber ball bundle2Pre-freezing the wet gel in liquid nitrogen for 1-6 h, and then carrying out vacuum freeze drying to obtain the glass fiber ball bundle loaded MXene/TiO2An aerogel composite.
In the step 1, the glass fiber ball bundle is prepared from the waste printed circuit board PCB non-metal powder according to the Chinese patent CN 107399928B.
In the step 1, the silane coupling agent is one of KH-550, KH-560, KH-570, KH-590 and KH-791
One or a combination of two or more.
In the above step 2, the MAX phase is Ti3AlC2A material.
In the step 3, the feeding ratio of the surface-treated glass fiber ball bundle to MXene powder to tetrabutyl titanate is 0.3-0.5 g: 0.1-0.2 g: 1-5 mL; the feeding ratio of the absolute ethyl alcohol to the tetrabutyl titanate to the deionized water is 20-60 mL to 1-5 mL to 5-15 mL.
In the step 3, the mesh number of the sieved screen is 20-120 meshes.
In the step 3, the acid is one or a combination of more than two of hydrochloric acid, glacial acetic acid, nitric acid, phosphoric acid and sulfuric acid.
In the step 3, the organic solution is ethylenediamine, diethylenetriamine, sodium ascorbate, triethylenetetramine and polyethylene glycol
One or more of the alkene imines.
In the step 3, the heating temperature is 90-120 ℃, and the heating time is 3-12 h.
In the step 4, the vacuum freeze drying temperature is-10 to-90 ℃, and the freeze drying time is 2 to 10 hours.
The invention also provides MXene/TiO loaded by the glass fiber ball bundle2Aerogel composite material prepared by the above method.
Compared with the prior art, the invention has the following advantages:
firstly, glass fiber ball bundles prepared by taking waste PCB non-metal powder as raw materials are taken as carriers, and MXene/TiO is formed in the huge internal space of the ball bundles2Aerogel is a new composite material.
② glass fiber ball bundle loaded MXene/TiO2The aerogel has larger internal gaps, so that pollutants can flow in the ball beam conveniently, and the organic pollutants are greatly improvedAdsorption and degradation efficiency.
Utilizing the synergistic effect of MXene material on titanium dioxide to greatly expand TiO2The application range of photocatalysis.
MXene/TiO loaded on glass fiber in the invention2Aerogel photocatalysis combined material, glass fiber ball bundle are as photocatalyst's carrier, can directly filter after the reaction is accomplished and wash the recovery, can also reuse after the drying, have solved the problem that powdered catalyst partly is extravagant and is difficult to retrieve, avoid secondary pollution.
Detailed Description
The technical solution of the present invention is further explained below.
The invention uses the glass fiber ball bundle prepared by Chinese patent CN107399928B as a carrier, carries MXene/TiO after the surface treatment of the glass fiber ball bundle2Aerogel for the adsorption and catalytic degradation of organic pollutants. The advantages of large internal space of the glass fiber ball bundle are fully exerted by utilizing the unique metal conductivity, hydrophilicity, good processability, high specific surface area and the like of MXenes, the photocatalytic performance of titanium dioxide is optimized, and the photocatalytic efficiency is greatly improved.
In the embodiment, glass fiber ball bundles are prepared according to the technical scheme of embodiment 1 of Chinese patent CN 107399928B;
in the examples, MXene powder was prepared as follows:
4gMAX phase material Ti3AlC2Slowly adding the mixed solution into 80mL of HF solution with the mass fraction of 40%, heating at the constant temperature of 45 ℃, stirring for 48 hours, cooling, centrifuging, washing the precipitate with deionized water until the pH value of the supernatant is 6, and drying to obtain MXene powder.
Example 1
Preparing glass fiber ball bundles by using waste PCB nonmetal powder, adding 0.1mL KH-550 and 0.2mL concentrated hydrochloric acid into 20mL absolute ethyl alcohol solution, soaking for 30min at normal temperature, filtering, and drying to obtain the glass fiber ball bundles after surface treatment. Adding 2mL of tetrabutyl titanate into 20mL of absolute ethyl alcohol, stirring for 2h, adding 0.15g of MXene powder, carrying out ultrasonic treatment for 30min, adding 0.3g of glass fiber ball bundles, mixing and stirring for 2h,slowly adding 5mL of deionized water, then adding 0.8mL of concentrated hydrochloric acid, measuring the pH value to be 1.2, finally adding 0.2mL of ethylenediamine solution with the concentration of 0.95g/mL, transferring the mixture into a reaction kettle, reacting for 10 hours at the temperature of 95 ℃, cooling, and sieving by a sieve of 80 meshes to obtain the MXene/TiO supported by the glass fiber ball bundle2Wet gel. MXene/TiO is loaded on glass fiber ball bundle2Freezing the wet gel in liquid nitrogen for 1h, and then carrying out vacuum freeze drying at-90 ℃ for 5h to obtain the glass fiber ball bundle loaded MXene/TiO2An aerogel composite.
Example 2
Preparing glass fiber ball bundles by using waste PCB nonmetal powder, adding 0.05mL of KH-550 and 0.15mL of concentrated hydrochloric acid into 10mL of absolute ethanol solution, soaking for 45min at normal temperature, filtering, and drying to obtain the glass fiber ball bundles after surface treatment. Adding 4mL of tetrabutyl titanate into 30mL of absolute ethyl alcohol, stirring for 4h, adding 0.1g of MXene powder, performing ultrasonic treatment for 60min, adding 0.4g of glass fiber ball bundles, mixing and stirring for 4h, slowly adding 5mL of deionized water, adding 1.0mL of concentrated hydrochloric acid to obtain a pH value of 1.6, finally adding 0.3mL of diethylenetriamine solution with the concentration of 0.95g/mL, transferring the mixture to a reaction kettle, reacting for 5h at 120 ℃, cooling, and sieving with a 40-mesh sieve to obtain MXene/TiO loaded by the glass fiber ball bundles2Wet gel. MXene/TiO is loaded on glass fiber ball bundle2Freezing the wet gel in liquid nitrogen for 3h, and then carrying out vacuum freeze drying at-20 ℃ for 9h to obtain the glass fiber ball bundle loaded MXene/TiO2An aerogel composite.
Example 3
Preparing glass fiber ball bundles by using waste PCB nonmetal powder, adding 0.15mL KH-550 and 0.3mL concentrated hydrochloric acid into 40mL absolute ethyl alcohol solution, soaking for 35min at normal temperature, filtering, and drying to obtain the glass fiber ball bundles after surface treatment. Dissolving 5mL of tetrabutyl titanate into 60mL of absolute ethyl alcohol, stirring for 6h, adding 0.2g of MXene powder, performing ultrasonic treatment for 90min, adding 0.5g of glass fiber ball bundle, mixing and stirring for 6h, slowly adding 10mL of deionized water, adding 1.8mL of concentrated hydrochloric acid to obtain a pH value of 2.1, finally adding 0.1mL of sodium ascorbate solution with the concentration of 0.1g/L, transferring to a reaction kettle, reacting for 6h at 100 ℃, cooling, and sieving with a 100-mesh sieve to obtain MXene/TiO supported by the glass fiber ball bundle2Wet gel. MXene/TiO is loaded on glass fiber ball bundle2Freezing the wet gel in liquid nitrogen for 5h, and then carrying out vacuum freeze drying at-50 ℃ for 2h to obtain the glass fiber ball bundle loaded MXene/TiO2An aerogel composite.
Example 4 (catalytic Performance test)
MXene/TiO Supported glass fiber bundles obtained in example 22Aerogel composite material 0.98g and glass fiber ball bundle loaded TiO20.98g of aerogel is respectively added into 100mL of methylene blue solution with the concentration of 20mg/L, the solution is put into a gas bath constant temperature oscillator for shading and oscillating for 30min at 180r/min, then a xenon lamp is started to irradiate the solution with the power of 300W and continuously oscillate, 3mL of suspension is collected every 30min, and the absorbance of the solution at the specified wavelength position is measured by using an ultraviolet-visible spectrophotometer after the solution is filtered. The experimental result shows that the glass fiber ball bundle loads MXene/TiO2The removal rate of the aerogel composite material after 2 hours of photocatalysis reaches 85.2 percent, and the glass fiber ball bundle loads TiO2The removal rate of the aerogel after 2 hours of photocatalysis is 23.1 percent.
In conclusion, the glass fiber ball bundles are prepared by using the waste PCB non-metal powder and subjected to surface active treatment; adding tetrabutyl titanate into an absolute ethyl alcohol solution, then adding MXene powder, performing ultrasonic treatment to disperse MXene in the alcohol solution, then adding glass fiber ball bundles, slowly adding a certain volume of deionized water, adjusting the pH value, then adding an organic solution, transferring the mixture into a reaction kettle, and reacting for a certain temperature and time to obtain glass fiber ball bundle loaded MXene/TiO2Wet gel; after sieving, carrying out freeze drying treatment to obtain the glass fiber ball bundle loaded MXene/TiO2An aerogel composite.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (10)
1.MXene/TiO loaded by glass fiber ball bundle2A method for preparing an aerogel composite, comprising
The following steps:
step 1, preparing glass fiber ball bundles by using waste PCB (printed Circuit Board) nonmetal powder, and performing surface treatment by using a silane coupling agent;
step 2, slowly adding 3-4 g of MAX phase into 60-80 mL of HF solution with the mass fraction of 25% -40%, stirring for 24-48 h at the temperature of 40-60 ℃, cooling, centrifuging, washing and precipitating with deionized water until the pH value is 5-7, and drying to obtain MXene powder;
step 3, adding tetrabutyl titanate into absolute ethyl alcohol, stirring for 2-6 hours, adding MXene powder prepared in the step 2, performing ultrasonic treatment for 30-90 minutes, adding the glass fiber ball bundle prepared in the step 1, stirring, adding a proper amount of deionized water, adjusting the pH value to 1-3 with acid, adding an organic solution, transferring the organic solution into a reaction kettle, heating, cooling and sieving to obtain the MXene/TiO loaded on the glass fiber ball bundle2Wet gel;
step 4, loading MXene/TiO on glass fiber ball bundle2Pre-freezing the wet gel in liquid nitrogen for 1-6 h, and then carrying out vacuum freeze drying to obtain the glass fiber ball bundle loaded MXene/TiO2An aerogel composite.
2. The process according to claim 1, wherein in the step 1, the silane coupling agent is KH-550, KH-560, or a mixture thereof,
KH-570, KH-590 and KH-791.
3. The method of claim 1, wherein in step 2, the MAX phase is Ti3AlC2A material.
4. The method according to claim 1, wherein in the step 3, the surface-treated glass fiber bundles,
The feeding ratio of MXene powder to tetrabutyl titanate is 0.3-0.5 g: 0.1-0.2 g: 1-5 mL; anhydrous ethanol, titanic acid
The feeding ratio of tetrabutyl ester to deionized water is 20-60 mL to 1-5 mL to 5-15 mL.
5. The method according to claim 1, wherein the number of the sieved mesh in step 3 is 20 to 120
To achieve the purpose.
6. The method according to claim 1, wherein in the step 3, the acid is hydrochloric acid, glacial acetic acid, nitric acid,
One or more of phosphoric acid and sulfuric acid.
7. The method according to claim 1, wherein in step 3, the organic solvent is ethylenediamine or diethylentriamine
One or more of ethylene triamine, sodium ascorbate, triethylene tetramine and polyethylene imine.
8. The method according to claim 1, wherein the heating temperature in step 3 is 90 to 120 ℃ and the heating time is 3 to 12 hours.
9. The method according to claim 1, wherein in the step 4, the vacuum freeze-drying temperature is from-10 to-90 ℃,
the freeze drying time is 2-10 h.
10. MXene/TiO loaded by glass fiber ball bundle2Aerogel composite material, characterized in that it is formed from the composition of claim 1 to
9 by the method of any one of the above items.
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