CN111905687A - Flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material and preparation method thereof - Google Patents
Flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 19
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003365 glass fiber Substances 0.000 claims abstract description 66
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000001354 calcination Methods 0.000 claims abstract description 47
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000004744 fabric Substances 0.000 claims abstract description 41
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000011259 mixed solution Substances 0.000 claims abstract description 40
- 239000002243 precursor Substances 0.000 claims abstract description 40
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940078494 nickel acetate Drugs 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 23
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 23
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 23
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 23
- 238000002791 soaking Methods 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002604 ultrasonography Methods 0.000 claims abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 description 35
- 239000000243 solution Substances 0.000 description 17
- 239000000463 material Substances 0.000 description 10
- 229910001385 heavy metal Inorganic materials 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 208000005374 Poisoning Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 231100000570 acute poisoning Toxicity 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 231100000739 chronic poisoning Toxicity 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention relates to a flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material and a preparation method thereof, which comprises the following steps of a, sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for ultrasound; then, arranging the glass fiber in a tube furnace, and calcining at a certain temperature for later use; b. dissolving manganese acetate, cobalt acetate, nickel acetate and a certain amount of thiourea in a certain molar ratio in a glycerol aqueous solution, stirring and ultrasonically treating for a certain time to form a mixed solution; c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a constant temperature box, and reacting for a certain time at a constant temperature to obtain a precursor product; d. and (3) placing the precursor product in a tubular furnace, and calcining and reacting at a certain temperature for a certain time to obtain the product. The method has the advantages of simple preparation process, high controllable degree, uniform product, novel appearance, excellent visible light photocatalysis performance and wide application in the energy and environmental protection industries.
Description
Technical Field
The invention belongs to the technical field of semiconductor nano material preparation processes, and relates to a flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material and a preparation method thereof.
Technical Field
With the rapid development of society and economy, environmental pollution is becoming more serious and the environmental quality is decreasing. Because industrial and mining wastewater, domestic sewage and the like are discharged without proper treatment, pollutants rich in heavy metals are input, the content of the heavy metals in the water body is rapidly increased, and the water body is polluted by the heavy metals.
When the pollutant discharge amount exceeds the self-purification capability of the environment, the ecological landscape is deteriorated, aquatic life is lost, human drinking water sources are polluted, the quality of the surrounding environment is reduced, and the health of the human body is influenced, and if the heavy metal exceeds the tolerance limit of the human body, acute poisoning, subacute poisoning and chronic poisoning of the human body can be caused. Heavy metals have the characteristics of strong stability, difficulty in collection, high toxicity and the like, not only deteriorate the composition, structure and function of soil, but also seriously harm human health through different channels. Heavy metals flow into water and soil and volatilize into the atmosphere, and then are taken into human bodies through channels such as respiratory tracts, plants, food and the like, so that the human health is harmed. Therefore, the work of treating heavy metal pollution is highly valued by researchers at home and abroad, and becomes an important research content in the field of scientific research.
The sewage treatment process is born till now, and pollutants in water are removed by treatment technologies such as a membrane filtration method, a biological oxidation method, a chemical precipitation method, an ion exchange method, an electrochemical method, an ion exchange method and the like, but the treatment methods have the defects of complex operation process, high operation cost, secondary pollution and the like. Compared with other treatment technologies, the adsorption separation technology is widely used in the wastewater treatment process due to the characteristics of abundant adsorbent resources, simple processing technology, low cost and the like. Therefore, the adsorption separation method is a treatment method for removing toxic pollutants in sewage, which is most actively researched and applied in recent years. As is known, an adsorbent material in an adsorption separation technology is very important, but the existing adsorbent material needs to be further improved, and particularly how to realize rapid separation and improve the adsorption performance of the material, the nano-sized adsorbent material has large specific surface area and high activity, but is difficult to separate and recover, and at present, a suitable carrier which not only maintains the activity of the adsorbent but also meets the physical and chemical performance requirements of a specific material is difficult to find. Therefore, the realization of large-scale industrial application of the adsorption material is still far from the right.
Disclosure of Invention
The invention aims to solve the primary technical problem of providing a preparation method of a flexible glass fiber cloth @ CoMnNi multi-hydroxide composite material, which has the advantages of simple process, low cost, short reaction period and uniformity.
A preparation method of a flexible carbon fiber cloth @ CoMnNi multi-hydroxide absorption composite material comprises the following steps:
a. sequentially placing the glass fiber cloth in acetone, ethanol and deionized water for soaking and ultrasound for a certain time; then, arranging the glass fiber in a tube furnace, and calcining at a certain temperature for later use; b. dissolving manganese acetate, cobalt acetate, nickel acetate and a certain amount of thiourea in a certain molar ratio in a glycerol aqueous solution, stirring and ultrasonically treating for a certain time to form a mixed solution; c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a constant temperature box, and reacting for a certain time at a constant temperature to obtain a precursor product; d. and placing the precursor product in a tubular furnace, calcining at a certain temperature for a certain time, and obtaining the flexible glass fiber cloth @ CoMnNi multi-hydroxide adsorbing material.
Further, the soaking and ultrasonic treatment time of the step a is 5-20 minutes; the calcination temperature is 300-800 ℃.
Further, the molar ratio of manganese acetate to cobalt acetate in the step b is 1:1-3:1, and the molar ratio of thiourea to nickel acetate is (0.5-5 mmol): 1 mol.
Preferably, the ultrasonic time of the step b is 10 to 50 minutes, and the stirring time is 30 to 120 minutes.
Further, the constant temperature of the step c is 100-200 ℃, and the reaction time is 3-12 h.
Further, the calcination temperature in the step d is 300-800 ℃, and the reaction time is 3-12 h.
The invention also discloses a flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material prepared by the preparation method, and the composite material can be used for adsorbing heavy metal ions.
Compared with the prior art, the invention has the outstanding effects that: the preparation process of the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material provided by the invention is simple, the requirement on equipment is low, and the controllability is high. The preparation method has the advantages that the preparation of the flexible and easily-recycled glass fiber cloth @ CoMnNi multi-hydroxide composite material is realized through reasonable process control, the flexible and easily-recycled adsorbing material of the glass fiber cloth is uniform in size, good in dispersion and novel in appearance, can adsorb heavy metal ions, has excellent adsorption performance, and has wide application in the energy and environment-friendly industries.
Drawings
Figure 1 is a Scanning Electron Microscope (SEM) photograph of the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite prepared in example 2.
Figure 2 is another Scanning Electron Microscope (SEM) photograph of the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite prepared in example 2.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited thereto.
Example 1
A preparation method of a flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material comprises the following specific steps:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 3 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 2
A preparation method of a flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material comprises the following specific steps:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
The attached figures 1-2 show SEM of the flexible glass fiber cloth @ CoMnNi multi-hydroxide adsorbing material prepared by the method, and the attached figures show that the flexible glass fiber cloth @ CoMnNi multi-hydroxide adsorbing material is successfully prepared and has uniform size.
Example 3
This example differs from example 2 in that the calcination temperature in step a was changed to 800 ℃ and otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 800 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 4
This example differs from example 2 in that the amount of thiourea was changed to 3mmol, and the other examples are the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 3mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 5
This example differs from example 2 in that the stirring time was changed to 60min, and the rest is the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 6
This example differs from example 2 in that the molar ratio of manganese acetate, cobalt acetate and nickel acetate was changed to 2:1:1, otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 2mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 7
This example differs from example 2 in that the temperature of the oven was changed to 160 ℃ and otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 160 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 8
This example differs from example 2 in that the reaction time in step c was changed to 6 hours, otherwise the same as example 2, as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 6 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 9
This example differs from example 2 in that the temperature of the oven was changed to 180 ℃ and otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 180 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 10
This example differs from example 2 in that the calcination temperature in step d was changed to 300 ℃ and otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 300 ℃ for 3h to obtain the product.
Example 11
This example differs from example 2 in that the calcination temperature in step d was changed to 800 ℃ and otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 800 ℃ for 3h to obtain the product.
Example 12
This example differs from example 2 in that the reaction time in step d was changed to 6h, otherwise the same as example 2, as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 6h to obtain the product.
Example 13
The difference between this example and example 2 is that the ultrasonic time in step b is changed to 30 minutes, and the rest is the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 30 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 14
This example differs from example 2 in that the stirring time in step b was changed to 60 minutes, and otherwise the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 60 minutes until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 15
This example differs from example 2 in that the reaction time in step d was changed to 12h, otherwise the same as example 2, as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 12h to obtain the product.
Example 16
This example differs from example 2 in that the soaking time in step a was changed to 20 minutes, and the rest is the same as example 2, specifically as follows:
a. sequentially placing the glass fiber cloth in acetone, ethanol and deionized water for soaking for 20 minutes, and respectively carrying out ultrasonic treatment for 15 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Example 17
The difference between this example and example 2 is that the ultrasound time was changed to 10 minutes in step a, and the rest is the same as example 2, specifically as follows:
a. sequentially soaking glass fiber cloth in acetone, ethanol and deionized water for 10 minutes, and respectively carrying out ultrasonic treatment for 10 minutes; then, arranging the glass fiber in a tube furnace, and calcining at 500 ℃ for later use;
b. dissolving 1mol of manganese acetate, 1mol of cobalt acetate, 1mol of nickel acetate and 1mmol of thiourea in a glycerol aqueous solution, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 2 hours until the solution is completely dissolved to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a thermostat, and reacting for 12 hours at 120 ℃ to obtain a product precursor;
d. and (3) placing the precursor product in a tube furnace, and calcining at 500 ℃ for 3h to obtain the product.
Claims (8)
1. A preparation method of a flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material is characterized by comprising the following steps:
a. sequentially placing the glass fiber cloth in acetone, ethanol and deionized water for soaking and ultrasound for a certain time; then, arranging the glass fiber in a tube furnace, and calcining at a certain temperature for later use;
b. dissolving manganese acetate, cobalt acetate, nickel acetate and a certain amount of thiourea in a glycerol aqueous solution, and ultrasonically stirring for a certain time to form a mixed solution;
c. adding the mixed solution and the pretreated glass fiber cloth into a tetrafluoroethylene reaction kettle, putting the reaction kettle into a constant temperature box, and reacting for a certain time at a constant temperature to obtain a precursor product;
d. and (3) placing the precursor product in a tubular furnace, and calcining and reacting at a certain temperature for a certain time to obtain the product.
2. The method for preparing the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material as claimed in claim 1, wherein the soaking ultrasound time of the step a is 5-20 minutes.
3. The method for preparing the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material as claimed in claim 1 or 2, wherein the calcination temperature in the step a is 300-800 ℃.
4. The method for preparing the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material as claimed in claim 1, wherein the molar ratio of manganese acetate, cobalt acetate and nickel acetate in the step b is 1:1:1 to 3:1:1, and the molar ratio of thiourea to nickel acetate is (0.5 to 5 mmol): 1 mol.
5. The method for preparing the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material as claimed in claim 1, wherein the ultrasonic time of the step b or 4 is 10-50 minutes, and the stirring time is 30-120 minutes.
6. The method for preparing the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material as claimed in claim 1, wherein the constant temperature of the step c is 100-.
7. The method for preparing the flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material as claimed in claim 1 or 6, wherein the calcination temperature in the step d is 300-.
8. A flexible carbon fiber cloth @ CoMnNi multi-hydroxide composite material, characterized by being prepared by the preparation method of any one of claims 1 to 7.
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| CN113856706A (en) * | 2021-11-04 | 2021-12-31 | 浙江理工大学 | Glass fiber cloth @ Tb doped CuxTe composite material and preparation method thereof |
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