CN108452767A - A kind of preparation method of nano zine oxide-sisal fiber Carbon composites - Google Patents

A kind of preparation method of nano zine oxide-sisal fiber Carbon composites Download PDF

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Publication number
CN108452767A
CN108452767A CN201810079950.6A CN201810079950A CN108452767A CN 108452767 A CN108452767 A CN 108452767A CN 201810079950 A CN201810079950 A CN 201810079950A CN 108452767 A CN108452767 A CN 108452767A
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sisal fiber
solution
added
nano zine
zine oxide
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覃爱苗
刘霞
郭胜
黄海源
梁怡婵
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Guilin University of Technology
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Guilin University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • 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
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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

Abstract

The invention discloses a kind of preparation methods of nano zine oxide sisal fiber Carbon composites.After sisal fiber is pre-processed, by two one-step hydrothermals, cleans and carbonize, obtain sisal fiber charcoal.Using sisal fiber charcoal, water-soluble zinc salt, sodium hydroxide as raw material, polyethylene glycol is dispersant, prepares nano zine oxide sisal fiber carbon composite using the method for precipitation dipping, the composite material photocatalysis and absorption property are studied with methylene blue solution.There is obtained nano zine oxide sisal fiber Carbon composites good absorption and photocatalysis performance to be up to 98% or more to the removal rate of methylene blue under action of ultraviolet light.Under the action of synergistic effect, nano zine oxide sisal fiber Carbon composites prepared by the present invention greatly enhance the removal rate of dyestuff than undoped sisal fiber charcoal, the absorption property for realizing sisal fiber charcoal is effectively combined with nano-oxide photocatalysis performance, and a more effective approach is provided for useless dirty processing.

Description

A kind of preparation method of nano zine oxide-sisal fiber Carbon composites
Technical field
The invention belongs to new materials and photochemistry field, are related to the preparation side of nano zine oxide-sisal fiber Carbon composites Method and its photocatalysis and Study on adsorption properties.
Background technology
Current environmental problem becomes increasingly severe because industry and economy are without purpose sexual development, dyestuff work difficult to degrade Industry contaminated wastewater is one of them.Since Fujishima in 1972 and Honda reports utilize TiO2The phenomenon that photocatalytic water Since, conductor photocatalysis degradable organic pollutant becomes a potential effective solution method.Such as titanium oxide, zinc oxide and oxygen Change that the metal oxides such as tin can effectively utilize that ultraviolet or sunlight carrys out degradable organic pollutant and becoming one kind has The photochemical catalyst of effect.Zinc oxide is as a kind of typical broadband n types semiconductor in solar cell, photocatalysis and gas sensing Equal fields show excellent performance.But it is relevant research shows that powdered nanoparticles oxide in use there is separation and The not high disadvantage of the difficulty and the efficiency of light energy utilization of recycling, limits its light-catalysed practical application.
Guangxi province Special plant resource-sisal hemp is natural plants high molecular material, and there are many natural holes in inside, living Activator is easily accessible inside it when change, therefore can directly be activated to it to prepare activated carbon fibre, and pre- oxygen is not necessarily to The experimentations such as change, shorten technological process and experimental period, save the energy；In addition sisal fiber charcoal (sisal fiber Carbon, SFC) its abundant micropore distribution characteristics and high-specific surface area make it have good characterization of adsorption.Utilize sisal hemp fibre The performances such as the photocatalysis of charcoal adsorption capacity and nano-oxide are tieed up, it is compound to prepare nano-oxide-sisal fiber charcoal (ZnO/SFC) Material is realized that the absorption property of sisal carbon is effectively combined with nano-oxide photocatalysis performance, is used under synergistic effect effect Useless dirty processing.
Invention prepares nano-ZnO/SFC composite materials using precipitation-impregnation method, and is research pair with methylene blue solution As studying its absorption and photocatalysis performance.By optimizing the preparation process of nano-ZnO-sisal hemp carbon composite, it is expected to improve and receives The shortcomings that catalytic efficiency of rice ZnO, when single use for overcoming nano-ZnO is difficult to recycling.
Invention content
It is an object of the present invention to provide nano zine oxide-sisal fiber charcoals that a kind of high efficiency removes organic dyestuff Compound（ZnO/SFC）Preparation method.
It is as follows：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long, 2g is then taken to be packed into the height of inner liner polytetrafluoroethylene It presses in reaction kettle.
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, 10- is reacted at 160 DEG C It 24 hours, is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, reaction kettle is placed again into after cleaning In, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 10-24 hours at 120 DEG C.
（3）Step (2) products therefrom is washed with deionized water to neutrality, after drying in a nitrogen atmosphere by obtained product Charing 0.5-1 hour is carried out, carbonization temperature is 650-750 DEG C, and heating rate is 1-5 DEG C/min, after cooled to room temperature, is obtained To sisal fiber charcoal, grind into powder is for use.
（4）0.2g polyethylene glycol is added to equipped in the beaker in 30mL distilled water, after polyethylene glycol is uniformly dispersed 1.50 × 10 are added into beaker solution-5-3.08×10-4The water-soluble zinc salt of mol, and make its uniform dissolution.
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, at the uniform velocity stir at room temperature It mixes 4-8 hours.
（6）The NaOH solution of a concentration of 0.0015-0.0307mol/L of 20mL is slowly dropped to step（5）Acquired solution In, so that pH value of solution is adjusted to 10.7-12.1, continues at the uniform velocity to stir 8-12 hours at room temperature after being added dropwise；Then it will mix molten Liquid is transferred in the thermostat water bath at 70 DEG C -90 DEG C, and constant temperature at the uniform velocity stirs lower reaction 30-90 minutes；It is taken out after the completion of reaction Beaker room temperature at the uniform velocity stirs lower cooling, after be filtered, washed, dry, obtain nano zine oxide-sisal fiber Carbon composites.
（7）By step（6）Obtained nano zine oxide-sisal fiber Carbon composites carry out photocatalysis and absorption property is surveyed Examination, experimental subjects are the methylene blue solution of 5mg/L, and maximum material removal rate is up to 99%.
The molecular weight polyethylene glycol is one kind in 6000,4000 and 2000.
The water-soluble zinc salt is one kind in zinc sulfate, zinc nitrate, zinc acetate and zinc chloride.
Preparation method of the present invention is simple, at low cost, pollution-free, and the composite material adsorption capacity of preparation is strong, to organic dyestuff Photocatalysis removal rate it is high；Raw material sisal hemp has abundance, renewable, degradable, pollution-free as a kind of biomass energy The advantages that, there is far-reaching significance to the sustainable development of environmental protection and agricultural；Sisal fiber charcoal (sisal fiber carbon, SFC) belong to hard carbon material, a large amount of micropore, zinc oxide sisal fiber Carbon composites prepared by the present invention, to dyestuff are contained in inside Removal ability is greatly enhanced than not compound sisal fiber charcoal, and solve powdered nanoparticles oxide using process separation and The not high disadvantage of the difficulty and the efficiency of light energy utilization of recycling.
Description of the drawings
Fig. 1 is the sisal fiber charcoal of the preparation of the embodiment of the present invention 1 to methylene blue solution（5mg/L）Absorption property figure.
Fig. 2 is that nano zine oxide-sisal fiber Carbon composites prepared by the different case study on implementation of the present invention are molten to methylene blue Liquid（5mg/L）Removal capacity distribution map.
Fig. 3 is the SEM figures of nano zine oxide-sisal fiber Carbon composites prepared by the embodiment of the present invention 4, ZnO nano grain Son is spherical shape, and average grain diameter is about 90nm.
Specific implementation mode
Embodiment 1：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long with scissors, 2g is then taken to be packed into liner polytetrafluoroethyl-ne In the autoclave of alkene.
（2）The hydrochloric acid of a concentration of 1mol/L of 75mL is added in aforesaid reaction vessel, is reacted 12 hours at 160 DEG C；Instead It should filter after the completion, take the solid on filter paper and be washed with deionized water to neutrality, be placed again into reaction kettle after cleaning drying, it will The hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL, is added in reaction kettle, is reacted 12 hours at 120 DEG C.
（3）After the completion of step (2) reaction, product is taken out, is washed with deionized water to neutrality, obtained product exists after drying Sisal fiber charcoal is carbonized 0.5 hour to obtain under the nitrogen atmosphere that gas flow is 45mL/min, carbonization temperature is 700 DEG C, heating speed Rate is 3 DEG C/min, after cooled to room temperature, obtains sisal fiber charcoal, grind into powder is for use.
（4）By step（3）It obtains sisal fiber charcoal and carries out absorption property test, experimental subjects is the methylene blue of 5mg/L Solution, maximum material removal rate are 87.7% (see attached drawing 1).
Embodiment 2：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long with scissors, 2g is then taken to be packed into liner polytetrafluoroethyl-ne In the autoclave of alkene.
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, 12 are reacted at 160 DEG C Hour, it is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, reaction is placed again into after cleaning drying In kettle, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 12 hours at 120 DEG C.
（3）Step (2) products therefrom is washed with deionized water to neutrality, is in gas flow by obtained product after drying Charing 0.5 hour is carried out under the nitrogen atmosphere of 45mL/min, carbonization temperature is 700 DEG C, and heating rate is 3 DEG C/min, naturally cold But to after room temperature, sisal fiber charcoal is obtained, grind into powder is for use.
（4）0.2g Macrogol 6000s are added to equipped in the beaker in 30mL distilled water, waiting for Macrogol 6000 point It dissipates in uniformly backward beaker solution and 0.0043g (1.50 × 10 is added-5Mol ZnSO)4·7H2O, and make its uniform dissolution.
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, at the uniform velocity stir at room temperature It mixes 4 hours.
（6）The NaOH solution of a concentration of 0.0015mol/L of 20mL is slowly dropped to step（5）In acquired solution, make molten Liquid pH is adjusted to 10.8, continues at the uniform velocity to stir 8 hours at room temperature after being added dropwise；Then mixed solution is transferred at 80 DEG C Thermostat water bath in, constant temperature at the uniform velocity stirs lower reaction 50 minutes；Beaker room temperature is taken out after the completion of reaction at the uniform velocity stirs lower cooling, It centrifuges afterwards, remove supernatant, drying, obtain nano zine oxide-sisal fiber Carbon composites.
（7）By step（6）Obtained nano zine oxide-sisal fiber Carbon composites carry out absorption and photocatalysis performance is surveyed Examination, experimental subjects are the methylene blue solution of 5mg/L, and maximum material removal rate is 94.8% (see attached drawing 2).
Embodiment 3：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long with scissors, 2g is then taken to be packed into liner polytetrafluoroethyl-ne In the autoclave of alkene.
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, 12 are reacted at 160 DEG C Hour, it is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, reaction is placed again into after cleaning drying In kettle, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 12 hours at 120 DEG C.
（3）Step (2) products therefrom is washed with deionized water to neutrality, is in gas flow by obtained product after drying Charing 0.5 hour is carried out under the nitrogen atmosphere of 45mL/min, carbonization temperature is 700 DEG C, and heating rate is 3 DEG C/min, naturally cold But to after room temperature, sisal fiber charcoal is obtained, grind into powder is for use.
（4）0.2g Macrogol 6000s are added to equipped in the beaker in 30mL distilled water, waiting for Macrogol 6000 point It dissipates in uniformly backward beaker solution and 0.0356g (1.24x10 is added-4Mol ZnSO)4·7H2O, and make its uniform dissolution.
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, at the uniform velocity stir at room temperature It mixes 4 hours.
（6）The NaOH solution of a concentration of 0.0123mol/L of 20mL is slowly dropped to step（5）In acquired solution, make molten Liquid pH is adjusted to 11.7, continues at the uniform velocity to stir 8 hours at room temperature after being added dropwise；Then mixed solution is transferred at 80 DEG C Thermostat water bath in, constant temperature at the uniform velocity stirs lower reaction 50 minutes；Beaker room temperature is taken out after the completion of reaction at the uniform velocity stirs lower cooling, It centrifuges afterwards, remove supernatant, drying, obtain nano zine oxide-sisal fiber Carbon composites.
（7）By step（6）Obtained nano zine oxide-sisal fiber Carbon composites carry out absorption and photocatalysis performance is surveyed Examination, experimental subjects are the methylene blue solution of 5mg/L, and maximum material removal rate is 95.9% (see attached drawing 2).
Embodiment 4：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long with scissors, 2g is then taken to be packed into liner polytetrafluoroethyl-ne In the autoclave of alkene.
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, 12 are reacted at 160 DEG C Hour, it is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, reaction is placed again into after cleaning drying In kettle, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 12 hours at 120 DEG C.
（3）Step (2) products therefrom is washed with deionized water to neutrality, is in gas flow by obtained product after drying Charing 0.5 hour is carried out under the nitrogen atmosphere of 45mL/min, carbonization temperature is 700 DEG C, and heating rate is 3 DEG C/min, naturally cold But to after room temperature, sisal fiber charcoal is obtained, grind into powder is for use.
（4）0.2g Macrogol 6000s are added to equipped in the beaker in 30mL distilled water, waiting for Macrogol 6000 point It dissipates in uniformly backward beaker solution and 0.0430g (1.50x10 is added-5Mol ZnSO)4·7H2O, and make its uniform dissolution.
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, at the uniform velocity stir at room temperature It mixes 4 hours.
（6）The NaOH solution of a concentration of 0.0150mol/L of 20mL is slowly dropped to step（5）In acquired solution, make molten Liquid pH is adjusted to 11.8, continues at the uniform velocity to stir 8 hours at room temperature after being added dropwise；Then mixed solution is transferred at 80 DEG C Thermostat water bath in, constant temperature at the uniform velocity stirs lower reaction 50 minutes；Beaker room temperature is taken out after the completion of reaction at the uniform velocity stirs lower cooling, It centrifuges afterwards, remove supernatant, drying, obtain nano zine oxide-sisal fiber Carbon composites.
（7）By step（6）Obtained nano zine oxide-sisal fiber Carbon composites field emission microscopy observation, The pattern of middle sisal carbon is " spring-like " and " spherical ", and the pattern for being attached to the nano-ZnO in sisal carbon is " spherical shape ", average grain Diameter is 90 nm（See attached drawing 3）.
（8）By step（6）It obtains nano zine oxide-sisal fiber Carbon composites and carries out absorption and photocatalysis performance test, Experimental subjects is the methylene blue solution of 5mg/L, and maximum material removal rate is 98.7% (see attached drawing 2).
Embodiment 5：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long with scissors, 2g is then taken to be packed into liner polytetrafluoroethyl-ne In the autoclave of alkene.
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, 12 are reacted at 160 DEG C Hour, it is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, reaction is placed again into after cleaning drying In kettle, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 12 hours at 120 DEG C.
（3）Step (2) products therefrom is washed with deionized water to neutrality, is in gas flow by obtained product after drying Charing 0.5 hour is carried out under the nitrogen atmosphere of 45mL/min, carbonization temperature is 700 DEG C, and heating rate is 3 DEG C/min, naturally cold But to after room temperature, sisal fiber charcoal is obtained, grind into powder is for use.
（4）0.2g Macrogol 6000s are added to equipped in the beaker in 30mL distilled water, waiting for Macrogol 6000 point It dissipates in uniformly backward beaker solution and 0.0554g (1.93x10 is added-4Mol ZnSO)4·7H2O, and make its uniform dissolution.
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, at the uniform velocity stir at room temperature It mixes 4 hours.
（6）The NaOH solution of a concentration of 0.0180mol/L of 20mL is slowly dropped to step（5）In acquired solution, make molten Liquid pH is adjusted to 11.9, continues at the uniform velocity to stir 8 hours at room temperature after being added dropwise；Then mixed solution is transferred at 80 DEG C Thermostat water bath in, constant temperature at the uniform velocity stirs lower reaction 50 minutes；Beaker room temperature is taken out after the completion of reaction at the uniform velocity stirs lower cooling, It centrifuges afterwards, remove supernatant, drying, obtain nano zine oxide-sisal fiber Carbon composites.
（7）By step（6）It obtains nano zine oxide-sisal fiber Carbon composites and carries out absorption and photocatalysis performance test, Experimental subjects is the methylene blue solution of 5mg/L, and maximum material removal rate is 93.2% (see attached drawing 2).
Embodiment 6：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long with scissors, 2g is then taken to be packed into liner polytetrafluoroethyl-ne In the autoclave of alkene.
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, 12 are reacted at 160 DEG C Hour, it is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, reaction is placed again into after cleaning drying In kettle, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 12 hours at 120 DEG C.
（3）Step (2) products therefrom is washed with deionized water to neutrality, is in gas flow by obtained product after drying Charing 0.5 hour is carried out under the nitrogen atmosphere of 45mL/min, carbonization temperature is 700 DEG C, and heating rate is 3 DEG C/min, naturally cold But to after room temperature, sisal fiber charcoal is obtained, grind into powder is for use.
（4）0.2g Macrogol 6000s are added to equipped in the beaker in 30mL distilled water, waiting for Macrogol 6000 point It dissipates in uniformly backward beaker solution and 0.0887g (3.08x10 is added-4Mol ZnSO)4·7H2O, and make its uniform dissolution.
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, at the uniform velocity stir at room temperature It mixes 4 hours.
（6）The NaOH solution of a concentration of 0.0307mol/L of 20mL is slowly dropped to step（5）In acquired solution, make molten Liquid pH is adjusted to 12.1, continues at the uniform velocity to stir 8 hours at room temperature after being added dropwise；Then mixed solution is transferred at 80 DEG C Thermostat water bath in, constant temperature at the uniform velocity stirs lower reaction 50 minutes；Beaker room temperature is taken out after the completion of reaction at the uniform velocity stirs lower cooling, It centrifuges afterwards, remove supernatant, drying, obtain nano zine oxide-sisal fiber Carbon composites.
（7）By step（6）It obtains nano zine oxide-sisal fiber Carbon composites and carries out absorption and photocatalysis performance test, Experimental subjects is the methylene blue solution of 5mg/L, and maximum material removal rate is 94.8% (see attached drawing 2).

Claims (1)

1. a kind of preparation method of nano zine oxide-sisal fiber Carbon composites, it is characterised in that the specific steps are：
（1）The sisal fiber cleaned and dried is cut into the segment of 2cm long, 2g is then taken to be packed into the height of inner liner polytetrafluoroethylene It presses in reaction kettle；
（2）The hydrochloric acid solution of a concentration of 1mol/L of 75mL is added to step（1）In reaction kettle, it is small that 10-24 is reacted at 160 DEG C When, it is filtered after the completion of reaction, takes the solid on filter paper and be washed with deionized water to neutrality, dried after cleaning and be placed again into reaction kettle In, the hydrazine hydrate dilute solution of a concentration of 1.65mol/L of 75mL is added, is reacted 10-24 hours at 120 DEG C；
（3）Step (2) products therefrom is washed with deionized water to neutrality, is carried out obtained product in a nitrogen atmosphere after drying Charing 0.5-1 hour, carbonization temperature are 650-750 DEG C, and heating rate is 1-5 DEG C/min, after cooled to room temperature, obtains sword Flaxen fiber charcoal, grind into powder are for use；
（4）0.2g polyethylene glycol is added to equipped in the beaker in 30mL distilled water, to burning after polyethylene glycol is uniformly dispersed It is added 1.50 × 10 in cup solution-5-3.08×10-4The water-soluble zinc salt of mol, and make its uniform dissolution；
（5）By 0.5g steps（3）Obtained sisal fiber charcoal is added to step（4）In acquired solution, 4-8 is at the uniform velocity stirred at room temperature Hour；
（6）The NaOH solution of a concentration of 0.0015-0.0307mol/L of 20mL is slowly dropped to step（5）In acquired solution, make PH value of solution is adjusted to 10.7-12.1, continues at the uniform velocity to stir 8-12 hours at room temperature after being added dropwise；Then mixed solution is turned It moves in the thermostat water bath at 70 DEG C -90 DEG C, constant temperature at the uniform velocity stirs lower reaction 30-90 minutes；Beaker is taken out after the completion of reaction Room temperature at the uniform velocity stirs lower cooling, and rear centrifugation, removal supernatant, drying obtain nano zine oxide-sisal fiber Carbon composites；
The molecular weight polyethylene glycol is one kind in 6000,4000 and 2000；
The water-soluble zinc salt is one kind in zinc sulfate, zinc nitrate, zinc acetate and zinc chloride.
CN201810079950.6A 2018-01-27 2018-01-27 A kind of preparation method of nano zine oxide-sisal fiber Carbon composites Pending CN108452767A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109529785A (en) * 2018-11-20 2019-03-29 浙江理工大学 A kind of have both adjusts pattern and the ultrafast Cellulose nanocrystal/zinc oxide composite preparation method for absorbing the dye of positive ion
CN110201660A (en) * 2019-06-19 2019-09-06 塔里木大学 A kind of zinc oxide/cotton stalk biomass carbon composite material and preparation method and application
US11472715B2 (en) 2020-10-23 2022-10-18 King Faisal University Method of making carbon-zinc oxide nanoparticles
CN115893473A (en) * 2022-11-09 2023-04-04 福州大学 Alcohol gas-sensitive material based on ZnO and activated carbon composite, and preparation method and application thereof
US20230311096A1 (en) * 2022-02-11 2023-10-05 Qingdao University Of Science And Technology Active zinc-based catalyst and preparation method thereof, and use in catalyzing rearrangement reaction of ibuprofen

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101947442A (en) * 2010-09-07 2011-01-19 桂林理工大学 Method for synthesizing nano zinc oxide/bamboo charcoal photocatalysis material by precipitation and impregnation
CN102432377A (en) * 2011-09-16 2012-05-02 桂林理工大学 Hydro-thermal synthetic method for nanometer selenium/sisal carbon fiber composite material used for preservation
CN106450314A (en) * 2016-11-19 2017-02-22 桂林理工大学 Spring-shaped SFC (sisal fiber carbon) and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101947442A (en) * 2010-09-07 2011-01-19 桂林理工大学 Method for synthesizing nano zinc oxide/bamboo charcoal photocatalysis material by precipitation and impregnation
CN102432377A (en) * 2011-09-16 2012-05-02 桂林理工大学 Hydro-thermal synthetic method for nanometer selenium/sisal carbon fiber composite material used for preservation
CN106450314A (en) * 2016-11-19 2017-02-22 桂林理工大学 Spring-shaped SFC (sisal fiber carbon) and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109529785A (en) * 2018-11-20 2019-03-29 浙江理工大学 A kind of have both adjusts pattern and the ultrafast Cellulose nanocrystal/zinc oxide composite preparation method for absorbing the dye of positive ion
CN110201660A (en) * 2019-06-19 2019-09-06 塔里木大学 A kind of zinc oxide/cotton stalk biomass carbon composite material and preparation method and application
US11472715B2 (en) 2020-10-23 2022-10-18 King Faisal University Method of making carbon-zinc oxide nanoparticles
US20230311096A1 (en) * 2022-02-11 2023-10-05 Qingdao University Of Science And Technology Active zinc-based catalyst and preparation method thereof, and use in catalyzing rearrangement reaction of ibuprofen
US11826726B2 (en) * 2022-02-11 2023-11-28 Qingdao University Of Science And Technology Active zinc-based catalyst and preparation method thereof, and use in catalyzing rearrangement reaction of ibuprofen
CN115893473A (en) * 2022-11-09 2023-04-04 福州大学 Alcohol gas-sensitive material based on ZnO and activated carbon composite, and preparation method and application thereof

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