CN104785237B - A kind of method that loose acicular type zinc oxide is prepared by template of cotton fiber - Google Patents
A kind of method that loose acicular type zinc oxide is prepared by template of cotton fiber Download PDFInfo
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- CN104785237B CN104785237B CN201510150060.6A CN201510150060A CN104785237B CN 104785237 B CN104785237 B CN 104785237B CN 201510150060 A CN201510150060 A CN 201510150060A CN 104785237 B CN104785237 B CN 104785237B
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- cotton fiber
- zinc oxide
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- type zinc
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Abstract
The invention discloses a kind of method that loose acicular type zinc oxide is prepared by template of cotton fiber, belong to the synthesis technical field of inorganic functional material zinc oxide.Technical scheme main points are:A kind of method that loose acicular type zinc oxide is prepared by template of cotton fiber, comprises the following steps:The 6h of cotton fiber 1 is impregnated after 80 120 DEG C of drying for standby with the sodium hydroxide solution dipping 10h of cotton fiber 4 that molar concentration is 1 6mol/L or with the ammonia spirit that molar concentration is 2 6mol/L;Treated cotton fiber is immersed in zinc nitrate and 2 10h in the colloidal sol of citric acid formation, is then dried in 60 90 DEG C and extremely forms gel;Gel is warming up to 400 600 DEG C of calcining 2h with 1 10 DEG C/min heating rate in temperature programming stove loose acicular type zinc oxide is made.The present invention using sol-gel process and adjusts response parameter and has synthesized the loose acicular type zinc oxide with high efficiency photocatalysis activity and air-sensitive performance using cotton fiber as template.
Description
Technical field
The invention belongs to the synthesis technical field of inorganic functional material zinc oxide, and in particular to one kind is using cotton fiber as template
The method for preparing loose acicular type zinc oxide.
Background technology
Developing rapidly for chemical industry brings huge environmental problem, and water pollution is an important side of environmental pollution
Face, compared with traditional water technology, photocatalysis technology has that environment-friendly, operating condition is easily-controllable and pollutant removal is thorough
The advantages of, the quality of catalyst performance directly affects photocatalysis effect in photocatalytic process.
Usually need to examine some poisonous and harmful, flammable explosive gas in industrial and agricultural production and people's life in addition
Survey, with the generation of accident prevention.Therefore, the gas sensor material with low cost, fast response, high sensitivity and high selectivity is
Current people are to one of study hotspot of gas sensor, as detecting concentration of alcohol in driver's drunk driving and industrial and agricultural production
Ethanol sensor is constantly subjected to the attention of researcher.
Zinc oxide is a kind of novel inorganic functional material, be widely used in solar cell, photocatalysis, gas sensor and
The fields such as light emitting diode.Due to the structure of material(Micro-structural), the factor such as size and pattern has to the performance of material and application
There is important influence, thus it is gentle to improving its photocatalysis performance using the zinc oxide of different preparation method synthesis specific morphologies
Quick performance has great importance.
Biological template method is a kind of new method for preparing material for having merged life science and material science and having grown up,
Biological template method has the advantages that a lot compared with traditional method, and such as reaction condition is gentle, preparation technology is simple, price is low
Honest and clean, process is easily controllable and can obtain the complex topography structure that general chemistry method can not be obtained.Some documents are had at present
Report prepares zinc oxide using biological template method, and mesoporous shape zinc oxide is such as prepared by template of lignin, is closed by template of paper
Into Nanometer-sized Rods ZnO and using coccus as templated synthesis hollow spheres zinc oxide etc., cotton fiber is inexpensive relative to other templates easily
Obtain and environment-friendly, relevant report is had no in the method for cotton fiber as biological templated synthesis inorganic functional material zinc oxide.
The content of the invention
Present invention solves the technical problem that a kind of method that loose acicular type zinc oxide is prepared by template of cotton fiber is there is provided,
Loose acicular type zinc oxide has efficient visible light catalytic performance and air-sensitive performance simultaneously made from this method.
The present invention adopts the following technical scheme that one kind prepares pine needle shape by template of cotton fiber to solve above-mentioned technical problem
The method of zinc oxide, it is characterised in that comprise the following steps:(1)The sodium hydroxide solution for being 1-6mol/L with molar concentration impregnates
Cotton fiber 4-10h or the ammonia spirit dipping cotton fiber 1-6h for being 2-6mol/L with molar concentration are standby after 80-120 DEG C of drying
With;(2)Treated cotton fiber is immersed in zinc nitrate and 2-10h in the colloidal sol of citric acid formation, zinc nitrate and citric acid
Mol ratio is 1:1-5, is then dried in 60-90 DEG C to formation gel;(3)By gel in temperature programming stove with 1-10 DEG C/min
Heating rate be warming up to 400-600 DEG C of calcining 2h loose acicular type zinc oxide be made.
Further limit, the pine needle length of obtained loose acicular type zinc oxide is 1-2 μm.
The present invention using sol-gel process and adjusts response parameter and synthesized with efficiency light using cotton fiber as template
The loose acicular type zinc oxide of catalytic activity and air-sensitive performance, the raw material for participating in reaction is cheap and easy to get, environment-friendly, simple to operate, production
Thing high income and photocatalysis performance and air-sensitive performance are preferable.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of loose acicular type zinc oxide made from the embodiment of the present invention 1, and Fig. 2 is that the embodiment of the present invention 1 is made
Loose acicular type zinc oxide degrade under visible light the photocatalytic degradation curve of 10mg/L active black solution, Fig. 3 is of the invention real
Response recovery curve of the loose acicular type zinc oxide under 350 DEG C of operating temperatures to 100ppm ethanol made from example 1 is applied, Fig. 4 is this hair
Sensitivity chart of the loose acicular type zinc oxide under 350 DEG C of operating temperatures to 100ppm gas with various made from bright embodiment 1.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
The sodium hydroxide solution for being 1mol/L with molar concentration impregnates cotton fiber 10h after 90 DEG C of drying for standby;Will processing
Cotton fiber afterwards is immersed in mol ratio for n(Zinc nitrate):n(Citric acid)= 1:8h in 4 colloidal sols formed, it is then dry in 60 DEG C
It is dry extremely to form gel;Gel is finally warming up to 400 DEG C of calcining 2h systems using 1 DEG C/min heating rate in temperature programming stove
Obtain loose acicular type zinc oxide.
Fig. 1 is the scanning electron microscope (SEM) photograph of loose acicular type zinc oxide made from the present embodiment, it can be seen that obtained pine needle
Shape zinc oxide is evenly distributed, and pine needle length is about 1-2 μm;Fig. 2 loose acicular type zinc oxides made from the present embodiment are under visible light
The photocatalytic degradation curve of degraded 10mg/L active black solution, the Photocatalytic Decoloration rate in 60min to dyestuff is 97.69%, can
See that obtained loose acicular type zinc oxide has preferable visible light catalytic performance;Fig. 3 is that loose acicular type zinc oxide exists made from the present embodiment
To the response recovery curve of 100ppm ethanol under 350 DEG C of operating temperatures, calculated by sensitivity definition S=Ra/Rg, the oxidation of pine needle shape
Zinc has higher sensitivity to ethanol, is 584.6, response recovery time is short, respectively 14s and 4s;Fig. 4 is the present embodiment system
Comparison figure of the loose acicular type zinc oxide obtained under 350 DEG C of operating temperatures to 100ppm gas with various sensitivity, according to selective system
Several definition(K A/B =S A /S B , wherein A is alcohol gas, and B is interference gas), can calculate loose acicular type zinc oxide to remaining seven
The selectivity factor of gas is planted, 105 are all higher than, it can be seen that, obtained loose acicular type zinc oxide has stronger resist to other gases
Interference performance, is expected to be further developed as the Alcohol Gas Sensor of high selectivity.
Embodiment 2
The sodium hydroxide solution for being 3mol/L with molar concentration impregnates cotton fiber 8h after 80 DEG C of drying for standby;After handling
Cotton fiber be immersed in mol ratio for n(Zinc nitrate):n(Citric acid)= 1:6h in 5 colloidal sols formed, then in 70 DEG C of dryings
To formation gel;Gel is finally warming up into 500 DEG C of calcining 2h in temperature programming stove using 3 DEG C/min heating rate to be made
Loose acicular type zinc oxide.
Embodiment 3
The sodium hydroxide solution for being 6mol/L with molar concentration impregnates cotton fiber 4h after 100 DEG C of drying for standby;Will processing
Cotton fiber afterwards is immersed in mol ratio for n(Zinc nitrate):n(Citric acid)= 1:4h in 3 colloidal sols formed, it is then dry in 80 DEG C
It is dry extremely to form gel;Gel is finally warming up to 600 DEG C of calcining 2h systems using 5 DEG C/min heating rate in temperature programming stove
Obtain loose acicular type zinc oxide.
Embodiment 4
The ammonia spirit for being 2mol/L with molar concentration impregnates cotton fiber 6h after 110 DEG C of drying for standby;After processing
Cotton fiber is immersed in mol ratio for n(Zinc nitrate):n(Citric acid)= 1:2h in 2 colloidal sols formed, is then dried extremely in 90 DEG C
Form gel;Gel is finally warming up to 400 DEG C of calcining 2h using 7 DEG C/min heating rate in temperature programming stove pine is made
Acicular type zinc oxide.
Embodiment 5
The ammonia spirit for being 4mol/L with molar concentration impregnates cotton fiber 5h after 120 DEG C of drying for standby;After processing
Cotton fiber is immersed in mol ratio for n(Zinc nitrate):n(Citric acid)= 1:10h in 1 colloidal sol formed, is then dried extremely in 75 DEG C
Form gel;Gel is finally warming up to 500 DEG C of calcining 2h using 8 DEG C/min heating rate in temperature programming stove pine is made
Acicular type zinc oxide.
Embodiment 6
The ammonia spirit for being 6mol/L with molar concentration impregnates cotton fiber 1h after 80 DEG C of drying for standby;By the cotton after processing
Fiber impregnation is n in mol ratio(Zinc nitrate):n(Citric acid)= 1:3h in 3 colloidal sols formed, is then dried to shape in 85 DEG C
Into gel;Gel is finally warming up to 600 DEG C of calcining 2h using 10 DEG C/min heating rate in temperature programming stove pine is made
Acicular type zinc oxide.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of method that loose acicular type zinc oxide is prepared by template of cotton fiber, it is characterised in that comprise the following steps:(1)With rubbing
Sodium hydroxide solution dipping cotton fiber 4-10h or the ammonia spirit for being 2-6mol/L with molar concentration that your concentration is 1-6mol/L
Cotton fiber 1-6h is impregnated after 80-120 DEG C of drying for standby;(2)Treated cotton fiber is immersed in zinc nitrate and citric acid shape
Into colloidal sol in 2-10h, the mol ratio of zinc nitrate and citric acid is 1:1-5, is then dried in 60-90 DEG C to formation gel;(3)
Gel is warming up to 400-600 DEG C of calcining 2h with 1-10 DEG C/min heating rate in temperature programming stove the oxidation of pine needle shape is made
Zinc.
2. the method according to claim 1 that loose acicular type zinc oxide is prepared by template of cotton fiber, it is characterised in that:It is made
Loose acicular type zinc oxide pine needle length be 1-2 μm.
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