CN102000607A - Method for preparing nano ZnO supported pre-oxidized ramie fiber photocatalyst - Google Patents
Method for preparing nano ZnO supported pre-oxidized ramie fiber photocatalyst Download PDFInfo
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Abstract
A method for preparing a nano ZnO supported pre-oxidized ramie fiber photocatalyst belongs to the technical field of photocatalysts. The method is characterized by taking zinc acetate dihydrate, sodium hydroxide and ethanol as the raw materials to prepare nano ZnO sol which has uniform granules and is stably dispersed, successfully supporting the nano ZnO sol on the ramie fibers and preparing the nano ZnO supported pre-oxidized ramie fiber photocatalyst after high temperature calcination. The method is simple to operate and the prepared photocatalyst can degrade the pollutants to nontoxic compounds.
Description
Technical field
The present invention relates to the pre-oxygen mercerising of a kind of loaded with nano ZnO flaxen fiber Preparation of catalysts method, belong to the photocatalyst technology field.
Background technology
The conductor photocatalysis oxidation technology has characteristics such as energy consumption is low, easy to operate, non-secondary pollution, has shown wide application prospect in the environmental improvement field.Multiphase photocatalysis reacts in the employed semiconductor catalyst, and ZnO is nontoxic because of it, catalytic activity is high, oxidability is strong, the advantage of good stability is most widely used.The nano-ZnO particle has tangible skin effect and size quantization effect, thereby shows extraordinary redox ability under light action, and photocatalysis efficiency is improved greatly.But generally the nano-ZnO suspended phase photochemical catalyst of Cai Yonging exists easy inactivation, easy shortcoming such as cohesion and difficult recovery, is not suitable for current system, has seriously limited application and the development of this system aspect water treatment.The effective ways that overcome this shortcoming are preparation loaded photocatalysts, compare with the suspended ZnO system, and the liquid-solid separation of support type ZnO system is more or less freely, and therefore recyclable and repeated use more likely is applied to reality.Selection for nano-ZnO load matrix, should note several problems: at first, avoid selected matrix that the performance of nano-ZnO function is not had influence even plays inhibition, the desirable selection is to have brought into play synergy to the function of nano-ZnO, promotes carrying out smoothly of its photocatalytic process; Secondly, selected matrix itself has the good adsorption performance, can accelerate the absorption degradation of loaded photocatalyst to pollutant; At last, selecting for use of load matrix should be standard not increase second environmental pollution, and natural fiber is a kind of good selection.
In various natural fibers, bast-fibre is cheap, recyclability good, distribution is wide, also have powerful high, moisture absorption loose wet fast, absorption property is good, antibacterial, mildew-resistant, anticorrosion, radiation proof, characteristics such as antistatic, can be described as the high-performance natural fiber, simultaneously, flaxen fiber is environmentally friendly as natural fiber, and is pollution-free, degradable has a extensive future.Ramee more is called as " China's grass " in the world, is important textile fabric crop.At present, to the existing a lot of bibliographical informations of the Photocatalytic Performance Study of nano ZnO powder, but the research of support type ZnO system is also rare, and the research that nano-ZnO is loaded on the flaxen fiber yet there are no report.
Summary of the invention
The objective of the invention is to give flaxen fiber some good properties on the environmentally friendly and biodegradable basis, develop a kind of pre-oxygen mercerising of loaded with nano ZnO flaxen fiber Preparation of catalysts method simple for production.
The present invention adopts the carrier of ramee as nano-ZnO, both can carry out part absorption to pollutant in photocatalytic process, and self can biodegradation not produce secondary pollution to environment again, thereby has realized purpose of the present invention.
Technical scheme of the present invention: the pre-oxygen mercerising of a kind of loaded with nano ZnO flaxen fiber Preparation of catalysts method, preparation process is as follows:
(1) 20:15 ~ 20:20 takes by weighing Zinc diacetate dihydrate and NaOH respectively in molar ratio; The ratio dissolving that is dissolved in 10 ~ 100mL absolute ethyl alcohol in the 1g Zinc diacetate dihydrate obtains zinc acetate/ethanolic solution, and the ratio dissolving that 0.2g NaOH is dissolved in 10 ~ 100mL absolute ethyl alcohol obtains sodium hydroxide/ethyl alcohol solution; Be heated to 30 ~ 60 ℃ respectively, under intense stirring condition, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution; Continue to be stirred to solution after sodium hydroxide/ethyl alcohol solution dropwises and be cooled to the nano-ZnO colloidal sol that room temperature can obtain stably dispersing;
(2) flaxen fiber being carried out alkali treatment, is 60 ~ 80 ℃ of insulation dipping 1 ~ 2h in 2 ~ 5% the sodium hydroxide solution in mass concentration;
(3) flaxen fiber with step (2) processing gained is immersed in the nano-ZnO colloidal sol for preparing, soaking into the back fully takes out 60 ~ 100 ℃ of oven dry down, in Muffle furnace, slowly be warming up to 100 ~ 200 ℃ again and calcined 1 ~ 2 hour down, promptly obtain the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber catalyst.
Described flaxen fiber is a ramee.
Described 20:18 ~ the 20:19 in molar ratio of step (1) takes by weighing analytically pure Zinc diacetate dihydrate and NaOH respectively.
Dropping, the hybrid reaction of the described sodium hydroxide/ethyl alcohol solution of step (1) and zinc acetate/ethanolic solution are carried out under 35 ~ 45 ℃ temperature conditions.
The described flaxen fiber that flooded nano-ZnO colloidal sol of step (3) is dried under 70 ~ 80 ℃ temperature conditions.
The flaxen fiber that is impregnated with nano-ZnO colloidal sol after the described oven dry of step (3) was calcined 2 hours under 130 ~ 140 ℃ in Muffle furnace.
Described flaxen fiber is a ramee.
Preferred plan of the present invention: 20:18 is that 10:9 takes by weighing analytically pure Zinc diacetate dihydrate and NaOH respectively in molar ratio, be dissolved in the ratio dissolving of 100mL absolute ethyl alcohol then in the 1g Zinc diacetate dihydrate, be dissolved in the ratio dissolving of 500mL absolute ethyl alcohol in 1g NaOH, the dissolving back is under 40 ℃ of intense agitation, with sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise join and make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continue to be stirred to solution and be cooled to the nano-ZnO colloidal sol that room temperature can obtain stably dispersing.Will be through being that the ramee that 80 ℃ of dippings of insulation 1h carry out alkali treatment in 5% the sodium hydroxide solution is immersed in the nano-ZnO colloidal sol for preparing at mass fraction, take out behind the certain hour 80 ℃ of oven dry down, in Muffle furnace, slowly be warming up to 140 ℃ again and calcined 2 hours down, promptly obtain the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber catalyst.
Beneficial effect of the present invention:
(1) simple to operate: as to adopt simple sol-gel technique.
(2) can obtain the less nano-ZnO colloidal sol of particle, and nano-ZnO is successfully loaded on the ramee.
(3) the pre-oxygen mercerising of the loaded with nano ZnO flaxen fiber catalyst photocatalytic activity height for preparing, can be used for contaminant degradation is non-toxic compound.
Description of drawings
Fig. 1 is mol (Zn
2+): mol (Na
+Nano-ZnO grading curve during)=10:9.
Fig. 2 is calcining back loading nano-ZnO ramee sem photograph (2000 times).
Fig. 3 is calcining back loading nano-ZnO ramee energy spectrum analysis figure.
Fig. 4 is the pre-oxygen mercerising of a loaded with nano ZnO ramee catalyst photocatalytic degradation curve, (a) the test sample: methylene blue solution concentration: 5mg/L, the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber catalytic amount: 10g/L; (b) blank sample.
The specific embodiment
Embodiment 1:
20:15 takes by weighing 0.219g Zinc diacetate dihydrate and 0.03g NaOH in molar ratio, be dissolved in respectively in each 20ml ethanol solution and dissolve, the dissolving back is under 40 ℃ of intense agitation, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continues agitating solution and is cooled to room temperature and promptly obtains nano-ZnO colloidal sol.The average grain diameter of measuring gained nano-ZnO colloidal sol through the nano particle size analyzer is 100.1nm.
Embodiment 2:
20:16 takes by weighing 0.219g Zinc diacetate dihydrate and 0.032g NaOH in molar ratio, be dissolved in respectively in each 30ml ethanol solution and dissolve, the dissolving back is under 40 ℃ of intense agitation, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continues agitating solution and is cooled to room temperature and promptly obtains nano-ZnO colloidal sol.The average grain diameter of measuring gained nano-ZnO colloidal sol through the nano particle size analyzer is 99.6nm.
Embodiment 3:
20:17 takes by weighing 0.219g Zinc diacetate dihydrate and 0.034g NaOH in molar ratio, be dissolved in respectively in each 40ml ethanol solution and dissolve, the dissolving back is under 40 ℃ of intense agitation, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continues agitating solution and is cooled to room temperature and promptly obtains nano-ZnO colloidal sol.The average grain diameter of measuring gained nano-ZnO colloidal sol through the nano particle size analyzer is 80.1nm.
Embodiment 4:
20:18 takes by weighing 0.219g Zinc diacetate dihydrate and 0.036g NaOH in molar ratio, be dissolved in respectively in each 20ml ethanol solution and dissolve, the dissolving back is under 40 ℃ of intense agitation, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continues agitating solution and is cooled to room temperature and promptly obtains nano-ZnO colloidal sol.The average grain diameter of measuring gained nano-ZnO colloidal sol through the nano particle size analyzer is 56.3nm.See Fig. 1
Embodiment 5:
20:19 takes by weighing 0.219g Zinc diacetate dihydrate and 0.038g NaOH in molar ratio, be dissolved in respectively in each 50ml ethanol solution and dissolve, the dissolving back is under 40 ℃ of intense agitation, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continues agitating solution and is cooled to room temperature and promptly obtains nano-ZnO colloidal sol.The average grain diameter of measuring gained nano-ZnO colloidal sol through the nano particle size analyzer is 85.7nm.
Embodiment 6:
20:20 takes by weighing 0.219g Zinc diacetate dihydrate and 0.04g NaOH in molar ratio, be dissolved in respectively in each 60ml ethanol solution and dissolve, the dissolving back is under 40 ℃ of intense agitation, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution, treat that sodium hydroxide/ethyl alcohol solution dropwises, continues agitating solution and is cooled to room temperature and promptly obtains nano-ZnO colloidal sol.The average grain diameter of measuring gained nano-ZnO colloidal sol through the nano particle size analyzer is 110.2nm.
Embodiment 7:
Is that 80 ℃ of dippings of insulation 1h carry out alkali treatment in 5% the sodium hydroxide solution with ramee at mass fraction, is immersed in Zn then
2+And Na
+20:18 is in the nano-ZnO colloidal sol that makes of embodiment 4 in molar ratio, soaks into the back fully and takes out 80 ℃ of oven dry down, slowly is warming up to 140 ℃ of calcinings 2 hours down again in Muffle furnace, obtains the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber catalyst.See Fig. 2,3.
Application Example 1 is carried out the photocatalytic degradation experiment in homemade photocatalytic degradation experimental provision
Preparation 5mg/L methylene blue solution is regulated pH to 9, adds the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber catalyst 10 g/L that made by embodiment 7, fully stirs, and adsorbs in advance in the dark 1 hour, makes to reach adsorption equilibrium.Solution is placed reaction under the 28W ultra violet lamp, light source is apart from liquid level 25cm, continue air blast, stirring in the course of reaction, 20min sampling at interval, get a certain amount of supernatant and survey its absorbance at methylene blue maximum absorption wavelength 664nm place with ultraviolet-uisible spectrophotometer, according to the variation of absorbance before and after the illumination, ask its degradation rate again.See Fig. 4.
Claims (6)
1. the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber Preparation of catalysts method is characterized in that preparation process is as follows:
(1) 20:15 ~ 20:20 takes by weighing Zinc diacetate dihydrate and NaOH respectively in molar ratio; The ratio dissolving that is dissolved in 10 ~ 100mL absolute ethyl alcohol in the 1g Zinc diacetate dihydrate obtains zinc acetate/ethanolic solution, and the ratio dissolving that 0.2g NaOH is dissolved in 10 ~ 100mL absolute ethyl alcohol obtains sodium hydroxide/ethyl alcohol solution; Be heated to 30 ~ 60 ℃ respectively, under intense stirring condition, sodium hydroxide/ethyl alcohol solution at the uniform velocity, slowly, dropwise joined make its abundant hybrid reaction in zinc acetate/ethanolic solution; Continue to be stirred to solution after sodium hydroxide/ethyl alcohol solution dropwises and be cooled to the nano-ZnO colloidal sol that room temperature can obtain stably dispersing;
(2) flaxen fiber being carried out alkali treatment, is 60 ~ 80 ℃ of insulation dipping 1 ~ 2h in 2 ~ 5% the sodium hydroxide solution in mass concentration;
(3) flaxen fiber with step (2) processing gained is immersed in the nano-ZnO colloidal sol for preparing, soaking into the back fully takes out 60 ~ 100 ℃ of oven dry down, in Muffle furnace, slowly be warming up to 100 ~ 200 ℃ of calcining 1 ~ 2h down again, promptly obtain the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber catalyst.
2. the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber according to claim 1 Preparation of catalysts method is characterized in that the described 20:18 ~ 20:19 in molar ratio of step (1) takes by weighing analytically pure Zinc diacetate dihydrate and NaOH respectively.
3. the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber according to claim 1 Preparation of catalysts method is characterized in that dropping, the hybrid reaction of the described sodium hydroxide/ethyl alcohol solution of step (1) and zinc acetate/ethanolic solution carried out under 35 ~ 45 ℃ temperature conditions.
4. the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber according to claim 1 Preparation of catalysts method is characterized in that the described flaxen fiber that flooded nano-ZnO colloidal sol of step (3) dries under 70 ~ 80 ℃ temperature conditions.
5. the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber according to claim 1 Preparation of catalysts method is characterized in that the flaxen fiber that is impregnated with nano-ZnO colloidal sol after the described oven dry of step (3) was calcined 2 hours under 130 ~ 140 ℃ in Muffle furnace.
6. the pre-oxygen mercerising of loaded with nano ZnO flaxen fiber according to claim 1 Preparation of catalysts method is characterized in that described flaxen fiber is a ramee.
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Cited By (3)
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| CN109267323A (en) * | 2018-08-31 | 2019-01-25 | 谭亚 | A kind of preparation method of antiultraviolet umbrella cloth |
| CN111086312A (en) * | 2019-12-04 | 2020-05-01 | 江阴芗菲服饰有限公司 | Anti-ultraviolet composite knitted fabric and processing method thereof |
| CN114775266A (en) * | 2022-05-12 | 2022-07-22 | 东华大学 | Zinc oxide-loaded antibacterial blood-like ultrashort fiber and preparation method and application thereof |
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| CN101011656A (en) * | 2007-01-26 | 2007-08-08 | 福建师范大学 | Preparing method of zinc oxide nano fiber film used as photocatalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109267323A (en) * | 2018-08-31 | 2019-01-25 | 谭亚 | A kind of preparation method of antiultraviolet umbrella cloth |
| CN111086312A (en) * | 2019-12-04 | 2020-05-01 | 江阴芗菲服饰有限公司 | Anti-ultraviolet composite knitted fabric and processing method thereof |
| CN114775266A (en) * | 2022-05-12 | 2022-07-22 | 东华大学 | Zinc oxide-loaded antibacterial blood-like ultrashort fiber and preparation method and application thereof |
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