CN102527346A - Method for preparing magnetic carbon nanotube/crosslinked chitosan composite nanomaterial adsorbent - Google Patents
Method for preparing magnetic carbon nanotube/crosslinked chitosan composite nanomaterial adsorbent Download PDFInfo
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Abstract
The invention relates to a method for preparing magnetic carbon nanotube/crosslinked chitosan composite nanomaterial adsorbent. According to the invention, a carbon nanotube original sample is adopted as a raw material; the magnetic performance of metal catalyst particles residual in the carbon nanotube original sample and the high-efficiency selective adsorption performance of the carbon nanotube are fully utilized; the adsorption performance of the material is significantly improved through compositing with biological material chitosan; therefore, the magnetic composite nanomaterial adsorbent with high efficiency in adsorbing dye in water phase is obtained. The magnetic composite nanomaterial adsorbent obtained in the invention has the advantages that: the carbon nanotube has no need to adopt strong acid treatment so that the structural integrity of the carbon nanotube is protected; the magnetic performance of the metal catalyst particles residual in the original sample is utilized so that additional process is not needed for composition of magnetic particles; moreover, the crosslinked chitosan has good biocompatibility to benefit the toxicity reduction of nanomaterial and potential biological application; and the obtained nano composite adsorbent can be conveniently and rapidly separated and recycled by adopting magnetic separation technology, so that secondary environmental pollution is avoided.
Description
Technical field
The invention belongs to the new technical field of function materials of environment nanometer; Be specifically related to a kind of magnetic carbon nano-tube/cross-linked chitosan composite nano materials preparation of adsorbent method; This adsorbent is used for the quick absorption of aqueous solution dyestuff to be removed, and guarantees simultaneously can pass through externally-applied magnetic field Separation and Recovery from the aqueous solution after the adsorbent powder uses.
Background technology
Along with the fast development of China's printing and dyeing industry and chemical industry, at present annual nearly 6 ~ 700,000,000 tons of dyeing waste waters enter in the environment, and waste water from dyestuff has become one of environment major polluting sources.Dye industry is various in style, complex process, and waste water from dyestuff has that component complicacy, colourity are high, COD and BOD concentration is high, suspension is many, water quality and the water yield changes greatly, characteristics such as more than the hard-degraded substance, is one of more unmanageable industrial wastewater.It is handled the focus that becomes the environmental protection concern day by day accordingly.The method that dye wastewater treatment using commonly used is gone up in industry at present has methods such as flocculation sediment, oxidation, absorption, biodegradation.With respect to other processing methods; Absorption method has that cost is low, efficient is high, simple to operation and to advantage such as noxious material is insensitive; Be considered to be superior to other dye wastewater treatment technology, thereby be adsorbed on to handle in the organic matter pollutant effluents comprise waste water from dyestuff and have a wide range of applications.
CNT (CNTs) has advantages such as specific area is big, adsorption capacity is big, can be used as a kind of novel sorbing material, has caused that people pay close attention to widely.With traditional sorbing material, to compare like active carbon, clay, CNT is more attractive because of advantages such as its excellent adsorption effect, stable physical chemistry structure, selectivity.Yet because CNTs is fine powder shape sample, how separation of C NTs becomes the difficult problem of CNT in practical application from the aqueous solution.In case the CNTs of absorption toxic pollutant gets in the ecological environment, will bring more serious secondary environmental pollution problem.Shitosan is to be obtained through deacetylation by the chitin that nature extensively exists; Chemical name is polydextrose amine (1-4)-2-amino-B-D glucose; Having excellent biological functionality and compatibility, blood compatibility, security, microbic resolvability etc. can; By all trades and professions extensive concern, have a wide range of applications at numerous areas such as medicine, food, chemical industry, cosmetics, water treatment, METAL EXTRACTION and recovery, biochemistry and biomedical engineerings.In the last few years; Magnetic adsorbent is paid close attention to because be easy to separate received widely; Many technology have been widely used in heavy metal ion, dyestuff, petroleum pollution etc., and adopting magnetic separation technique from water body, to separate tiny CNT, to have a cost low, simple operation and other advantages.Yet shortcomings such as traditional magnetic carbon nano-tube adsorbent prepares and has complex process, can't in acid solution, use; Though the magnetic carbon nano-tube after the load can reclaim through the mode of Magnetic Isolation; But still exist with fine powder shape form; The problem that still has bio-toxicity; Therefore it is good to develop bio-compatibility, and the high power capacity novel magnetic carbon nanotube adsorption agent that can in acid solution, use is promoted and had very important significance reduction adsorbent cost, raising adsorption capacity, life-saving, promotion practicability.
Summary of the invention
The objective of the invention is to base oneself upon that bio-compatibility is good, the demand of high power capacity, the research and development of low-cost magnetic carbon nano-tube adsorbent provides a kind of magnetic carbon nano-tube/cross-linked chitosan composite nano materials preparation of adsorbent method.
The present invention adopts the CNT primary sample as raw material; Made full use of the efficient selective absorption property that magnetic behavior and CNT had that the metal remained catalyst granules is had in the CNT primary sample; Compound through with the biomaterial shitosan significantly improves the absorption property of material, prepares the magnetic composite nano adsorbent with efficient absorption aqueous phase dyestuff; Be implemented in effective Magnetic Isolation effect in the aqueous solution; Said method has been avoided in the traditional magnetic made of carbon nanotubes, and at first purifying is removed metallic catalyst iron particle, the complex process of the carbon tube-surface carried magnetic ferric oxide particles behind purifying then in the primary sample; The method cost is low, and technology is simple.And cross-linked chitosan has excellent biological compatibility; Help the reduction of nano material toxicity; Through crosslinking Treatment the stability of shitosan in acid solution is provided, thus guarantee magnetic carbon nano-tube/cross-linked chitosan composite nano materials adsorbent can be in acid solution stable existence.The gained nano-compound adsorbent can adopt magnetic separation technique to separate quickly and easily, reclaim, and avoids causing secondary environmental pollution.In addition, raw material of the present invention is simple and easy to, preparation technology is simple, condition is prone to control, with low cost, be suitable for serialization extensive, produce in batches.
Magnetic carbon nano-tube/cross-linked chitosan composite nano materials preparation of adsorbent method that the present invention proposes, concrete steps are following:
(1) take by weighing 0.1-1g shitosan and 0.1-1g CNT in beaker, adding mass fraction is in the dilute acetic acid solution of 1%-5%, stirs 5-10min, makes to mix;
(2) add 0.1-0.6g carbonate, it is even to be stirred to bubble; Continue to add 1-25ml formalin, stir 5min, leave standstill 10min behind the mixing;
(3) post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10;
(4) add the 1-10ml epoxychloropropane, under 60-90 ℃ of condition, reaction 2-8h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 5-30min;
(5) adopt sodium hydroxide solution cyclic washing, suction filtration when the pH value of solution value is neutrality, to end; Vacuum drying promptly gets required product.
Among the present invention, used not purifying carbon nano-tube primary sample, its sample can be chemical vapour deposition technique, laser method or arc process and prepare unpurified CNT primary sample.
Among the present invention, said CNT primary sample is SWCN or multi-walled carbon nano-tubes primary sample.
Among the present invention, used carbonate can be: in sodium acid carbonate, sodium carbonate or the ammonium hydrogencarbonate etc. any.
Among the present invention, the dyestuff that said adsorbent is removed comprise methylene blue, methyl orange or rose-red in any or mix.
The method of testing of the absorption property of dyestuff is in the adsorbents adsorb water of gained of the present invention: utilize ultraviolet-uisible spectrophotometer to be directed against the measurement that the dye solution different concentration is carried out absorbance; With data drawing standard curve after measuring, thus the concentration of dyestuff in the mensuration water.
The invention has the advantages that:
(1) directly adopt the synthetic CNT primary sample of preparation as raw material; But make full use of the effect of kish catalyst granules realization Magnetic Isolation in the primary sample; Avoided in traditional magnetic iron oxide/carbon nano tube composite adsorbent preparation; Elder generation's purifying is removed the metallic particles that exists in the CNT primary sample, and then in the complex process of carbon tube-surface carried magnetic oxide.To the magnetic carbon nano-tube primary sample, adopt the good chitosan-modified CNT primary sample of bio-compatibility, through the further crosslinked structural stability that shitosan/magnetic carbon nano-tube is provided.And then obtain can be in acid solution dyestuff to be had the cross-linked chitosan/magnetic carbon nano-tube adsorbent of excellent absorption property.
(2) the inventive method can adopt the preparation of conventional methods such as chemical vapour deposition technique, laser method, arc process the CNT that contains metal catalyst particles as primary sample; It is surface modified to carry out shitosan, all can prepare cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent.
(3) preparation technology of the present invention is simple, condition is prone to control, stable performance; Adopt the chitosan-modified carbon nano tube surface structure of biomaterial, the shitosan raw material is easy to get, and is cheap; Can effectively improve the hydrophobicity of CNT; Improve its dispersive property in the aqueous solution, cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent can adopt magnetic separation technique to separate, reclaim adsorbent fast, avoid causing secondary environmental pollution.
The specific embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
Take by weighing in the dilute acetic acid solution that is dissolved in 100ml after the dried CNT of 1g shitosan and 1g mixes (mass fraction of acetic acid is 2%), stir 20min, it is mixed; In mixed solution, add the 0.6g sodium acid carbonate, it is even to be stirred to bubble; Continue to add 25ml formalin, stir 20min, leave standstill 10min behind the mixing; Post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10; Add the 2ml epoxychloropropane, under 70 ℃ of conditions, reaction 4h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 30min; End when adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.It is in the 500mg/L solution that 30 mg adsorbents are joined 40 mL methyl orange concentration; And Magnetic Isolation goes out adsorbent from solution; The solution that will reach after the adsorption equilibrium carries out the ultraviolet-uisible spectrophotometer test, and the result shows: the adsorption capacity of the cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent methyl orange of the present invention's preparation is 546.8mg/g.
Embodiment 2
Take by weighing in the dilute acetic acid solution that is dissolved in 100ml after the dried CNT of 1g shitosan and 0.25g mixes (mass fraction of acetic acid is 2%), stir 20min, it is mixed; In mixed solution, add the 0.6g sodium acid carbonate, it is even to be stirred to bubble; Continue to add 25ml formalin, stir 20min, leave standstill 10min behind the mixing; Post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10; Add the 2ml epoxychloropropane, under 70 ℃ of conditions, reaction 4h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 30min; End when adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.It is in the 500mg/L solution that 30 mg adsorbents are joined 40 mL methyl orange concentration; And Magnetic Isolation goes out adsorbent from solution; The solution that will reach after the adsorption equilibrium carries out the ultraviolet-uisible spectrophotometer test, and the result shows: the adsorption capacity of the cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent methyl orange of the present invention's preparation is 604mg/g.
Embodiment 3
Take by weighing in the dilute acetic acid solution that is dissolved in 100ml after the dried CNT of 1g shitosan and 0.02g mixes (mass fraction of acetic acid is 2%), stir 20min, it is mixed; In mixed solution, add the 0.6g sodium acid carbonate, it is even to be stirred to bubble; Continue to add 25ml formalin, stir 20min, leave standstill 10min behind the mixing; Post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10; Add the 2ml epoxychloropropane, under 70 ℃ of conditions, reaction 4h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 30min; End when adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.It is in the 500mg/L solution that 30 mg adsorbents are joined 40 mL methyl orange concentration; And Magnetic Isolation goes out adsorbent from solution; The solution that will reach after the adsorption equilibrium carries out the ultraviolet-uisible spectrophotometer test, and the result shows: the adsorption capacity of the cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent methyl orange of the present invention's preparation is 574mg/g.
Embodiment 4
Take by weighing in the dilute acetic acid solution that is dissolved in 100ml after the dried CNT of 0.02g shitosan and 1g mixes (mass fraction of acetic acid is 2%), stir 20min, it is mixed; In mixed solution, add the 0.6g sodium acid carbonate, it is even to be stirred to bubble; Continue to add 25ml formalin, stir 20min, leave standstill 10min behind the mixing; Post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10; Add the 2ml epoxychloropropane, under 70 ℃ of conditions, reaction 4h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 30min; End when adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.It is in the 500mg/L solution that 30 mg adsorbents are joined 40 mL methyl orange concentration; And Magnetic Isolation goes out adsorbent from solution; The solution that will reach after the adsorption equilibrium carries out the ultraviolet-uisible spectrophotometer test, and the result shows: the adsorption capacity of the cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent methyl orange of the present invention's preparation is 176.2mg/g.
Embodiment 5
Take by weighing in the dilute acetic acid solution that is dissolved in 100ml after the dried CNT of 1g shitosan and 1g mixes (mass fraction of acetic acid is 2%), stir 20min, it is mixed; In mixed solution, add the 0.6g sodium acid carbonate, it is even to be stirred to bubble; Continue to add 25ml formalin, stir 20min, leave standstill 10min behind the mixing; Post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10; Add the 2ml epoxychloropropane, under 70 ℃ of conditions, reaction 4h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 30min; End when adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.It is in the 500mg/L solution that 30 mg adsorbents are joined 40 mL methyl orange concentration; And Magnetic Isolation goes out adsorbent from solution; The solution that will reach after the adsorption equilibrium carries out the ultraviolet-uisible spectrophotometer test, and the result shows: the adsorption capacity of the cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent methyl orange of the present invention's preparation is 546.8mg/g.
Embodiment 6
Take by weighing in the dilute acetic acid solution that is dissolved in 100ml after the dried CNT of 0.11g shitosan and 1g mixes (mass fraction of acetic acid is 2%), stir 20min, it is mixed; In mixed solution, add the 0.6g sodium acid carbonate, it is even to be stirred to bubble; Continue to add 25ml formalin, stir 20min, leave standstill 10min behind the mixing; Post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10; Add the 2ml epoxychloropropane, under 70 ℃ of conditions, reaction 4h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 30min; End when adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.It is in the 500mg/L solution that 30 mg adsorbents are joined 40 mL methyl orange concentration; And Magnetic Isolation goes out adsorbent from solution; The solution that will reach after the adsorption equilibrium carries out the ultraviolet-uisible spectrophotometer test, and the result shows: the adsorption capacity of the cross-linked chitosan/magnetic carbon nano-tube composite nano materials adsorbent methyl orange of the present invention's preparation is 56.3mg/g.
Claims (5)
1. magnetic carbon nano-tube/cross-linked chitosan composite nano materials preparation of adsorbent method is characterized in that concrete steps are following:
(1) take by weighing 0.1-1g shitosan and 0.1-1g CNT in beaker, adding mass fraction is in the dilute acetic acid solution of 1%-5%, stirs 5-10min, makes to mix;
(2) add 0.1-0.6g carbonate, it is even to be stirred to bubble; Continue to add 1-25ml formalin, stir 5min, leave standstill 10min behind the mixing;
(3) post reaction mixture is filtered, after washing repeatedly with distilled water, pour into once more in the sodium hydrate aqueous solution, regulate this pH of mixed value greater than 10;
(4) add the 1-10ml epoxychloropropane, under 60-90 ℃ of condition, reaction 2-8h; Post reaction mixture is filtered, after washing repeatedly with distilled water, join in the 1mol/L hydrochloric acid solution and stir 5-30min;
End when (5) adopting sodium hydroxide solution cyclic washing, suction filtration to pH value of solution value to be neutral; Vacuum drying promptly gets required product.
2. preparation method according to claim 1 is characterized in that the used not purifying carbon nano-tube of step (1) primary sample, and its sample is that chemical vapour deposition technique, laser method or arc process prepare unpurified CNT primary sample.
3. preparation method according to claim 1 is characterized in that the used not purifying carbon nano-tube of step (1) primary sample is SWCN or multi-walled carbon nano-tubes.
4. preparation method according to claim 1, it is characterized in that the used carbonate of step (2) be in sodium acid carbonate, sodium carbonate or the ammonium hydrogencarbonate any.
One kind according to claim 1 the dyestuff that magnetic carbon nano-tube/cross-linked chitosan composite nano materials adsorbent is used for removing that obtains of preparation method comprise methylene blue, methyl orange or rose-red any or mix.
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| CN103447008A (en) * | 2013-09-06 | 2013-12-18 | 山东理工大学 | Three-component cationic dye adsorbent and preparation method thereof |
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| CN104289199A (en) * | 2014-10-25 | 2015-01-21 | 济南大学 | Preparation method of magnetic HPCS/GO adsorbing agent for removing heavy metals and application |
| CN104289200A (en) * | 2014-10-25 | 2015-01-21 | 济南大学 | Preparation method and application of magnetic HACC/oxidized multi-walled carbon nanotube adsorbent |
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| CN105983394A (en) * | 2015-03-05 | 2016-10-05 | 江南石墨烯研究院 | Method for preparing efficient and magnetically separable dye adsorbent |
| CN108745306A (en) * | 2018-06-27 | 2018-11-06 | 东华理工大学 | A kind of preparation method of epoxychloropropane cross-linked chitosan/aminated carbon nano tube composite aerogel |
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| CN103447008A (en) * | 2013-09-06 | 2013-12-18 | 山东理工大学 | Three-component cationic dye adsorbent and preparation method thereof |
| CN103933949B (en) * | 2014-04-18 | 2016-03-09 | 梁吉 | A kind of Carbon Nanotubes/Chitosan mesoporous sphere composite and preparation method thereof |
| CN103933949A (en) * | 2014-04-18 | 2014-07-23 | 梁吉 | Carbon nano tube/chitosan mesoporous spherical composite material as well as preparation method thereof |
| CN104289199A (en) * | 2014-10-25 | 2015-01-21 | 济南大学 | Preparation method of magnetic HPCS/GO adsorbing agent for removing heavy metals and application |
| CN104289200A (en) * | 2014-10-25 | 2015-01-21 | 济南大学 | Preparation method and application of magnetic HACC/oxidized multi-walled carbon nanotube adsorbent |
| CN104289200B (en) * | 2014-10-25 | 2016-12-14 | 济南大学 | A kind of preparation method and application of magnetic HACC/ oxidation multi-walled carbon nano-tubes adsorbent |
| CN105983394A (en) * | 2015-03-05 | 2016-10-05 | 江南石墨烯研究院 | Method for preparing efficient and magnetically separable dye adsorbent |
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| CN108745306A (en) * | 2018-06-27 | 2018-11-06 | 东华理工大学 | A kind of preparation method of epoxychloropropane cross-linked chitosan/aminated carbon nano tube composite aerogel |
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Application publication date: 20120704 |