CN102553532A - Method for preparing magnetic carbon nano-tube adsorbent having high adsorption capacity and used for removing dye from aqueous phase - Google Patents
Method for preparing magnetic carbon nano-tube adsorbent having high adsorption capacity and used for removing dye from aqueous phase Download PDFInfo
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Abstract
The invention relates to a method for preparing a magnetic carbon nano-tube adsorbent having high adsorption capacity and used for removing a dye from an aqueous phase. The method comprises the following steps of: mixing an original sample of unpurified carbon nano-tubes and potassium hydroxide powder, and grinding uniformly; putting into a reaction container, introducing insert gas, reacting, raising to certain temperature, and regulating carrier gas; and continuously reacting for several hours, filtering a reaction product, washing, and performing vacuum drying to obtain the magnetic carbon nano-tube composite adsorbent. A solid-phase oxidant is used for modifying a surface structure of the carbon nano-tubes, so that the specific surface area and hydrophilic nature of the carbon nano-tubes are remarkably improved, and the hydrophobic property of the carbon nano-tubes and the dispersion performance of the carbon nano-tubes in an aqueous solution are improved; and the adsorbent can be conveniently and quickly separated and recovered by a magnetic separation technology, so that secondary environmental pollution is avoided. In addition, raw materials are readily available, the preparation process is simple and low in cost, and is suitable for continuous large-scale batch production, and conditions are easy to control.
Description
Technical field
The invention belongs to the new technical field of function materials of environment nanometer; Be specifically related to a kind of high-adsorption-capacity and remove the magnetic carbon nano-tube preparation of adsorbent method of aqueous phase dyestuff; 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.In recent years, begin to have the adsorption effect of scholar's research CNT to dyestuff, the research of CNTs aspect the absorption of waste water from dyestuff is at the early-stage, is a focus of absorption research field.The improvement of production technology at present makes the price of CNTs reduce significantly, and environmental applications becomes possibility gradually.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.At present, separation of C NTs mainly takes centrifugal and filtration method from liquid phase, and centrifugal process needs high rotational speed, is not easy to industrial applications, and filtration method stops up and the accumulation of generation bulk filtrate filter opening, and these two kinds of methods all are difficult for making fully Separation of Solid and Liquid.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 there are shortcomings such as complex process in traditional magnetic oxide/carbon nano-tube hybridization material adsorbent preparation; The existence of the problems referred to above influences and has limited the further development and application of magnetic carbon nano-tube adsorbent, therefore develops the high power capacity novel magnetic carbon nanotube adsorption agent that can under sour environment, use reduction adsorbent cost, raising adsorption capacity, life-saving, the popularization of promotion practicability are had very important significance.
Summary of the invention
The object of the present invention is to provide a kind of high-adsorption-capacity to remove the magnetic carbon nano-tube adsorbent of aqueous phase dyestuff.
The present invention adopts the CNT primary sample as adsorbent; Utilize carbon control to be equipped with the metal catalyst particles that produces in the process; Realize the Magnetic Isolation effect; Method through adopting phase oxidative agent modification is carried out the absorption property that modification further improves magnetic carbon nano-tube for the magnetic carbon nano-tube surface; 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.This method cost is low, and technology is simple.Result of the test shows: adopt present new technology effectively to improve the hydrophobicity of magnetic carbon nano-tube in the aqueous solution, the material after the modification has quick absorption and enrichment performance to the dyestuff in the aqueous solution.
But the high power capacity magnetic carbon nano-tube preparation of adsorbent method of the removal dyestuff Magnetic Isolation that the present invention proposes, concrete steps are following: the purifying carbon nano-tube primary sample does not mix with the potassium hydroxide powder, grinds evenly; Place reaction vessel to feed inert gas and react, be warming up to 500～900 ℃, regulate carrier gas; Reaction continued to carry out 0.5-3 hour, after product taking-up cooling, added the deionized water cyclic washing, ended when suction filtration to pH value of solution value is neutral; Vacuum drying promptly gets required product.Wherein: the mass ratio of used CNT primary sample and potassium hydroxide is 1:1～1:6.
Among the present invention, used CNT is the CNT primary sample, and its sample can be the CNT primary sample of chemical vapour deposition technique, laser method, arc process preparation.
Among the present invention, among the present invention, said CNT is SWCN or multi-walled carbon nano-tubes.
Among the present invention, said intensification is that the speed with 15 ℃/min is warming up to 500～900 ℃.
Among the present invention, said inert gas is nitrogen or argon gas.
Among the present invention, said adjusting carrier gas is specially and regulates said inert gas flow is 6～60L/h.
Among the present invention, said reaction vessel is a quartz tube furnace.
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 surface texture and the character of carbon pipe in the carbon nano-tube modified primary sample of phase oxidative agent; Make full use of the modifiable physics of carbon nano tube surface, chemical characteristic, make it have good adsorption and enriched character dyestuff in the aqueous solution.
(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, carry out surface modifiedly, all can prepare the magnetic carbon nano-tube compound adsorbent.
(3) preparation technology of the present invention is simple, condition is prone to control, stable performance; Adopt the carbon nano-tube modified surface texture of oxidizing solution; Improve the hydrophobicity of CNT; Improve its dispersive property in the aqueous solution, adsorbent can adopt magnetic separation technique to separate, reclaim adsorbent quickly and easily, avoids 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 the dry unpurified CNT primary sample powder 1.0g in back, to press mass ratio 1:6 mixed grinding even with potassium hydroxide; In quartz tube furnace, being warmed up to reaction temperature with the speed of 15 ℃/min is 750 ℃, feeds nitrogen flow to do
8L/h, 1 hour reaction time cooling is taken out, again with deionized water wash repeatedly, the suction filtration CNT reaches till 7 until the pH value of solution value; The activated carbon nano-tube that obtains is scattered in the alcohol, and it is dry to put into 120 ℃ of vacuum drying chambers, obtains water-soluble good activated carbon nano-tube sorbing material.With magnetic carbon nano-tube sample filtering, washing, the vacuum drying after the modification, obtain magnetic carbon nano-tube high power capacity adsorbent.It is in the 50mg/L solution that this material of 30 mg is 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 magnetic carbon nano-tube adsorbent of the present invention's preparation is 49.5mg/g to the adsorption capacity of methyl orange.
Embodiment 2
Take by weighing the dry unpurified CNT primary sample powder 1.0g in back, to press mass ratio 1:4 mixed grinding even with potassium hydroxide; In quartz tube furnace, being warmed up to reaction temperature with the speed of 15 ℃/min is 750 ℃, feeds nitrogen flow to do
8L/h, 1 hour reaction time cooling is taken out, again with deionized water wash repeatedly, the suction filtration CNT reaches till 7 until the pH value of solution value; The activated carbon nano-tube that obtains is scattered in the alcohol, and it is dry to put into 120 ℃ of vacuum drying chambers, obtains water-soluble good activated carbon nano-tube sorbing material.With magnetic carbon nano-tube sample filtering, washing, the vacuum drying after the modification, obtain magnetic carbon nano-tube high power capacity adsorbent.It is in the 50mg/L solution that this material of 30 mg is 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 magnetic carbon nano-tube adsorbent of the present invention's preparation is 68.6mg/g to the adsorption capacity of methyl orange.
Embodiment 3
Take by weighing the dry unpurified CNT primary sample powder 1.0g in back, to press mass ratio 1:2 mixed grinding even with potassium hydroxide; In quartz tube furnace, being warmed up to reaction temperature with the speed of 15 ℃/min is 750 ℃, feeds nitrogen flow to do
8L/h, 1 hour reaction time cooling is taken out, again with deionized water wash repeatedly, the suction filtration CNT reaches till 7 until the pH value of solution value; The activated carbon nano-tube that obtains is scattered in the alcohol, and it is dry to put into 120 ℃ of vacuum drying chambers, obtains water-soluble good activated carbon nano-tube sorbing material.With magnetic carbon nano-tube sample filtering, washing, the vacuum drying after the modification, obtain magnetic carbon nano-tube high power capacity adsorbent.It is in the 50mg/L solution that this material of 30 mg is 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 magnetic carbon nano-tube adsorbent of the present invention's preparation is 53.4mg/g to the adsorption capacity of methyl orange.
Embodiment 4
Take by weighing the dry unpurified CNT primary sample powder 1.0g in back, to press mass ratio 1:1 mixed grinding even with potassium hydroxide; In quartz tube furnace, being warmed up to reaction temperature with the speed of 15 ℃/min is 750 ℃, feeds nitrogen flow to do
8L/h, 1 hour reaction time cooling is taken out, again with deionized water wash repeatedly, the suction filtration CNT reaches till 7 until the pH value of solution value; The activated carbon nano-tube that obtains is scattered in the alcohol, and it is dry to put into 120 ℃ of vacuum drying chambers, obtains water-soluble good activated carbon nano-tube sorbing material.With magnetic carbon nano-tube sample filtering, washing, the vacuum drying after the modification, obtain magnetic carbon nano-tube high power capacity adsorbent.It is in the 50mg/L solution that this material of 30 mg is 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 magnetic carbon nano-tube adsorbent of the present invention's preparation is 57.8mg/g to the adsorption capacity of methyl orange.
Embodiment 5
Take by weighing the dry unpurified CNT primary sample powder 1.0g in back, to press mass ratio 1:4 mixed grinding even with potassium hydroxide; In quartz tube furnace, being warmed up to reaction temperature with the speed of 15 ℃/min is 750 ℃, feeds nitrogen flow to do
8L/h, 1 hour reaction time cooling is taken out, again with deionized water wash repeatedly, the suction filtration CNT reaches till 7 until the pH value of solution value; The activated carbon nano-tube that obtains is scattered in the alcohol, and it is dry to put into 120 ℃ of vacuum drying chambers, obtains water-soluble good activated carbon nano-tube sorbing material.With magnetic carbon nano-tube sample filtering, washing, the vacuum drying after the modification, obtain magnetic carbon nano-tube high power capacity adsorbent.It is in the 125mg/L solution that this material of 30 mg is joined 40 mL methylene blue 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 magnetic carbon nano-tube adsorbent of the present invention's preparation is 158.6mg/g to the adsorption capacity of methylene blue.
Embodiment 6
Take by weighing the dry unpurified CNT primary sample powder 1.0g in back, to press mass ratio 1:4 mixed grinding even with potassium hydroxide; In quartz tube furnace, being warmed up to reaction temperature with the speed of 15 ℃/min is 750 ℃, feeds nitrogen flow to do
8L/h, 1 hour reaction time cooling is taken out, again with deionized water wash repeatedly, the suction filtration CNT reaches till 7 until the pH value of solution value; The activated carbon nano-tube that obtains is scattered in the alcohol, and it is dry to put into 120 ℃ of vacuum drying chambers, obtains water-soluble good activated carbon nano-tube sorbing material.With magnetic carbon nano-tube sample filtering, washing, the vacuum drying after the modification, obtain magnetic carbon nano-tube high power capacity adsorbent.It is in the 30mg/L solution that this material of 30 mg is joined the rose-red concentration of 40 mL; 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 magnetic carbon nano-tube adsorbent of the present invention's preparation is 56.7mg/g to rosy adsorption capacity.
Claims (8)
1. a high-adsorption-capacity is removed the magnetic carbon nano-tube preparation of adsorbent method of aqueous phase dyestuff, it is characterized in that concrete steps are: the purifying carbon nano-tube primary sample does not mix with the potassium hydroxide powder, and grinding is even; Place reaction vessel to feed inert gas and react, be warming up to 500～900 ℃, regulate carrier gas; Reaction continued to carry out 0.5-3 hour, after product taking-up cooling, added the deionized water cyclic washing, ended when suction filtration to pH value of solution value is neutral; Vacuum drying promptly gets required product; Wherein: the mass ratio of said not purifying carbon nano-tube primary sample and potassium hydroxide is 1:1～1:6.
2. preparation method according to claim 1 is characterized in that used not purifying carbon nano-tube 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 said CNT is SWCN or multi-walled carbon nano-tubes.
4. preparation method according to claim 1 is characterized in that said intensification is that speed with 15 ℃/min is warming up to 500～900 ℃.
5. preparation method according to claim 1 is characterized in that said inert gas is nitrogen or argon gas.
6. preparation method according to claim 1 is characterized in that said adjusting carrier gas is 6～60L/h for regulating inert gas flow.
7. preparation method according to claim 1 is characterized in that said reaction vessel is a quartz tube furnace.
One kind according to claim 1 the high-adsorption-capacity that obtains of preparation method remove dyestuff that the magnetic carbon nano-tube adsorbent of aqueous phase dyestuff is used for removing comprise methylene blue, methyl orange or rose-red any or mix.
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Cited By (8)
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|---|---|---|---|---|
| CN103303997A (en) * | 2013-06-14 | 2013-09-18 | 湖北大学 | Use of magnetic solid-phase extraction agent in treatment of dye wastewater |
| CN104148032A (en) * | 2014-08-01 | 2014-11-19 | 渤海大学 | Synthesis method for biomass-based carbon nano tube waterborne polyurethane foam adsorbent |
| CN104874355A (en) * | 2015-06-12 | 2015-09-02 | 安徽师范大学 | Simple synthetic method for renewable magnetic carbon micro-sphere with effective adsorption property and application thereof |
| CN109248655A (en) * | 2018-10-17 | 2019-01-22 | 天津大学 | A kind of method of preparation and use and application of magnetic carbon nano-tube |
| CN111468070A (en) * | 2020-03-24 | 2020-07-31 | 杭州市富阳区浙工大银湖创新创业研究院 | Simple, convenient and efficient preparation method of magnetically separable biomass dye adsorbent |
| CN112316927A (en) * | 2020-11-11 | 2021-02-05 | 扬州工业职业技术学院 | Water treatment agent capable of rapidly adsorbing methylene blue and preparation method thereof |
| CN114534698A (en) * | 2022-02-17 | 2022-05-27 | 世纪华扬环境工程有限公司 | Preparation method of multifunctional adsorptive gel balls |
| CN115400738A (en) * | 2021-05-27 | 2022-11-29 | 北京化工大学 | Tannin-carbon nanotube adsorbent and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303997A (en) * | 2013-06-14 | 2013-09-18 | 湖北大学 | Use of magnetic solid-phase extraction agent in treatment of dye wastewater |
| CN103303997B (en) * | 2013-06-14 | 2015-04-22 | 湖北大学 | Use of magnetic solid-phase extraction agent in treatment of dye wastewater |
| CN104148032A (en) * | 2014-08-01 | 2014-11-19 | 渤海大学 | Synthesis method for biomass-based carbon nano tube waterborne polyurethane foam adsorbent |
| CN104874355A (en) * | 2015-06-12 | 2015-09-02 | 安徽师范大学 | Simple synthetic method for renewable magnetic carbon micro-sphere with effective adsorption property and application thereof |
| CN109248655A (en) * | 2018-10-17 | 2019-01-22 | 天津大学 | A kind of method of preparation and use and application of magnetic carbon nano-tube |
| CN111468070A (en) * | 2020-03-24 | 2020-07-31 | 杭州市富阳区浙工大银湖创新创业研究院 | Simple, convenient and efficient preparation method of magnetically separable biomass dye adsorbent |
| CN111468070B (en) * | 2020-03-24 | 2022-06-24 | 杭州市富阳区浙工大银湖创新创业研究院 | Simple, convenient and efficient preparation method of magnetically separable biomass dye adsorbent |
| CN112316927A (en) * | 2020-11-11 | 2021-02-05 | 扬州工业职业技术学院 | Water treatment agent capable of rapidly adsorbing methylene blue and preparation method thereof |
| CN112316927B (en) * | 2020-11-11 | 2023-04-25 | 扬州工业职业技术学院 | Water treatment agent capable of rapidly adsorbing methylene blue and preparation method thereof |
| CN115400738A (en) * | 2021-05-27 | 2022-11-29 | 北京化工大学 | Tannin-carbon nanotube adsorbent and preparation method and application thereof |
| CN115400738B (en) * | 2021-05-27 | 2023-08-08 | 北京化工大学 | Tannic acid-carbon nano tube adsorbent and preparation method and application thereof |
| CN114534698A (en) * | 2022-02-17 | 2022-05-27 | 世纪华扬环境工程有限公司 | Preparation method of multifunctional adsorptive gel balls |
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Application publication date: 20120711 |