CN103212382A - Self-assembly electrostatic spinning nanofiber membrane for absorbing heavy metal ions and preparation method of self-assembly electrostatic spinning nanofiber membrane - Google Patents
Self-assembly electrostatic spinning nanofiber membrane for absorbing heavy metal ions and preparation method of self-assembly electrostatic spinning nanofiber membrane Download PDFInfo
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- CN103212382A CN103212382A CN 201310110692 CN201310110692A CN103212382A CN 103212382 A CN103212382 A CN 103212382A CN 201310110692 CN201310110692 CN 201310110692 CN 201310110692 A CN201310110692 A CN 201310110692A CN 103212382 A CN103212382 A CN 103212382A
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Abstract
The invention relates to a self-assembly electrostatic spinning nanofiber membrane for absorbing heavy metal ions and a preparation method of the self-assembly electrostatic spinning nanofiber membrane. The preparation method disclosed by the invention comprises the following steps of: firstly, preparing an electrostatic spinning nanofiber membrane with an average diameter of 88nm-135nm and a porosity of 30%-80% in an electrostatic spinning method, and dipping the electrostatic spinning nanofiber membrane in 100% ethanol for 1-2 hours; secondly, dipping the electrostatic spinning nanofiber membrane processed by the ethanol in an alkali solution for 30-90 minutes; and finally, processing and preparing the electrostatic spinning nanofiber membrane assembled by 2-6 layers of polyethyleneimine by a polyethyleneimine solution. The self-assembly electrostatic spinning nanofiber membrane prepared by the preparation method disclosed by the invention has the characteristics of large specific surface area, high porosity and more inner pore spaces and has the advantages of increasing contact area with the metal ions, improving the absorption capability, shortening the time for reaching absorption balance, effectively absorbing the heavy metal ions in wastewater, being biologically degraded and not causing environment pollution.
Description
Technical field
The invention belongs to the sorbing material field, the plain nano fibrous membrane of particularly a kind of self assembly electrostatic spinning of efficiently Adsorption of Heavy Metal Ions.
Background technology
Heavy metal pollution is meant the environmental pollution that is caused by heavy metal or its compound.Heavy metal pollution can cause by natural cause (as soil, rock decay and volcano eruption etc.), but mainly is due to mining, industrial manufacturing, sewage irrigation and the human factors such as use heavy metal goods or containing metal pollutant.Heavy metal can not but can be become thousands of times ground enrichment by biodegradation under the biological magnification of food chain, enter human body at last.Although some heavy metal such as manganese, copper, zinc etc. are the essential trace elements of vital movement, most of heavy metal is not that life is necessary.Surpass finite concentration, just will cause damage to health, cause various diseases, as: dehydration, stomachache, nauseating, dizzy, muscle dysfunction, children's nervous system destruction, lung pain, inflammatory eye, fash, vomiting, stomachache, pain, expiratory dyspnea, hepatic injury etc.Along with the fast development of China's economic society, the quickening of population growth, industrialization and urbanization advances, and the industry that relates to heavy metal is just keeping stronger growth, and the heavy metal pollution incident takes place frequently, and has brought severe impairment for the environment and the people's health.
The method of removing the middle heavy metal ion of anhydrating is a lot, traditional have chemical precipitation method, oxidation-reduction method, ferrite process, electrolysis, evaporation concentration method, ion-exchange-resin process etc., but these methods exist mostly that investment is big, operating cost is high, operational administrative trouble and can produce secondary pollution and can not solve metal well and water resource such as utilizes again at problem.
Using at present more in practice is absorption method, or by electrostatic interaction (interacting between positively charged metal ion and the electronegative matrix), or by chelation (providing lone pair electrons and metal ion to form co-ordinate covalent bond by matrix).Adsorbent commonly used comprises active carbon, bentonite, zeolite and biological adsorption agent, and wherein biological absorption has advantages such as the adsorbent source is abundant, wide in variety, cost is low, adsorption capacity is big, speed is fast, can remedy the defective of conventional process method and has been subjected to extensive concern.Fibroin albumen is the main body of silk, account for the 70%-80% of silk quality, it is a kind of big molecule of natural biological that does not have physiologically active, be formed by connecting by 18 seed amino acids such as aminoacetic acid, alanine, serine, tyrosine, the amino acid composition Semi-polarity amino acid of fibroin albumen mainly contains glycine, tyrosine, asparatate, glutamic acid, threonine, serine, account for 54.85%, these polar amino acids will play a major role in heavy metal ion adsorbed.
The fibre diameter of the aperture of sorbing material and formation sorbing material is the principal element that influences sorbing material absorption precision and efficient, and fibre diameter is thin more, and the absorption precision and the efficient of corresponding sorbing material are high more.Utilizing electrospinning process can access diameter is tens fibers to the hundreds of nanometer, the non woven fibre film that forms is in light weight, good penetrability, the aperture is little, specific area is big, porosity is high, internal void connective good, combine with nano level chemical substance or functional materials easily, this makes it have more high adsorption rate and adsorbance, is a kind of absorption and filtering substrate of excellent performance.
Summary of the invention
The invention provides plain nano fibrous membrane of self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions and preparation method thereof, this nano fibrous membrane sorbing material is the heavy metal ion in the adsorbent solution efficiently.
Plain nano fibrous membrane of the self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions of the present invention and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 10%-16%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 25-35KV, and spinning is apart from 5-15cm, spinning solution feed quantity 0.5-2ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 1-2h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 30-90min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning;
(8) step 7 is repeated 0-4 time, can obtain the plain nano fibrous membrane of 2-6 layers of polyethylene imines assembling electrostatic spinning.
The plain nano fibrous membrane average diameter of the electrostatic spinning that described step (3) obtains 88-135nm, porosity 30-80%.
Aqueous slkali in the described step (5) is a kind of in NaOH, sodium acid carbonate, sodium carbonate, potassium hydroxide, the ammoniacal liquor.
The present invention has following beneficial effect: the plain nano fibrous membrane of self assembly electrostatic spinning of the present invention, have characteristics such as specific area is big, porosity is high, internal void is many, can increase contact area with metal ion, increase adsorbance, shorten and reach time for adsorption balance, adsorb the heavy metal ion in the waste water effectively, and biodegradable, can not cause environmental pollution.
Description of drawings
Fig. 1 is the plain nano fibrous membrane SEM of 4 layers of polyethylene imines assembling electrostatic spinning Electronic Speculum figure.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.
Embodiment 1:
Plain nano fibrous membrane of the self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions of the present invention and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen that 5g is pure is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 10%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 25kV, and spinning is apart from 5cm, spinning solution feed quantity 0.5ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 1h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 30min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning.
The plain nano fibrous membrane average diameter of the electrostatic spinning that described step (3) obtains 107nm, porosity 62%.
Aqueous slkali in the described step (5) is a NaOH.
Embodiment 2:
Plain nano fibrous membrane of the self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions of the present invention and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen that 5g is pure is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 12%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 30kV, and spinning is apart from 8cm, spinning solution feed quantity 1ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 1h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 45min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning;
(8) step 7 is repeated 1 time, can obtain the plain nano fibrous membrane of 3 layers of polyethylene imines assembling electrostatic spinning.
The plain nano fibrous membrane average diameter of the electrostatic spinning that described step (3) obtains 115nm, porosity 56%.
Aqueous slkali in the described step (5) is a sodium acid carbonate.
Embodiment 3:
Plain nano fibrous membrane of the self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions of the present invention and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen that 5g is pure is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 14%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 30kV, and spinning is apart from 12cm, spinning solution feed quantity 1.2ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 1.5h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 60min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning;
(8) step 7 is repeated 2 times, can obtain the plain nano fibrous membrane of 4 layers of polyethylene imines assembling electrostatic spinning.
The plain nano fibrous membrane average diameter of the electrostatic spinning that described step (3) obtains 93nm, porosity 74%.
Aqueous slkali in the described step (5) is a sodium carbonate.
Embodiment 4:
Plain nano fibrous membrane of the self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions of the present invention and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen that 5g is pure is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 16%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 35kV, and spinning is apart from 15cm, spinning solution feed quantity 2ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 2h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 75min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning;
(8) step 7 is repeated 3 times, can obtain the plain nano fibrous membrane of 5 layers of polyethylene imines assembling electrostatic spinning.
The plain nano fibrous membrane average diameter of the electrostatic spinning that described step (3) obtains 127nm, porosity 46%.
Aqueous slkali in the described step (5) is a potassium hydroxide.
Embodiment 5:
Plain nano fibrous membrane of the self assembly electrostatic spinning of a kind of Adsorption of Heavy Metal Ions of the present invention and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen that 5g is pure is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 14%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 30kV, and spinning is apart from 10cm, spinning solution feed quantity 1.5ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 1.5h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 60min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning;
(8) step 7 is repeated 4 times, can obtain the plain nano fibrous membrane of 6 layers of polyethylene imines assembling electrostatic spinning.
Aqueous slkali in the described step (5) is an ammoniacal liquor.
Table 1 is that the plain nano fibrous membrane of the self assembly electrostatic spinning among each embodiment is to Cu
2+, Cr
3+, Pb
2+, Cd
2+Adsorbance, unit: mg/g.
Cu
2+ Cr
3+ Pb
2+ Cd
2+
Embodiment 1 14.3 6.7 11.2 8.5
Embodiment 2 29.8 11.2 25.9 17.3
Embodiment 3 47.4 19.3 38.6 31.8
Embodiment 4 63.9 23.8 42.5 53.6
Embodiment 5 65.1 26.4 47.7 59.8
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention amplifies out or change still are in protection scope of the present invention.
Claims (3)
1. plain nano fibrous membrane of the self assembly electrostatic spinning of an Adsorption of Heavy Metal Ions and preparation method thereof is characterized in that this preparation method comprises following operating procedure:
(1) silk that will not come unstuck through come unstuck, dissolving, infiltration, purifying, drying, obtain pure fibroin albumen;
(2) fibroin albumen is dissolved in 98% formic acid solution, the spinning solution of configuration quality mark 10%-16%;
(3) above-mentioned spinning solution is joined in the electrospinning device, prepare the fibroin nano fibrous membrane with method of electrostatic spinning, the technology of electrostatic spinning is: voltage 25-35kV, and spinning is apart from 5-15cm, spinning solution feed quantity 0.5-2ml/h;
(4) the plain nano fibrous membrane of the electrostatic spinning that makes is dipped in 1-2h in 100% ethanol;
(5) the plain nano fibrous membrane of the electrostatic spinning after the Ethanol Treatment is dipped in 30-90min in the aqueous slkali, deionized water rinsing is clean;
(6) with the polyethyleneimine: amine aqueous solution 10-30min of the plain nano fibrous membrane immersion of the electrostatic spinning after aqueous slkali processing 1-5g/L, take out, deionized water rinsing is clean, and natural air drying under the room temperature obtains 1 layers of polyethylene imines assembling electrostatic spinning element nano fibrous membrane;
(7) surface-assembled there is the plain nano fibrous membrane of electrostatic spinning of 1 layers of polyethylene imines immerse 10-30min in the 1-5g/L silk fibroin solution, it is clean to take out the back deionized water rinsing, immerse 10-30min in the polyethyleneimine: amine aqueous solution of 1-5g/L again, it is clean to take out the back deionized water rinsing, natural air drying under the room temperature obtains the plain nano fibrous membrane of 2 layers of polyethylene imines assembling electrostatic spinning;
(8) step 7 is repeated 0-4 time, can obtain the plain nano fibrous membrane of 2-6 layers of polyethylene imines assembling electrostatic spinning.
2. plain nano fibrous membrane of the self assembly electrostatic spinning of Adsorption of Heavy Metal Ions according to claim 1 and preparation method thereof is characterized in that, the plain nano fibrous membrane average diameter of the electrostatic spinning that step (3) obtains 88-135nm, porosity 30-80%.
3. plain nano fibrous membrane of the self assembly electrostatic spinning of Adsorption of Heavy Metal Ions according to claim 1 and preparation method thereof, it is characterized in that the aqueous slkali in the step (5) is a kind of in NaOH, sodium acid carbonate, sodium carbonate, potassium hydroxide, the ammoniacal liquor.
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| CN103468002A (en) * | 2013-09-03 | 2013-12-25 | 太原理工大学 | Preparation method of silk fibroin/metal nanoparticle composite system |
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| CN103468002A (en) * | 2013-09-03 | 2013-12-25 | 太原理工大学 | Preparation method of silk fibroin/metal nanoparticle composite system |
| CN103638910B (en) * | 2013-11-07 | 2015-12-30 | 青岛文创科技有限公司 | The preparation method of a kind of crosslinked starch, fullerene composite membrane |
| CN103638908A (en) * | 2013-11-07 | 2014-03-19 | 青岛文创科技有限公司 | Preparation method for crosslinked-fish-scale-gelatin/fullerene composite membrane |
| CN103638910A (en) * | 2013-11-07 | 2014-03-19 | 青岛文创科技有限公司 | Preparation method for crosslinked-starch/fullerene composite membrane |
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| CN104163463B (en) * | 2014-08-04 | 2016-04-13 | 浙江大学 | Utilize the method for silk fibroin adsorbent solution heavy metal ion |
| CN104163463A (en) * | 2014-08-04 | 2014-11-26 | 浙江大学 | Method for adsorbing heavy metal ions in solution by virtue of silk fibroin |
| CN105615047A (en) * | 2014-12-01 | 2016-06-01 | 上海正克电器有限公司 | Air purification mask |
| CN104984744B (en) * | 2015-06-02 | 2017-05-17 | 中山大学 | Plant fiber based solid amine adsorption material, preparation method and application thereof |
| CN106823562A (en) * | 2016-12-27 | 2017-06-13 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of artificial pulmonary surfactant is used for the method for removing PM2.5 |
| CN108905970A (en) * | 2018-07-23 | 2018-11-30 | 山东建筑大学 | The preparation method and application of cadmium adsorbent is removed based on the modified water body of clinoptilolite |
| CN108905970B (en) * | 2018-07-23 | 2021-02-26 | 山东建筑大学 | Preparation method and application of clinoptilolite modification-based water body cadmium removal adsorbent |
| CN111135802A (en) * | 2020-01-19 | 2020-05-12 | 浙江大学 | Preparation method for constructing water treatment biomembrane by modifying manganese dioxide particles with silk fibroin planar wires |
| CN114575152A (en) * | 2022-01-30 | 2022-06-03 | 华北理工大学 | Preparation process of amino acid modified ethylene-vinyl alcohol copolymer nanofiber membrane |
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Application publication date: 20130724 |