CN105289539A - Graphene/ polyvinyl alcohol nanofibers membrane adsorbent, preparation method and appliance - Google Patents
Graphene/ polyvinyl alcohol nanofibers membrane adsorbent, preparation method and appliance Download PDFInfo
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Abstract
本发明公开了一种石墨烯/聚乙烯醇纳米纤维膜吸附剂及其制备方法和应用，包括以下步骤：(1)将氧化石墨烯加入去离子水中，超声0.5～4h后，得到分散均匀的氧化石墨烯溶液；(2)将聚乙烯醇加入到去离子水中，将溶液加热到40～100℃溶解，冷却至室温，得到聚乙烯醇溶液；(3)将氧化石墨烯溶液和聚乙烯醇溶液混合并搅拌，得到纺丝溶液；(4)将上述纺丝溶液进行静电纺丝，得到氧化石墨烯与聚乙烯醇纳米纤维膜；(5)将纳米纤维膜冷冻干燥，即制得石墨烯/聚乙烯醇纳米纤维膜吸附剂。制得的纤维膜具有比表面积大、孔隙率高，可以增大与重金属离子的接触面积，增加吸附容量，缩短吸附平衡时间，能有效吸附废水中的重金属离子。
The invention discloses a graphene/polyvinyl alcohol nanofiber membrane adsorbent and its preparation method and application, comprising the following steps: (1) adding graphene oxide into deionized water, and ultrasonicating for 0.5 to 4 hours to obtain evenly dispersed Graphene oxide solution; (2) adding polyvinyl alcohol to deionized water, heating the solution to 40-100°C to dissolve, cooling to room temperature to obtain a polyvinyl alcohol solution; (3) mixing graphene oxide solution and polyvinyl alcohol The solutions are mixed and stirred to obtain a spinning solution; (4) electrospinning the above spinning solution to obtain graphene oxide and polyvinyl alcohol nanofiber membranes; (5) freeze-drying the nanofiber membranes to obtain graphene / Polyvinyl alcohol nanofiber membrane adsorbent. The prepared fiber membrane has large specific surface area and high porosity, can increase the contact area with heavy metal ions, increase adsorption capacity, shorten adsorption equilibrium time, and can effectively adsorb heavy metal ions in wastewater.
Description
Technical field
The invention belongs to sorbing material field, particularly a kind of can the Electrospun nano-fibers membrane adsorbent of efficient adsorption heavy metal ion.
Background technology
Along with the fast development of the society of China's economy, the quickening that population growth, industrialization and cities and towns are talked about advances, and the industry relating to heavy metal is just remain stronger growth, and heavy metal pollution event takes place frequently.Because heavy metal has larger toxicity, can not be biodegradable, but can be enriched in animal and plant body by food chain, finally be trapped in environment and human body, bring serious harm to the health of ecological environment and the mankind.
The method of heavy-metal ion removal is a lot, traditional method has chemical precipitation method, membrane separation process, ion-exchange-resin process, electrochemical process, oxidation-reduction method etc., but these methods also exist that investment is large, operating cost is high, complicated operation and easily produce secondary pollution and not can solve the problem such as heavy metal removal and water resource recycling.
Absorption method due to simple to operate, cost is lower, efficient, can heavy metal be reclaimed, be a kind of process for treating heavy-metal waste water the most frequently used at present.Conventional adsorbent comprises active carbon, zeolite, kaolin and bentonite, however these materials adsorption capacity and efficiency lower, be difficult to large-scale application.Graphene oxide has huge specific area, abundant oxygen-containing functional group (hydroxyl, carbonyl, carboxyl and epoxy radicals etc.) and a large amount of delocalizedπelectron, and be considered to a kind of superabsorbent, heavy metal has good absorption property.But, because graphene oxide is nano-grade matter, easily disperse in aqueous, be difficult to the graphene oxide after to absorption and carry out separation recycling.Mainly prepare the graphene-based composite with separating power by the method for chemical modification graphene oxide at present, and chemical modification often relates to the use of organic solvent and chemical agent, this just increases preparation cost, may face the risk revealing poisonous and harmful substance simultaneously.
Electrospinning process is a kind of simple, can be used in the technology preparing continuous multifunctional nano fiber.Utilizing electrostatic spinning technique can obtain diameter is tens to the fibers of hundreds of nanometer, the non woven fibre of formation have lightweight, specific area large, porosity high.Polyvinyl alcohol is a kind of important water-soluble (under high temperature) nontoxic polymer, has been widely used in the Electrospun nano-fibers preparing different purposes.Adopt electrostatic spinning technique that graphene oxide and polyvinyl alcohol mixing solution are carried out spinning and can prepare graphene oxide/polyvinyl alcohol nanofiber adsorbent, because graphene oxide and polyvinyl alcohol can produce hydrogen bond, prevent coming off of graphene oxide, making graphene oxide/polyvinyl alcohol nano fibrous membrane have higher adsorption efficiency and adsorption capacity, is a kind of adsorption substrates of excellent performance.
Summary of the invention
Electrospun nano-fibers film that the invention provides a kind of Adsorption of Heavy Metal Ions and preparation method thereof, this nano fibrous membrane can heavy metal ion in efficient adsorption solution.
A preparation method for Graphene/polyvinyl alcohol nanofiber membrane adsorbent, comprises the following steps:
(1) graphene oxide is added in deionized water, after ultrasonic 0.5 ~ 4h, obtain finely dispersed graphene oxide solution;
(2) polyvinyl alcohol is joined in deionized water, solution is heated to 40 ~ 100 DEG C of dissolvings (1 ~ 10h), is cooled to room temperature, obtains poly-vinyl alcohol solution;
(3) graphene oxide solution and poly-vinyl alcohol solution mixed and stir, obtaining the spinning solution of graphene oxide and polyvinyl alcohol, in described spinning solution, the mass fraction of polyvinyl alcohol is 1 ~ 80wt%;
(4) above-mentioned spinning solution is joined in electrospinning device carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 10 ~ 35kV, receiving range 5 ~ 20cm, flow velocity 0.01 ~ 25mL/h, receiving system rotating speed 50 ~ 800rpm, temperature 10 ~ 35 DEG C, humidity 30 ~ 55%;
(5) by the nano fibrous membrane freeze drying (5 ~ 48h) that step (4) is obtained, i.e. obtained Graphene/polyvinyl alcohol nanofiber membrane adsorbent.
Step (3) mixing speed is 50 ~ 600 turns/min, and mixing time is 0.5 ~ 12h.
Graphene oxide in step (3) described spinning solution is 1 ~ 80wt% relative to the mass fraction of polyvinyl alcohol.
In described spinning solution, the mass fraction of polyvinyl alcohol is 6 ~ 15wt%.
Graphene/polyvinyl alcohol nanofiber membrane adsorbent prepared by said method, the average diameter of described nano fibrous membrane is 30 ~ 600nm, and porosity is 20 ~ 90%.
Described Graphene/the application of polyvinyl alcohol nanofiber membrane adsorbent in Adsorption of Heavy Metal Ions.
The present invention has following beneficial effect:
The preparation process environmental protection of Electrospun nano-fibers film of the present invention, non-secondary pollution, uses deionization water as solvent, without the need to an organic solvent and toxic chemical substance; Adsorption operations is simple; The graphene oxide prepared and polyvinyl alcohol nanofiber membrane have that specific area is large, porosity high, the contact area with heavy metal ion can be increased, increase adsorption capacity, shorten time of equilibrium adsorption, effectively can adsorb the heavy metal ion in waste water, and can effectively be separated; There is interaction of hydrogen bond between graphene oxide and polyvinyl alcohol, can prevent graphene oxide from coming off from nano fibrous membrane, enable nano fibrous membrane recycling.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of Electrospun nano-fibers film preparation of the present invention, shown in it: the mixed solution of 1 graphene oxide and polyvinyl alcohol; 2 syringes; 3 high voltage sourcies; 4 cylinder collectors; 5 graphene oxides and polyvinyl alcohol nanofiber membrane; 6 polyvinyl alcohol nanos; 7 graphene oxides.
Fig. 2 is the SEM Electronic Speculum figure of the Electrospun nano-fibers film that embodiment 4 obtains.
Fig. 3 is the TEM Electronic Speculum figure of the Electrospun nano-fibers film that embodiment 4 obtains.
Fig. 4 is that the obtained Electrospun nano-fibers film of embodiment 4 is at different temperatures to Cu
2+(a) and Cd
2+the absorption property figure of (b).
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.
Embodiment 1
A preparation method for the Electrospun nano-fibers film of Adsorption of Heavy Metal Ions, comprises following operating procedure:
(1) 12mg graphene oxide is added in 5g deionized water, after ultrasonic process 0.5h, obtain finely dispersed graphene oxide solution;
(2) 1.2g polyvinyl alcohol is joined in 10g deionized water, solution is heated to 88 DEG C, dissolve 3h, be cooled to room temperature, obtain poly-vinyl alcohol solution;
(3) by graphene oxide water solution and poly-vinyl alcohol solution mixing, then low whipping speed is stir 0.5h under 100 turns/min condition, obtain the spinning solution of graphene oxide and polyvinyl alcohol, in this spinning solution, the mass fraction of polyvinyl alcohol is 8wt%;
(4) joined in electrospinning device by above-mentioned spinning solution and carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 18kV, receiving range 15cm, flow velocity 1mL/h, receiving system rotating speed 200rpm, temperature 25 DEG C, humidity 45%;
(5) obtained graphene oxide and polyvinyl alcohol nanofiber membrane are put into the dry 24h of freeze-dryer.
Graphene oxide in the solution that described step (3) obtains is 1wt% relative to the mass fraction of polyvinyl alcohol.
The average diameter of the Electrospun nano-fibers film that described step (4) obtains is 82nm, and porosity is 66%.
Embodiment 2
A preparation method for the Electrospun nano-fibers film of Adsorption of Heavy Metal Ions, comprises following operating procedure:
(1) 84mg graphene oxide is added in 5g deionized water, after ultrasonic process 1h, obtain finely dispersed graphene oxide solution;
(2) 1.2g polyvinyl alcohol is joined in 10g deionized water, solution is heated to 92 DEG C, dissolve 3h, be cooled to room temperature, obtain poly-vinyl alcohol solution;
(3) by graphene oxide water solution and poly-vinyl alcohol solution mixing, then low whipping speed is stir 3h under 150 turns/min condition, and obtain the spinning solution of graphene oxide and polyvinyl alcohol, in this spinning solution, the mass fraction of polyvinyl alcohol is 8wt%;
(4) joined in electrospinning device by above-mentioned spinning solution and carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 24kV, receiving range 15cm, flow velocity 1mL/h, receiving system rotating speed 250rpm, temperature 25 DEG C, humidity 45%;
(5) obtained graphene oxide and polyvinyl alcohol nanofiber membrane are put into the dry 24h of freeze-dryer.
Graphene oxide in the solution that described step (3) obtains is 7wt% relative to the mass fraction of polyvinyl alcohol.
The average diameter of the Electrospun nano-fibers film that described step (4) obtains is 140nm, and porosity is 74%.
Embodiment 3
A preparation method for the Electrospun nano-fibers film of Adsorption of Heavy Metal Ions, comprises following operating procedure:
(1) 120mg graphene oxide is added in 5g deionized water, after ultrasonic process 3h, obtain finely dispersed graphene oxide solution;
(2) 1.2g polyvinyl alcohol is joined in 10g deionized water, solution is heated to 95 DEG C, dissolve 3.5h, be cooled to room temperature, obtain poly-vinyl alcohol solution;
(3) by graphene oxide water solution and poly-vinyl alcohol solution mixing, then low whipping speed is stir 5h under 250 turns/min condition, and obtain the spinning solution of graphene oxide and polyvinyl alcohol, in this spinning solution, the mass fraction of polyvinyl alcohol is 8wt%;
(4) joined in electrospinning device by above-mentioned spinning solution and carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 30kV, receiving range 15cm, flow velocity 0.8mL/h, receiving system rotating speed 300rpm, temperature 25 DEG C, humidity 42%;
(5) obtained graphene oxide and polyvinyl alcohol nanofiber membrane are put into the dry 48h of freeze-dryer.
Graphene oxide in the solution that described step (3) obtains is 10wt% relative to the mass fraction of polyvinyl alcohol.
The average diameter of the Electrospun nano-fibers film that described step (4) obtains is 90nm, and porosity is 78%.
Embodiment 4
A preparation method for the Electrospun nano-fibers film of Adsorption of Heavy Metal Ions, comprises following operating procedure:
(1) 182mg graphene oxide is added in 5g deionized water, after ultrasonic process 4h, obtain finely dispersed graphene oxide solution;
(2) 0.9g polyvinyl alcohol is joined in 10g deionized water, solution is heated to 95 DEG C, dissolve 4h, be cooled to room temperature, obtain poly-vinyl alcohol solution;
(3) by graphene oxide water solution and poly-vinyl alcohol solution mixing, then low whipping speed is stir 10h under 300 turns/min condition, and obtain the spinning solution of graphene oxide and polyvinyl alcohol, in this spinning solution, the mass fraction of polyvinyl alcohol is 6wt%;
(4) joined in electrospinning device by above-mentioned spinning solution and carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 23kV, receiving range 15cm, flow velocity 0.8mL/h, receiving system rotating speed 400rpm, temperature 25 DEG C, humidity 45%;
(5) obtained graphene oxide and polyvinyl alcohol nanofiber membrane are put into the dry 48h of freeze-dryer.
Graphene oxide in the solution that described step (3) obtains is 20wt% relative to the mass fraction of polyvinyl alcohol.
The average diameter of the Electrospun nano-fibers film that described step (4) obtains is 110nm, and porosity is 83%.
Embodiment 5
A preparation method for the Electrospun nano-fibers film of Adsorption of Heavy Metal Ions, comprises following operating procedure:
(1) 600mg graphene oxide is added in 5g deionized water, after ultrasonic process 4h, obtain finely dispersed graphene oxide solution;
(2) 1.5g polyvinyl alcohol is joined in 10g deionized water, solution is heated to 95 DEG C, dissolve 4h, be cooled to room temperature, obtain poly-vinyl alcohol solution;
(3) by graphene oxide water solution and poly-vinyl alcohol solution mixing, then low whipping speed is stir 10h under 300 turns/min condition, obtain the spinning solution of graphene oxide and polyvinyl alcohol, in this spinning solution, the mass fraction of polyvinyl alcohol is 10wt%;
(4) joined in electrospinning device by above-mentioned spinning solution and carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 28kV, receiving range 15cm, flow velocity 0.7mL/h, receiving system rotating speed 300rpm, temperature 25 DEG C, humidity 45%;
(5) obtained graphene oxide and polyvinyl alcohol nanofiber membrane are put into the dry 48h of freeze-dryer.
Graphene oxide in the solution that described step (3) obtains is 40wt% relative to the mass fraction of polyvinyl alcohol.
The average diameter of the Electrospun nano-fibers film that described step (4) obtains is 200nm, and porosity is 89%.
Embodiment 6
A preparation method for the Electrospun nano-fibers film of Adsorption of Heavy Metal Ions, comprises following operating procedure:
(1) 1g graphene oxide is added in 5g deionized water, after ultrasonic process 4h, obtain finely dispersed graphene oxide solution;
(2) 1.8g polyvinyl alcohol is joined in 10g deionized water, solution is heated to 95 DEG C, dissolve 4h, be cooled to room temperature, obtain poly-vinyl alcohol solution;
(3) by graphene oxide water solution and poly-vinyl alcohol solution mixing, then low whipping speed is stir 10h under 300 turns/min condition, obtain the spinning solution of graphene oxide and polyvinyl alcohol, in this spinning solution, the mass fraction of polyvinyl alcohol is 12wt%;
(4) joined in electrospinning device by above-mentioned spinning solution and carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 23kV, receiving range 15cm, flow velocity 0.9mL/h, receiving system rotating speed 500rpm, temperature 25 DEG C, humidity 45%;
(5) obtained graphene oxide and polyvinyl alcohol nanofiber membrane are put into the dry 48h of freeze-dryer.
Graphene oxide in the solution that described step (3) obtains is 60wt% relative to the mass fraction of polyvinyl alcohol.
The average diameter of the Electrospun nano-fibers film that described step (4) obtains is 250nm, and porosity is 88%.
The present invention is with heavy metal ion Cu
2+and Cd
2+for example, investigate Electrospun nano-fibers film prepared in assessment embodiment 1 ~ 6 to Cu
2+and Cd
2+removal effect, result is as shown in table 1.
Table 1 Electrospun nano-fibers film is to Cu
2+and Cd
2+adsorption capacity
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not defining embodiments of the present invention.For those of ordinary skill in the field, other multi-form change or variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (8)
1. a preparation method for Graphene/polyvinyl alcohol nanofiber membrane adsorbent, is characterized in that, comprise the following steps:
(1) graphene oxide is added in deionized water, after ultrasonic 0.5 ~ 4h, obtain finely dispersed graphene oxide solution;
(2) polyvinyl alcohol is joined in deionized water, solution is heated to 40 ~ 100 DEG C of dissolvings, is cooled to room temperature, obtains poly-vinyl alcohol solution;
(3) graphene oxide solution and poly-vinyl alcohol solution mixed and stir, obtaining the spinning solution of graphene oxide and polyvinyl alcohol, in described spinning solution, the mass fraction of polyvinyl alcohol is 1 ~ 80wt%;
(4) above-mentioned spinning solution is joined in electrospinning device carry out spinning, obtain graphene oxide and polyvinyl alcohol nanofiber membrane, electrospinning conditions is: spinning voltage 10 ~ 35kV, receiving range 5 ~ 20cm, flow velocity 0.01 ~ 25mL/h, receiving system rotating speed 50 ~ 800rpm, temperature 10 ~ 35 DEG C, humidity 30 ~ 55%;
(5) by the nano fibrous membrane freeze drying that step (4) is obtained, i.e. obtained Graphene/polyvinyl alcohol nanofiber membrane adsorbent.
2. method according to claim 1, is characterized in that, step (3) mixing speed is 50 ~ 600 turns/min, and mixing time is 0.5 ~ 12h.
3. method according to claim 1 and 2, is characterized in that, the graphene oxide in step (3) described spinning solution is 1 ~ 80wt% relative to the mass fraction of polyvinyl alcohol.
4. method according to claim 3, is characterized in that, in described spinning solution, the mass fraction of polyvinyl alcohol is 6 ~ 15wt%.
5. method according to claim 1 and 2, is characterized in that, the nano fibrous membrane cryodesiccated time that step (5) obtains is 5 ~ 48h.
6. Graphene/polyvinyl alcohol nanofiber membrane adsorbent of preparing of method described in any one of Claims 1 to 5.
7. Graphene according to claim 6/polyvinyl alcohol nanofiber membrane adsorbent, is characterized in that, the average diameter of described nano fibrous membrane is 30 ~ 600nm, and porosity is 20 ~ 90%.
8. Graphene described in the claim 6 or 7/application of polyvinyl alcohol nanofiber membrane adsorbent in Adsorption of Heavy Metal Ions.
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Application publication date: 20160203 |