CN105200666A - Preparation method of superhydrophobic/superoleophylic hollow microspherical PVDF nano fibers - Google Patents
Preparation method of superhydrophobic/superoleophylic hollow microspherical PVDF nano fibers Download PDFInfo
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Abstract
The invention belongs to the field of nano fiber material preparation, and in particular relates to a preparation method of superhydrophobic/superoleophylic hollow microspherical PVDF nano fibers. The preparation method comprises the following steps of: (1) preparing a PVDF electrostatic spinning liquid: dissolving PVDF in N,N-dimethylformamide (DMF) to prepare the PVDF electrostatic spinning solution, and dropwise adding a small amount of deionized water to the electrostatic spinning solution; (2) carrying out electrostatic spinning on the solution, wherein the hollow microspherical PVDF nano fibers are promoted to form by a phase separation mechanism of the small amount of water. The PVDF hollow microspherical nano fibers are prepared by an electrostatic spinning technology, and the morphology of the nano fibers is controlled by adjusting the content of deionized water in the electrostatic spinning solution. The preparation method is low in cost, simple to operate and environmentally friendly; and the product has excellent hydrophobic and oleophylic effects.
Description
Technical field
The invention belongs to a kind of preparation method field of novel nano fibrous material, be specifically related to a kind of preparation method of super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber.
Background technology
In recent years, in the process of oil exploitation, transport and use, be usually attended by the situation of Oil spills contaminated environment.Discharge severe contamination natural environment that is industrial and oil-polluted water in living in addition, therefore develops water body oil pollution improvement new material, new technology is significant.China processes petroleum pollution in ocean at present and mainly adopts oil absorption material, and the method can be avoided secondary pollution and effectively can reclaim oil spilling.Conventional oil absorption material comprises traditional oil absorption material, such as maize straw, cotton fiber, bombax cotton, zeolite etc.; Also comprise new function material, such as resinae oil absorption material, carbon sponge, CNT, metal-organic framework material (MOF).
The method of current electrospun nanofibers is subject to extensive concern.Researcher can obtain the nanofiber with New function by the microstructure of regulation and control nanofiber, thus meets material function requirement.Nanofiber prepared by electrostatic spinning can be used as oil absorption material can make oil enter in material void and material matrix, thus makes it have higher oil suction efficiency.
Summary of the invention
The object of the present invention is to provide a kind of simple to operate, with low cost, object product environmental friendliness, the preparation method of the super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber that oil absorbency is strong.
For solving the problems of the technologies described above, the present invention realizes like this.
A preparation method for super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber, can implement as follows.
(1) preparation of electrostatic spinning solution: remove ionized water and add in DMF (DMF), adds PVDF, finally 50 when stirring in solution
okeep agitation 24 hours under C condition.
(2) object product preparation: step (1) gained electrostatic spinning solution is carried out electrostatic spinning; After DMF (DMF) volatilization solidification, form fibrofelt at receiving terminal; Dry after fibrofelt is collected, obtain object product super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber.
As a kind of preferred version, in step of the present invention (2), step (1) gained electrostatic spinning solution is placed in 10 ~ 20ml injector for medical purpose and carries out electrostatic spinning; The voltage of electrostatic spinning is 18kV, and the distance between injector for medical purpose shower nozzle and receiver is 15cm, and the flow control of electrostatic spinning solution is 2.0ml/h.
Further, in step of the present invention (1), in mass percentage, PVDF accounts for DMF (DMF) and removes 5% ~ 15% of ionized water.
Further, in step of the present invention (2), in mass percentage, in electrostatic spinning solution, deionized water accounts for 0 ~ 20% of PVDF.
Further, in step of the present invention (2), in mass percentage, in electrostatic spinning solution, deionized water content is 0 ~ 2.5%.
Further, in step of the present invention (2), receiver adopts high-speed rotary rotary drum aluminium foil receiver, and rotating speed is 500 turns/min.
The present invention have selected the PVDF parting material with excellent chemical stability and stain resistance.By PVDF/DMF/H in electrostatic spinning liquid
2h in O
2the control of O content, makes PVDF realize liquid-liquid phase separation in the process of electrostatic spinning thus prepares the PVDF nanofiber with hollow microsphere structure.Have studied the infiltrating impact of fiber surface microstructure effects on surface and be applied to, in oil suction experiment, obtain the PVDF nano-fiber material with super-hydrophobic/super-oleophilic.
The present invention is simple to operate, with low cost, and object product environmental friendliness, oil absorbency is strong.The present invention utilizes in electrostatic spinning solution and adds non-solvent deionized water, thus in the process of electrostatic spinning, define tiny balloon shape PVDF nanofiber mats.Respectively preparation-obtained nanofiber is immersed in lubricating oil to be measured, takes out after 1 minute in immersion, check weighing after it leaves standstill 2 minutes.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Protection scope of the present invention is not only confined to the statement of following content.
The SEM figure of Fig. 1-1, Fig. 1-2, Fig. 1-3, Fig. 1-4, Fig. 1-5 and Fig. 1-6 PVDF nanofiber obtained by the Electrospun solution of different moisture content of the present invention.
Fig. 2 is the water contact angle of PVDF nanofiber mats of the present invention.
Fig. 3 is water droplet of the present invention and the photo of oil droplet on nanofiber.
Fig. 4 is PVDF nanofiber oil absorption of the present invention curve over time.
Detailed description of the invention
Water used in following example is deionized water; Agents useful for same, except special instruction, all adopts AR; In embodiment, the SEM picture of obtained PVDF nanofiber oil absorption material is scanned by HitachiS-3500N type ESEM and obtains; Videomicroscopy carries out measurement for the contact angle and water droplet photo that have studied nanofiber surface and water and takes pictures in the present invention.The SEM figure of the PVDF nanofiber of Fig. 1 obtained by the Electrospun solution of different moisture content of the present invention; Wherein, A:0.0%, B:0.5%, C:1.0%, D:1.5%, E:2.0%, F:2.5%.
embodiment 1.
Take 3gPVDF powder, slowly join in 18gDMF under magnetic stirring, be then placed in 50 DEG C of water-bath magnetic agitation 24h and form electrostatic spinning solution.By this solution cool to room temperature state before electrostatic spinning.The 20ml plastic injector be placed in by above-mentioned electrostatic spinning solution, syringe is furnished with 0.5mm diameter stainless steel syringe needle.The voltage of electrostatic spinning is 18kV, and the distance between shower nozzle and receiver is 15cm, and the fltting speed of syringe is 2ml/h, casing humidity 50%.Solidify due to the volatilization of volatile solvent DMF in electrostatic spinning process, aluminium foil is formed one deck PVDF fibrofelt.PVDF fibrofelt is collected and is placed on 50
odry 24h in C vacuum drying oven, obtains hollow microspheroidal PVDF nanofiber.Take the PVDF nanofiber mats sample of 0.5g, be placed in the close net corbeil of stainless steel.Then it is fully immersed in lubricating oil to be measured.Take out the corbeil holding PVDF nanofiber mats in immersion after 1 minute, after it leaves standstill 2 minutes, be positioned over check weighing on electronic balance.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.The oil absorbency of PVDF nanofiber mats can use following formula to calculate:
, m in formula
0for the original quality of PVDF nanofiber mats, m
tfor the quality after its oil suction a period of time.Nanofiber reaches oil suction balance (see figure 4) after oil absorbency reaches optimum value 11.76g/g 2 minutes time substantially.
embodiment 2.
Take 3gPVDF powder, slowly join in the mixed solution of 18gDMF and 0.1g deionized water under magnetic stirring, be then placed in 50 DEG C of water-bath magnetic agitation 24h and form electrostatic spinning solution.By this solution cool to room temperature state before electrostatic spinning.The 20ml plastic injector that above-mentioned electrostatic spinning solution is placed in, syringe is furnished with 0.5mm diameter stainless steel syringe needle.The voltage of electrostatic spinning is 18kV, and the distance between shower nozzle and receiver is 15cm, and the fltting speed of syringe is 2ml/h, casing humidity 50%.Solidify due to the volatilization of volatile solvent DMF in electrostatic spinning process, aluminium foil is formed one deck PVDF fibrofelt.PVDF fibrofelt is collected and is placed on 50
odry 24h in C vacuum drying oven, obtains hollow microspheroidal PVDF nanofiber.Take the PVDF nanofiber mats sample of 0.5g, be placed in the close net corbeil of stainless steel.Then it is fully immersed in lubricating oil to be measured.Take out the corbeil holding PVDF nanofiber mats in immersion after 1 minute, after it leaves standstill 2 minutes, be positioned over check weighing on electronic balance.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.The oil absorbency of PVDF nanofiber mats can use following formula to calculate:
, m in formula
0for the original quality of PVDF nanofiber mats, m
tfor the quality after its oil suction a period of time.Nanofiber reaches oil suction balance (see figure 4) after oil absorbency reaches optimum value 14.9g/g 5 minutes time substantially.
embodiment 3.
Take 3gPVDF powder, slowly join in the mixed solution of 18gDMF and 0.2g deionized water under magnetic stirring, be then placed in 50 DEG C of water-bath magnetic agitation 24h and form electrostatic spinning solution.By this solution cool to room temperature state before electrostatic spinning.The 20ml plastic injector that above-mentioned electrostatic spinning solution is placed in, syringe is furnished with 0.5mm diameter stainless steel syringe needle.The voltage of electrostatic spinning is 18kV, and the distance between shower nozzle and receiver is 15cm, and the fltting speed of syringe is 2ml/h, casing humidity 50%.Solidify due to the volatilization of volatile solvent DMF in electrostatic spinning process, aluminium foil is formed one deck PVDF fibrofelt.PVDF fibrofelt is collected and is placed on 50
odry 24h in C vacuum drying oven, obtains hollow microspheroidal PVDF nanofiber.Take the PVDF nanofiber mats sample of 0.5g, be placed in the close net corbeil of stainless steel.Then it is fully immersed in lubricating oil to be measured.Take out the corbeil holding PVDF nanofiber mats in immersion after 1 minute, after it leaves standstill 2 minutes, be positioned over check weighing on electronic balance.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.The oil absorbency of PVDF nanofiber mats can use following formula to calculate:
, m in formula
0for the original quality of PVDF nanofiber mats, m
tfor the quality after its oil suction a period of time.Nanofiber reaches oil suction balance (see figure 4) after oil absorbency reaches optimum value 15.7g/g 7 minutes time substantially.
embodiment 4.
Take 3gPVDF powder, slowly join in the mixed solution of 18gDMF and 0.3g deionized water under magnetic stirring, be then placed in 50 DEG C of water-bath magnetic agitation 24h and form electrostatic spinning solution.By this solution cool to room temperature state before electrostatic spinning.The 20ml plastic injector that above-mentioned electrostatic spinning solution is placed in, syringe is furnished with 0.5mm diameter stainless steel syringe needle.The voltage of electrostatic spinning is 18kV, and the distance between shower nozzle and receiver is 15cm, and the fltting speed of syringe is 2ml/h, casing humidity 50%.Solidify due to the volatilization of volatile solvent DMF in electrostatic spinning process, aluminium foil is formed one deck PVDF fibrofelt.PVDF fibrofelt is collected and is placed on 50
odry 24h in C vacuum drying oven, obtains hollow microspheroidal PVDF nanofiber.Take the PVDF nanofiber mats sample of 0.5g, be placed in the close net corbeil of stainless steel.Then it is fully immersed in lubricating oil to be measured.Take out the corbeil holding PVDF nanofiber mats in immersion after 1 minute, after it leaves standstill 2 minutes, be positioned over check weighing on electronic balance.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.The oil absorbency of PVDF nanofiber mats can use following formula to calculate:
, m in formula
0for the original quality of PVDF nanofiber mats, m
tfor the quality after its oil suction a period of time.Nanofiber reaches oil suction balance (see figure 4) after oil absorbency reaches optimum value 17.08g/g 6 minutes time substantially.
embodiment 5.
Take 3gPVDF powder, slowly join in the mixed solution of 18gDMF and 0.4g deionized water under magnetic stirring, be then placed in 50 DEG C of water-bath magnetic agitation 24h and form electrostatic spinning solution.By this solution cool to room temperature state before electrostatic spinning.The 20ml plastic injector that above-mentioned electrostatic spinning solution is placed in, syringe is furnished with 0.5mm diameter stainless steel syringe needle.The voltage of electrostatic spinning is 18kV, and the distance between shower nozzle and receiver is 15cm, and the fltting speed of syringe is 2ml/h, casing humidity 50%.Solidify due to the volatilization of volatile solvent DMF in electrostatic spinning process, aluminium foil is formed one deck PVDF fibrofelt.PVDF fibrofelt is collected and is placed on 50
odry 24h in C vacuum drying oven, obtains hollow microspheroidal PVDF nanofiber.Take the PVDF nanofiber mats sample of 0.5g, be placed in the close net corbeil of stainless steel.Then it is fully immersed in lubricating oil to be measured.Take out the corbeil holding PVDF nanofiber mats in immersion after 1 minute, after it leaves standstill 2 minutes, be positioned over check weighing on electronic balance.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.The oil absorbency of PVDF nanofiber mats can use following formula to calculate:
, m in formula
0for the original quality of PVDF nanofiber mats, m
tfor the quality after its oil suction a period of time.Nanofiber reaches oil suction balance (see figure 4) after oil absorbency reaches optimum value 17.36g/g 7 minutes time substantially.
embodiment 6.
Take 3gPVDF powder, slowly join in the mixed solution of 18gDMF and 0.5g deionized water under magnetic stirring, be then placed in 50 DEG C of water-bath magnetic agitation 24h and form electrostatic spinning solution.By this solution cool to room temperature state before electrostatic spinning.The 20ml plastic injector that above-mentioned electrostatic spinning solution is placed in, syringe is furnished with 0.5mm diameter stainless steel syringe needle.The voltage of electrostatic spinning is 18kV, and the distance between shower nozzle and receiver is 15cm, and the fltting speed of syringe is 2ml/h, casing humidity 50%.Solidify due to the volatilization of volatile solvent DMF in electrostatic spinning process, aluminium foil is formed one deck PVDF fibrofelt.PVDF fibrofelt is collected and is placed on 50
odry 24h in C vacuum drying oven, obtains hollow microspheroidal PVDF nanofiber.Take the PVDF nanofiber mats sample of 0.5g, be placed in the close net corbeil of stainless steel.Then it is fully immersed in lubricating oil to be measured.Take out the corbeil holding PVDF nanofiber mats in immersion after 1 minute, after it leaves standstill 2 minutes, be positioned over check weighing on electronic balance.Repeat above operation, until the oil absorption of PVDF nanofiber mats sample is no longer calculate its oil absorbency after increase trend.The oil absorbency of PVDF nanofiber mats can use following formula to calculate:
, m in formula
0for the original quality of PVDF nanofiber mats, m
tfor the quality after its oil suction a period of time.Nanofiber reaches oil suction balance (see figure 4) after oil absorbency reaches optimum value 21.48g/g 6 minutes time substantially.
Claims (6)
1. a preparation method for super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber, is characterized in that, implements as follows:
(1) preparation of electrostatic spinning solution: remove ionized water and add in DMF (DMF), adds PVDF, finally 50 when stirring in solution
okeep agitation 24 hours under C condition;
(2) object product preparation: step (1) gained electrostatic spinning solution is carried out electrostatic spinning; DMF (DMF) and micro-deionized water volatilize solidification jointly, form fibrofelt at receiving terminal; Dry after fibrofelt is collected, obtain object product super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber.
2. the preparation method of super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber according to claim 1, is characterized in that: in described step (2), step (1) gained electrostatic spinning solution is placed in 10 ~ 20ml injector for medical purpose and carries out electrostatic spinning; The voltage of electrostatic spinning is 18kV, and the distance between injector for medical purpose shower nozzle and receiver is 15cm, and the flow control of electrostatic spinning solution is 2.0ml/h.
3. the preparation method of super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber according to claim 2, it is characterized in that: in described step (1), in mass percentage, PVDF accounts for DMF (DMF) and removes 5% ~ 15% of ionized water.
4. the preparation method of super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber according to claim 3, is characterized in that: in described step (2), in mass percentage, in electrostatic spinning solution, deionized water accounts for 0 ~ 20% of PVDF.
5. the preparation method of super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber according to claim 4, it is characterized in that: in described step (2), in mass percentage, in electrostatic spinning solution, deionized water content is 0 ~ 2.5%.
6. the preparation method of super-hydrophobic/super-oleophilic tiny balloon shape PVDF nanofiber according to claim 5, is characterized in that: in described step (2), and receiver adopts high-speed rotary rotary drum aluminium foil receiver, and rotating speed is 500 turns/min.
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| CN112877794A (en) * | 2020-12-21 | 2021-06-01 | 辽宁石油化工大学 | Method for preparing PVDF porous fiber through electrostatic spinning |
| CN113832706A (en) * | 2021-09-24 | 2021-12-24 | 天津工业大学 | Electrostatic spinning-based in-situ water electret method and fiber material with charge bubbles |
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