CN111648044A - Super-absorbent nanofiber membrane and preparation method thereof - Google Patents
Super-absorbent nanofiber membrane and preparation method thereof Download PDFInfo
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- CN111648044A CN111648044A CN201910160707.1A CN201910160707A CN111648044A CN 111648044 A CN111648044 A CN 111648044A CN 201910160707 A CN201910160707 A CN 201910160707A CN 111648044 A CN111648044 A CN 111648044A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
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Abstract
The invention discloses a super water-absorbing nanofiber membrane and a preparation method thereof, wherein the nanofiber membrane is prepared from polyacrylic acid and polyvinyl alcohol, and the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10: 1; the diameter of the super water absorption nano fiber is 150-300nm, the aperture is 0.5-1.5 mu m, the porosity is 50-85%, and the water absorption multiplying power is 5-200 g/g. The preparation method comprises the steps of dissolving two polymers of polyacrylic acid and polyvinyl alcohol in water to prepare a mixed water-soluble spinning solution, preparing the super water-absorbing nano fiber membrane by an electrostatic spinning technology, and inducing the fiber membrane to perform esterification crosslinking reaction in a heating treatment mode to endow the crosslinked fiber membrane with water-absorbing but water-insoluble capacity in oil/water emulsion. The prepared nanofiber membrane has high porosity and large specific surface area, can quickly absorb moisture in an oil phase medium containing water, and can efficiently and quickly remove trace moisture and impurities in oil phase liquid environments such as fuel and the like.
Description
Technical Field
The invention belongs to the technical field of water-absorbing fibers, and particularly relates to a super water-absorbing nanofiber membrane and a preparation method thereof.
Background
The super absorbent fiber is a special functional fiber developed after super absorbent resin, and is extension and expansion of the super absorbent resin. As the super absorbent fiber has many superiorities, the research on the super absorbent fiber at home and abroad is very active. At present, the production countries of the super absorbent fiber mainly comprise Canada, Japan, United states, British, Germany and the like.
Polyvinyl alcohol (PVA) is a polyhydroxy polymer with excellent performance and wide application, the polyvinyl alcohol (PVA) fiber has the advantages of hydrophilicity, high strength, high modulus, good wear resistance, good thermal performance, excellent corrosion resistance and weather resistance, good interfacial adhesion with a matrix material in a composite material and the like, and the polyvinyl alcohol (PVA) can be applied to the preparation of water-absorbing fibers, but has slower water-absorbing speed and is gradually dissolved in water. Polyacrylic Acid (PA) is another water-soluble polymer resin, and is widely applied to the fields of sewage treatment and water-absorbent resin; also, Polyacrylic Acid (PA) fibers dissolve in water by themselves and cannot be used alone as a water absorbing material.
Disclosure of Invention
The invention aims to provide a super water-absorbing nanofiber membrane and a preparation method thereof, which overcome the defects of low water absorption rate and water solubility of the existing water-absorbing resin used in an oil-water separation system and realize one-time water removal through permeation of water-containing oil-phase emulsion.
Therefore, the invention provides a super water-absorbing nanofiber membrane which is prepared from polyacrylic acid and polyvinyl alcohol, wherein the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10: 1; the diameter of the super water absorption nano fiber is 150-300nm, the pore diameter is 0.5-1.5 mu m, the porosity is 50-85%, and the water absorption multiplying power is 5-200 g/g.
The invention also provides a preparation method of the super water-absorbing nanofiber membrane, which comprises the following steps:
(1) uniformly mixing polyacrylic acid, polyvinyl alcohol and deionized water to obtain a mixed solution, wherein the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10:1, and the mass concentration of the mixed solution is 5-30%;
(2) injecting the mixed solution into an electrostatic spinning device for spinning to obtain nano fibers; the voltage is 20-35 kilovolts, and the collecting roller is grounded;
(3) and (3) drying and carrying out thermal crosslinking treatment on the nano-fibers in sequence to obtain the super water-absorbing nano-fiber membrane.
Preferably, in the step (1), the polyacrylic acid has a molecular weight of 10 to 50 ten thousand, the polyvinyl alcohol has a molecular weight of 5 to 25 ten thousand, and the alcoholysis degree is 88 to 99.9%.
Preferably, in the step (3), the drying temperature is 50-90 ℃, the thermal crosslinking temperature is 130-190 ℃, and the thermal crosslinking time is 10-120 min.
Compared with the prior art, the invention has the advantages and positive effects that: the invention provides a super water-absorbing nano-fiber membrane and a preparation method thereof, which are characterized in that two polymers of polyacrylic acid and polyvinyl alcohol are dissolved in water to prepare a mixed water-soluble spinning solution, the super water-absorbing nano-fiber membrane with the diameter within the range of 150-300nm is prepared by an electrostatic spinning technology, and the fiber membrane is induced to carry out esterification crosslinking reaction by a heating treatment mode, so that the water-absorbing but water-insoluble capacity of the crosslinked fiber membrane in oil/water emulsion is endowed. The prepared polyacrylic acid/polyvinyl alcohol super-absorbent nanofiber membrane has high porosity and large specific surface area, can quickly absorb moisture in an oil phase medium containing water, and can efficiently and quickly remove trace moisture and impurities in oil phase liquid environments such as fuel and the like. In addition, water is used as a solvent in the electrostatic spinning process, environmental protection problems such as organic solvent recovery and the like are not involved, the raw material source is wide, and the electrostatic spinning method has good market application value.
Other features and advantages of the present invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
Drawings
FIG. 1 is an SEM image of super absorbent nanofibers prepared in example 1 of the present invention;
FIG. 2 is an optical micrograph of an oil-water emulsion;
FIG. 3 is an optical micrograph of an oil-water emulsion after filtration treatment of the super absorbent nanofibers prepared in example 1 of the present invention.
Detailed Description
The following detailed description of specific embodiments of the present invention is provided to illustrate and explain the present invention and to be understood not to limit the present invention.
The super water absorption nanofiber membrane is prepared from polyacrylic acid and polyvinyl alcohol, wherein the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10: 1; the diameter of the super water absorption nano fiber is 150-300nm, the pore diameter is 0.5-1.5 mu m, and the porosity is 75-82%.
(1) Uniformly mixing polyacrylic acid, polyvinyl alcohol and deionized water to obtain a mixed solution, wherein the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10:1, and the mass concentration of the mixed solution is 5-30%;
(2) injecting the mixed solution into an electrostatic spinning device for spinning to obtain nano fibers; the receiving distance is 10-25 cm, the operating speed of the sliding table is 0-2 m/min, the rotating speed of the roller is 0-120 r/min, and the propelling speed of the injector is 0.2-2 ml/h; connecting the positive high voltage of a high-voltage direct-current power supply to a syringe needle, adjusting the voltage to be 20-35 kilovolts, and grounding a collecting roller;
(3) and (3) drying and carrying out thermal crosslinking treatment on the nano-fibers in sequence to obtain the super water-absorbing nano-fiber membrane.
In the step (1), the molecular weight of polyacrylic acid is 10-50 ten thousand, the molecular weight of polyvinyl alcohol is 5-25 ten thousand, and the alcoholysis degree is 88-99.9%.
In the step (3), the drying temperature is 50-90 ℃, the thermal crosslinking temperature is 130-190 ℃, and the thermal crosslinking time is 10-120 min.
The invention discloses a super water-absorbing nano-fiber membrane and a preparation method thereof, which are characterized in that two polymers of polyacrylic acid and polyvinyl alcohol are dissolved in water to prepare a mixed water-soluble spinning solution, a super water-absorbing nano-fiber membrane with the diameter within the range of 150-300nm is prepared by an electrostatic spinning technology, and the fiber membrane is induced to carry out esterification crosslinking reaction by a heating treatment mode, so that the water-absorbing but water-insoluble capacity of the crosslinked fiber membrane in oil/water emulsion is endowed. The prepared polyacrylic acid/polyvinyl alcohol super-absorbent nanofiber membrane has high porosity and large specific surface area, can quickly absorb moisture in an oil phase medium containing water, and can efficiently and quickly remove trace moisture and impurities in oil phase liquid environments such as fuel and the like. In addition, water is used as a solvent in the electrostatic spinning process, environmental protection problems such as organic solvent recovery and the like are not involved, the raw material source is wide, and the electrostatic spinning method has good market application value.
Example 1
The preparation method of the super water-absorbing nanofiber membrane comprises the following steps:
(1) adding 5g of polyvinyl alcohol into 45g of deionized water, stirring and dissolving for 2 hours in a water bath heating environment at 80 ℃, and cooling to room temperature to obtain a polyvinyl alcohol solution with the mass fraction of 10 wt%; the molecular weight of the polyvinyl alcohol is 8 ten thousand, and the alcoholysis degree is 88%. Adding polyacrylic acid into deionized water to prepare a polyacrylic acid solution with the mass fraction of 30wt%, wherein the molecular weight of the polyacrylic acid is 20 ten thousand. Mixing 30wt% polyacrylic acid aqueous solution, 10wt% polyvinyl alcohol aqueous solution and deionized water according to the weight ratio of 3.99 g: 48 g: 8.01g, and stirring at room temperature for 12 hours to obtain a uniform polyacrylic acid/polyvinyl alcohol mixed electrospinning solution with the mass fraction of 10 wt%.
(2) The mixed electrospinning solution was drawn into a 10ml syringe and spun simultaneously on a multi-needle electrospinning apparatus with 4 needles. The spinning parameters were as follows: the injection speed of the spinning solution was 1 ml per hour, the slide moved by 20 cm, and the take-up distance from the needle to the drum was 20 cm. A layer of glossy paper is covered on the roller to be used as a receiving end, and the rotating speed of the roller is adjusted to be 50 revolutions per minute. Connecting the positive high voltage of a high voltage power supply to a syringe needle, adjusting the voltage to 25 kilovolts, grounding a roller, and spinning for 3 hours in an environment with the temperature of 22 ℃ and the humidity of 35 wt%.
(3) And (3) after spinning is finished, removing the glossy paper and the nanofiber membrane on the glossy paper from the roller, and treating the glossy paper and the nanofiber membrane in a 60-DEG C oven for 2 hours to remove residual solvent water on the fiber membrane. And (3) placing the dried nanofiber membrane in a vacuum oven which is heated to 160 ℃ for treatment for 30 minutes to obtain the super-absorbent nanofiber membrane.
The super water absorbent nanofiber membrane prepared in example 1 had a pore diameter of 523.2nm and a porosity of 79.6%.
Fig. 1 is a scanning electron microscope photograph of the super absorbent nanofiber membrane prepared in example 1, and as can be seen from fig. 1, the fiber diameter distribution is uniform, the average diameter is about 200 nm, the fiber surface is smooth, beads and point-throwing defects do not exist, the fiber membrane has a pore size distribution of nano-micron scale, and the filtration of substances of nano-micron and above can be realized.
Fig. 2 is an optical microscope photograph of an oil-water emulsion subjected to self-made ultrasonic dispersion treatment, the super water-absorbent nanofiber membrane prepared in example 1 can be used as a disposable permeable water-fine membrane of the oil-water emulsion, and fig. 3 is an optical microscope photograph of an oil-water emulsion subjected to filtration treatment by the super water-absorbent nanofiber membrane prepared in example 1. As can be seen from the comparison of FIG. 2 and FIG. 3, the oil-water emulsion before filtration is in a turbid emulsion state, and a plurality of dispersed water droplets can be seen from an optical microscope; the oil phase is clear after filtration, and dispersed water droplets are not found in an optical fiber microscope photo, which shows that the super-absorbent nanofiber membrane in example 1 has an excellent effect on removing trace water in the oil phase; measured by a karl fischer automatic moisture meter, the water content of the oil-water emulsion filtered by the super water-absorbing nanofiber membrane prepared in example 1 is reduced to 4.5% of the original content, and the oil phase is changed from turbid to clear.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (4)
1. A super water-absorbing nanofiber membrane is characterized in that,
the polyacrylic acid and polyvinyl alcohol composite material is prepared from polyacrylic acid and polyvinyl alcohol, wherein the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10: 1;
the diameter of the super water absorption nano fiber is 150-300nm, the pore diameter is 0.5-1.5 mu m, the porosity is 50-85%, and the water absorption multiplying power is 5-200 g/g.
2. The method for preparing a superabsorbent nanofiber membrane as claimed in claim 1, comprising the steps of:
(1) uniformly mixing polyacrylic acid, polyvinyl alcohol and deionized water to obtain a mixed solution, wherein the mass ratio of the polyacrylic acid to the polyvinyl alcohol is 1:10-10:1, and the mass concentration of the mixed solution is 5-30%;
(2) injecting the mixed solution into an electrostatic spinning device for spinning to obtain nano fibers; the voltage is 20-35 kilovolts, and the collecting roller is grounded;
(3) and (3) drying and carrying out thermal crosslinking treatment on the nano-fibers in sequence to obtain the super water-absorbing nano-fiber membrane.
3. The method of preparing a superabsorbent nanofiber membrane as claimed in claim 2,
in the step (1), the molecular weight of polyacrylic acid is 10-50 ten thousand, the molecular weight of polyvinyl alcohol is 5-25 ten thousand, and the alcoholysis degree is 88-99.9%.
4. The method of preparing a superabsorbent nanofiber membrane as claimed in claim 2,
in the step (3), the drying temperature is 50-90 ℃, the thermal crosslinking temperature is 130-190 ℃, and the thermal crosslinking time is 10-120 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910160707.1A CN111648044A (en) | 2019-03-04 | 2019-03-04 | Super-absorbent nanofiber membrane and preparation method thereof |
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| CN201910160707.1A CN111648044A (en) | 2019-03-04 | 2019-03-04 | Super-absorbent nanofiber membrane and preparation method thereof |
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| CN114515518A (en) * | 2022-03-07 | 2022-05-20 | 四川大学 | Skin collagen fiber-based composite membrane material and preparation method and application thereof |
| CN115198442A (en) * | 2022-06-17 | 2022-10-18 | 青岛大学 | Preparation method and application of nano-film with directional water transmission and efficient antibacterial functions |
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| CN115198442B (en) * | 2022-06-17 | 2024-04-12 | 青岛大学 | Preparation method and application of nano film with directional moisture transmission and efficient antibacterial functions |
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Application publication date: 20200911 |