CN101928996A - Preparation method of fibrous membrane with super hydrophobic multi-stage nanometer structure - Google Patents
Preparation method of fibrous membrane with super hydrophobic multi-stage nanometer structure Download PDFInfo
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- CN101928996A CN101928996A CN 201010231199 CN201010231199A CN101928996A CN 101928996 A CN101928996 A CN 101928996A CN 201010231199 CN201010231199 CN 201010231199 CN 201010231199 A CN201010231199 A CN 201010231199A CN 101928996 A CN101928996 A CN 101928996A
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Abstract
The invention provides a preparation method of fibrous membrane with a super hydrophobic multi-stage nanometer structure, which is characterized by comprising the following specific steps: 1, at room temperature, adding hydrophobic polymer and hydrophobic inorganic nanoparticles into a sealed container filled with solvent, putting the sealed container on a magnetic stirrer to stir at the revolving speed of 10-200 rpm, and obtaining solution with even property; 2, at room temperature, inputting solution obtained in step 1 onto a spinning nozzle at constant flow velocity; connecting the spinning nozzle to a high voltage static generator to carry out electrostatic spinning; and receiving spun fiber by a receiver to obtain the fibrous membrane with super hydrophobic multi-stage nanometer structure. The invention can drastically improve the hydrophobic performance of the fibrous membrane.
Description
Technical field
The present invention relates to a kind of preparation method, belong to technical field of nano material with tunica fibrosa of super hydrophobic multi-stage nanometer structure.
Background technology
In recent years, electrostatic spinning technique is distributed in the simple but effective method that hundreds of nanometers arrives fiber in several micrometer ranges as a kind of diameter for preparing, and more and more comes into one's own, and has caused the extensive concern of various countries' researchers.Up to now, existing nearly hundred kinds of polymer are used to be prepared into the electrostatic spinning nano fiber film by solution or melt spinning.In in the past nearly 10 years, the electrostatic spinning nano fiber film has been applied in fields such as filtration, super hydrophobic material, catalytic reaction agent carrier, hypersensitivity biology sensor, bioengineered tissue, DSSC.
The researcher has reported the research for preparing superhydrophobic fibers by means of electrostatic spinning technique both at home and abroad, mainly concentrates on two aspects, the one, modify the electrostatic spinning fiber surface by fluorine-containing material, and obtain super-hydrophobic effect; But by increasing the roughness of fiber surface, the bead that promptly increases in the tunica fibrosa reaches super-hydrophobic effect; Also have the method for researcher in addition, on the electrostatic spinning fiber surface, decorate nano particle, obtain superhydrophobic fibers by self assembly layer by layer.These methods, the process that needs is comparatively loaded down with trivial details, and the mechanical strength of tunica fibrosa is relatively poor, has limited the practical application of superhydrophobic fibers film.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method, overcome that superhydrophobic fibers prepares shortcoming loaded down with trivial details, bad mechanical strength under the existence conditions with tunica fibrosa of super hydrophobic multi-stage nanometer structure.
In order to achieve the above object, the invention provides a kind of preparation method, it is characterized in that concrete steps are with tunica fibrosa of super hydrophobic multi-stage nanometer structure:
The first step: at room temperature, hydrophobic polymer and hydrophobicity inorganic nanoparticles are joined in the airtight vessel that fill solvent, be placed on the magnetic stirring apparatus,, obtain the solution of character homogeneous with the rotating speed stirring of 10-200rpm;
Second step: at room temperature, the solution that the first step is obtained is input on the spinning head with constant flow velocity, simultaneously spinning head is connected HV generator and carry out electrostatic spinning, spun fiber receives with receiving system, obtains having the tunica fibrosa of super hydrophobic multi-stage nanometer structure.
Hydrophobic polymer in the described first step is preferably polystyrene, polymethyl methacrylate, acetyl cellulose, Merlon, polyvinyl acetate, PLA, polyvinyl chloride, polyacrylonitrile, polycaprolactone, poly butylene succinate, poly-succinic acid-butanediol-altogether-and the mutual-phenenyl two acid bromide two alcohol ester, poly-hydroxyl valerate, polyethylene terephthalate, polyamide, PEI, polyformaldehyde or ethyl cellulose.
Hydrophobicity inorganic nanoparticles in the described first step is preferably the hydrophobic silica nano particle, and diameter is the 2-40 nanometer, and addition is the 5-20wt% of hydrophobic polymer fiber.
Solvent in the described first step is preferably N, dinethylformamide, N,N-dimethylacetamide, oxolane, carrene, dichloroethanes, chloroform, monochloro methane, acetone, formic acid, benzene, toluene, cyclohexane, the mixture of one or two or more kinds in hexafluoroisopropanol and trifluoro one alcohol.
Used voltage is the 15-30 kilovolt during electrostatic spinning in described second step, solution the speed on the spinning head of being input to be the 2-6 milliliter/hour.
Reception material in described second step is aluminium foil, copper mesh, fabric or nonwoven fabric, and spinning head and the vertical interval that receives between the material are 10-20 centimetre.
Basic principle of the present invention is to utilize the hydrophobic polymer of low-potential energy, prepare the superfine fibre that fibre diameter reaches in sub-micron by electrospinning process, utilize being separated that the small liquid stream of polymer produces in high-voltage electrostatic field high speed stretching flight course in the high volatile volatile of solvent and the electrostatic spinning process to form micro/nano level projection and fold simultaneously at fiber surface, simultaneously by in spinning solution, adding the nano SiO 2 particle of hydrophobic type, can increase the roughness of fiber surface greatly, the micro/nano level projection of fiber surface and pleated structure can coat a large amount of air like this, when water droplet contact fiber surface, the air that is coated and the polymeric fiber surface of low-potential energy make the contact angle of solid liquid interface (containing liquid) increase substantially, surpass 150 °, thereby reach super-hydrophobic effect.
The present invention compared with prior art, advantage is as follows:
(1) the super hydrophobic multi-stage nanometer structure fiber that makes of the present invention can improve the hydrophobic performance of tunica fibrosa greatly.With the polystyrene is example, add the inorganic particle electrostatic spinning again after, hydrophobic angle is brought up to 157.2 ° from 148.6 °, hydrophobic angular lag drops to 2.2 ° from 7.0 °.Because the reflection of hydrophobic angular lag is the dynamic hydrophobic performance on surface, and in practical application in that dynamically the field is more extensive, so the present invention has bigger meaning for the raising of hydrophobic performance.
(2) super hydrophobic multi-stage nanometer structure fiber preparation method of the present invention need not process FAS processing and promptly has the hydrophobic angle of superelevation, has removed the puzzlement of fluorine from, has advantages such as technology is simple, cheap, pollution-free.
The specific embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1
Under 25 ℃ of room temperatures, with 3g polystyrene (molecular weight 208kg/mol), 0.5g diameter be the hydrophobic silica nano particle of 2-40 nanometer with rotating speed 10rpm stirring and dissolving at 7gN, in the dinethylformamide solution, being stirred to solid all dissolves, solution is colourless transparent liquid, obtains the polystyrene solution that mass fraction is 30wt% (is 14.3wt% with respect to polystyrene nano SiO 2 particle content).
Under the condition of 25 ℃ of room temperatures, the polystyrene/silica dioxide solution that the disposed flow velocity with 6mL/h is input on the spinning head, simultaneously spinning head is connected 15 kilovolts HV generator, receive fiber with aluminium foil, the fiber receiving range is 10cm, promptly obtain novel super hydrophobic multi-stage nanometer structure fiber, its hydrophobic angle is 157.2 °.Under the similarity condition, do not add nano SiO 2 particle and obtain fiber, its hydrophobic angle is 146.5 °.
Embodiment 2
Under 25 ℃ of room temperatures, with 2g polymethyl methacrylate (molecular weight 110kg/mol), 0.5g diameter be the hydrophobic silica nano particle of 2-40 nanometer with rotating speed 100rpm stirring and dissolving at 8gN, in the dinethylformamide solution, being stirred to solid all dissolves, solution is colourless transparent liquid, obtains the polymethyl methacrylate solution (is 20wt% with respect to polymethyl methacrylate nano SiO 2 particle content) of mass fraction 20%.
Under the condition of 25 ℃ of room temperatures, the polymethyl methacrylate/silicon dioxide solution the prepared flow velocity with 3mL/h is input on the spinning head, simultaneously spinning head is connected 30 kilovolts HV generator, receive fiber with copper mesh, the fiber receiving range is 20cm, promptly obtain novel super hydrophobic multi-stage nanometer structure fiber, its hydrophobic angle is 153.2 °.Under the similarity condition, do not add nano SiO 2 particle and obtain fiber, its hydrophobic angle is 135.5 °.
Embodiment 3
Under 25 ℃ of room temperatures, with 1g acetyl cellulose (molecular weight 40kg/mol), 0.05g diameter be the hydrophobic silica nano particle of 2-40 nanometer with rotating speed 200rpm stirring and dissolving at 9gN, in N-dimethylacetylamide/acetone (weight ratio 2/1) solution, being stirred to solid all dissolves, solution is colourless transparent liquid, obtains the cellulose acetate ester solution (being about 5wt% with respect to acetyl cellulose nano SiO 2 particle content) of mass fraction 10%.
Under the condition of 25 ℃ of room temperatures, acetyl cellulose/silicon dioxde solution of being prepared flow velocity with 2mL/h is input on the spinning head, simultaneously spinning head is connected 20 kilovolts HV generator, receive fiber (twining above the cylinder) with nonwoven fabric, the fiber receiving range is 15cm, promptly obtain novel hydrophobic multi-level nano-structure tunica fibrosa, its hydrophobic angle is 140.2 °.Under the similarity condition, do not add nano SiO 2 particle and obtain fiber, its hydrophobic angle is 125.5 °.
Embodiment 4
Under 25 ℃ of room temperatures, with 1.5g Merlon (molecular weight 1100kg/mol), 0.3g diameter be the hydrophobic silica nano particle of 2-40 nanometer with rotating speed 50rpm stirring and dissolving in 8.5g carrene/chloroform (weight ratio 3/1) solution, being stirred to solid all dissolves, solution is colourless transparent liquid, obtains the polycarbonate solution (being about 16.6wt% with respect to Merlon nano SiO 2 particle content) of mass fraction 15%.
Under the condition of 25 ℃ of room temperatures, Merlon/silicon dioxde solution of being prepared flow velocity with 2mL/h is input on the spinning head, simultaneously spinning head is connected 25 kilovolts HV generator, receive fiber with nonwoven fabric, the fiber receiving range is 10cm, promptly obtain novel super hydrophobic multi-stage nanometer structure tunica fibrosa, its hydrophobic angle is 156.7 °.Under the similarity condition, do not add nano SiO 2 particle and obtain fiber, its hydrophobic angle is 145.5 °.
Embodiment 5
Under 25 ℃ of room temperatures, with 1.5g polyvinyl chloride (molecular weight 110kg/mol), 0.3g diameter be the hydrophobic silica nano particle of 2-40 nanometer with rotating speed 50rpm stirring and dissolving at 8.5gN, in the dinethylformamide solution, being stirred to solid all dissolves, solution is colourless transparent liquid, obtains the polyvinyl chloride solution (being about 16.7wt% with respect to polyvinyl chloride nano SiO 2 particle content) of mass fraction 15%.
Under the condition of 25 ℃ of room temperatures, Merlon/silicon dioxde solution of being prepared flow velocity with 2mL/h is input on the spinning head, simultaneously spinning head is connected 25 kilovolts HV generator, receive fiber with aluminium foil, the fiber receiving range is 10cm, promptly obtain novel super hydrophobic multi-stage nanometer structure tunica fibrosa, its hydrophobic angle is 155.8 °.Under the similarity condition, do not add nano SiO 2 particle and obtain fiber, its hydrophobic angle is 145 °.
Embodiment 6
Under 25 ℃ of room temperatures, with 0.5g PLA (molecular weight 350kg/mol), 0.05g diameter be the hydrophobic silica nano particle of 2-40 nanometer with rotating speed 100rpm stirring and dissolving in 9.5g carrene/chloroform (weight ratio 3/1) solution, being stirred to solid all dissolves, solution is colourless transparent liquid, obtains the PLA (being about 9wt% with respect to PLA nano SiO 2 particle content) of mass fraction 10%.
Under the condition of 25 ℃ of room temperatures, PLA/silicon dioxde solution of being prepared flow velocity with 2mL/h is input on the spinning head, simultaneously spinning head is connected 25 kilovolts HV generator, receive fiber with copper mesh, the fiber receiving range is 18cm, promptly obtain novel super hydrophobic multi-stage nanometer structure tunica fibrosa, its hydrophobic angle is 166.7 °.Under the similarity condition, do not add nano SiO 2 particle and obtain fiber, its hydrophobic angle is 151.5 °.
At the solution process for preparation, the difference of nano SiO 2 particle addition and electrospinning parameter difference, with respect to pure-spinning fibre, all there is raising in various degree at the hydrophobic angle of mixing fiber that is obtained.
Claims (7)
1. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure is characterized in that, concrete steps are:
The first step: at room temperature, hydrophobic polymer and hydrophobicity inorganic nanoparticles are joined in the airtight vessel that fill solvent, be placed on the magnetic stirring apparatus,, obtain the solution of character homogeneous with the rotating speed stirring of 10-200rpm;
Second step: at room temperature, the solution that the first step is obtained is input on the spinning head with constant flow velocity, simultaneously spinning head is connected HV generator and carry out electrostatic spinning, spun fiber receives with receiving system, obtains having the tunica fibrosa of super hydrophobic multi-stage nanometer structure.
2. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure as claimed in claim 1, it is characterized in that, hydrophobic polymer in the described first step is a polystyrene, polymethyl methacrylate, acetyl cellulose, Merlon, polyvinyl acetate, PLA, polyvinyl chloride, polyacrylonitrile, polycaprolactone, poly butylene succinate, poly-succinic acid-butanediol-altogether-and the mutual-phenenyl two acid bromide two alcohol ester, poly-hydroxyl valerate, polyethylene terephthalate, polyamide, PEI, polyformaldehyde or ethyl cellulose.
3. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure as claimed in claim 1, it is characterized in that, hydrophobicity inorganic nanoparticles in the described first step is the hydrophobic silica nano particle, and diameter is the 2-40 nanometer, and addition is the 5-20wt% of hydrophobic polymer fiber.
4. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure as claimed in claim 1 is characterized in that, the solvent in the described first step is N, dinethylformamide, N,N-dimethylacetamide, oxolane, carrene, dichloroethanes, chloroform, monochloro methane, acetone, formic acid, benzene, toluene, cyclohexane, the mixture of one or two or more kinds in hexafluoroisopropanol and trifluoro one alcohol.
5. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure as claimed in claim 1 is characterized in that, used voltage is the 15-30 kilovolt during electrostatic spinning in described second step, solution the speed on the spinning head of being input to be the 2-6 milliliter/hour.
6. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure as claimed in claim 1 is characterized in that, the reception material in described second step is aluminium foil, copper mesh, fabric or nonwoven fabric.
7. the preparation method with tunica fibrosa of super hydrophobic multi-stage nanometer structure as claimed in claim 1 is characterized in that, spinning head in described second step and the vertical interval that receives between the material are 10-20 centimetre.
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