CN101301592A - Preparation of polyimides/titanic oxide compound sub-micron fiber film - Google Patents
Preparation of polyimides/titanic oxide compound sub-micron fiber film Download PDFInfo
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- CN101301592A CN101301592A CNA2008100591398A CN200810059139A CN101301592A CN 101301592 A CN101301592 A CN 101301592A CN A2008100591398 A CNA2008100591398 A CN A2008100591398A CN 200810059139 A CN200810059139 A CN 200810059139A CN 101301592 A CN101301592 A CN 101301592A
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 26
- 239000000835 fiber Substances 0.000 title claims abstract description 25
- -1 titanic oxide compound Chemical class 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000004642 Polyimide Substances 0.000 title abstract description 15
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims description 28
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 24
- 239000002243 precursor Substances 0.000 claims description 12
- 229920005575 poly(amic acid) Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 13
- 239000004408 titanium dioxide Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- 239000002121 nanofiber Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 230000007547 defect Effects 0.000 abstract 1
- 230000009970 fire resistant effect Effects 0.000 abstract 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 28
- 229940043267 rhodamine b Drugs 0.000 description 28
- 230000015556 catabolic process Effects 0.000 description 20
- 238000006731 degradation reaction Methods 0.000 description 20
- 239000010408 film Substances 0.000 description 13
- 239000002131 composite material Substances 0.000 description 12
- 238000009413 insulation Methods 0.000 description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 12
- 229910010413 TiO 2 Inorganic materials 0.000 description 10
- 239000012528 membrane Substances 0.000 description 8
- 239000010936 titanium Substances 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000012456 homogeneous solution Substances 0.000 description 4
- CGJMROBVSBIBKP-UHFFFAOYSA-N malonamic acid Chemical compound NC(=O)CC(O)=O CGJMROBVSBIBKP-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000001523 electrospinning Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000001891 gel spinning Methods 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 125000000879 imine group Chemical group 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The present invention discloses a production method of polyimide/titanium dioxide compound submicron fiber film, which combines colloidal sol gel and electrostatic spinning. The polyimide/titanium dioxide compound submicron fiber film obtained by electrostatic spinning method of the invention has larger specific surface area and high photocatalysis activity. The polyimide/titanium dioxide compound submicron fiber film contains fire-resistant polyimide with strong plasticity, consequently overcomes the defects of high brittleness and friability of titanium dioxide nano fiber film. The present invention has simple industrial process, reliable quality and high repeatability. The polyimide/titanium dioxide compound submicron fiber film produced by the invention can be widely used in the field of photocatalysis and filtration.
Description
Technical field
The present invention relates to a kind of preparation method of polyimide film.
Background technology
Composite not only can improve the various aspects of performance of material as a kind of new material, can also give polymer composites new function, makes new material have more wide application space.
Polyimides is the high polymer that contains imine group, is widely used in fields such as Aeronautics and Astronautics, nuclear power and microelectronics owing to having superior hot property, electrical property and mechanical performance; Having preferably, radiation resistance and electrical insulation capability make polyimide fiber have the advantage bigger than other polymer fiber in high temperature, radioactive environment.
Titanium dioxide is the inanimate matter photochemical catalyst that application potential is arranged up to now most, sub-micron titanium dioxide has special skin effect, small-size effect and Kubo effect etc. because of it, organic pollution, degerming, the degraded water surface petroleum pollution of the processing, degraded that can effectively be applied to organic pollution in the liquid phase in the atmosphere, removes nitrogen oxide and deodorizing etc. in the air.The research of sub-micron photocatalysis titanium dioxide has become a focus of nano material exploitation.At present, main preparation methods has chemical precipitation method, sol-gel method, microemulsion, gas-phase reaction method etc.Utilize sol-gel technology as Gao Jiwei etc., adopt butyl titanate-absolute ethyl alcohol-hydrochloric acid system material, prepare and have the good light catalytic performance and get the titanium oxide crystal sol; F.-D.Duminica etc. utilize the AP-MOCVD method,, deposit on stainless steel and silicon (110) substrate and have photocatalysis performance and hydrophilic TiO less than 420 ℃ in temperature
2Film (F.-D.Duminica, F.Maury and R.Hausbrand.Growth of TiO
2Thin films by AP-MOCVD on stainless steel substrates forphotocatalytic applications.Surface and Coatings Technology.Surf.Coat.Technol. (2007), doi:10.1016/j.surfcoat.2007.04.011).
Polyimides/TiO
2Composite nano materials preparation and research aspect have also obtained very big progress, adopt in-situ polymerization to prepare polyimides/nano titanium oxide (TiO if any the people
2) compound, studied its morphosis and the dispersiveness of nano particle in compound with TEM, FTIR, with infrared spectrum the existence of nano particle in the compound, machinery, the dielectric properties of the nano-complex of having analyzed and researched simultaneously.Nano particle is favorable dispersibility in compound; Nano-TiO
2Adding cause the conventional mechanical, dielectric properties of nano-complex to descend, but along with nano-TiO
2The increase of content, the anti-corona ability and the hot strength of composite are improved.(Fan Youbing, the synthetic and performance study of polyimides/nano titanium oxide compound. insulating materials 20O4No.3)
Before electrostatic spinning technique resulted from 60 years, early 1990s, the Reneker seminar of U.S. University of Akron had begun research again to this technology.Yet the exploitation along with nanofiber in nearly 10 years of a large amount of experimental works of electrostatic spinning and the deep theoretical research is grown up.Utilize electrostatic spinning technique to make polyimide, the photocatalysis performance that the former superior hot property, electrical property and mechanical performance and the latter are superior just can obtain comprehensive utilization.Yet, still have nothing to do at present and prepare the report of polyimide in electrospinning process.
Summary of the invention
The purpose of this invention is to provide a kind of polyimide (PI/TiO with highlight catalytic active
2) preparation method of compound submicron fiber film.
The preparation method of polyimide film provided by the invention, employing be the method that collosol and gel and electrostatic spinning combine, specifically may further comprise the steps:
1) butyl titanate is dissolved in the N-N dimethyl formamide, the mass ratio of butyl titanate and N-N dimethyl formamide is 3: 5~2: 1, and adds acetylacetone,2,4-pentanedione as dispersant, and magnetic agitation becomes uniform solution;
2) at N
2Under the gas shiled, the drips of solution that step 1) is made is added in the polyamic acid solution, stirs into mixed solution, and wherein butyl titanate mass percent scope is 5%-20%, obtains precursor solution;
3) utilize electrostatic spinning apparatus, precursor solution is made polyamic acid/butyl titanate compound submicron fiber film, heat-treat again after the drying, make its imidization, form the polyimide film.
Among the present invention, the parameter of electrostatic spinning apparatus can be selected: supply voltage 10-20KV, spinning head with receive substrate apart from 10-15cm, feeding speed 0.3-0.5ml/h.
By changing the mass percent of butyl titanate, can change PI/TiO in the preparation process
2The photocatalysis performance of compound submicron fiber film.
Beneficial effect of the present invention is:
1. the present invention utilizes method of electrostatic spinning to prepare PI/TiO
2Compound submicron fiber film obtains the electrospinning filament diameter at 300~600nm.Because the tunica fibrosa specific area that the electrospinning silk forms is bigger, thereby can improve its photocatalytic activity greatly.
2. the PI/TiO that makes of the present invention
2Compound submicron fiber film, to have plasticity strong owing to combine, and the polyimides of advantage such as high temperature resistant, and this has just overcome pure titinium dioxide nanofiber fragility height, the defective of easy fracture.
3. technical process of the present invention is simple, and reliable in quality is repeatable high.The PI/TiO that makes
2Compound submicron fiber film can be widely used in photocatalysis and filtration art, has good market prospects.
Description of drawings
Fig. 1 is PI/TiO
2The compound submicron fiber sem photograph;
Fig. 2 is PI/TiO
2Compound submicron fiber photocatalysis design sketch.
The specific embodiment
The present invention is further described according to example below:
Example 1
1) with 0.3g tetrabutyl titanate Ti (OC
4H
9)
4(analyzing pure) stirred down and splashed into 0.5g N-N dimethyl formamide, magnetic agitation 2h, and adding 0.2g acetylacetone,2,4-pentanedione does dispersant, makes it to be mixed into homogeneous solution;
2) at N
2Under the gas shiled, the uniform solution that step 1) is made is added drop-wise in the 5g malonamic acid solution, continues to stir 24h, obtains evenly, has the precursor solution (PAA-Ti (OC of certain viscosity
4H
9)
4);
3) above-mentioned precursor solution is packed in the plastic injector of electrostatic spinning apparatus, it is as follows to adjust the electrostatic spinning parameter: supply voltage 20KV, receive between substrate and the spinning head apart from 12cm, feeding speed 0.4ml/h obtains polyamic acid/butyl titanate compound submicron fiber film;
4) composite cellulosic membrane that will prepare by method of electrostatic spinning is after 80 ℃ of dryings, again this composite membrane is heat-treated: 140 ℃ of insulation 1h, 200 ℃ of insulation 1h, 280 ℃ of insulation 1h, make its imidization, form polyimide film (see figure 1).
PI-TiO
2The photocatalysis performance detection method of sub-micron fibers is as follows: with PI/TiO
2Submicron fiber film is put into rhodamine B solution, carries out photocatalytic degradation under uviol lamp, and utilizes ultraviolet-visual spectrometer to measure in the solution organic matter solubility over time, assessment PI/TiO
2The photocatalysis performance of submicron fiber film.The original solubility of rhodamine B is 20mg/L, tunica fibrosa macroscopic view area 20cm
2Behind the 60min, the degradation rate of rhodamine B is 53.6% under uviol lamp; Behind the 90min, the degradation rate of rhodamine B is 72%; Behind the 120min, the degradation rate of rhodamine B is 73.8%; Behind the 150min, the degradation rate of rhodamine B is 90.2%; Behind the 180min, the degradation rate of rhodamine B is 93.2%, (see figure 2).
Example 2
1) with 0.5g tetrabutyl titanate Ti (OC
4H
9)
4(analyzing pure) splashes into 0.5g N-N dimethyl formamide, magnetic agitation 2h under stirring.And add the 0.2g acetylacetone,2,4-pentanedione and do dispersant, make it to be mixed into homogeneous solution;
2) at N
2Under the gas shiled, the uniform solution that step 1) is made is added drop-wise in the 5g malonamic acid solution, continues to stir 24h, obtains evenly, has the precursor solution (PAA-Ti (OC of certain viscosity
4H
9)
4);
3) above-mentioned precursor solution is packed in the plastic injector of electrostatic spinning apparatus, it is as follows to adjust the electrostatic spinning parameter: supply voltage 15KV, receive between substrate and the spinning head apart from 10cm, feeding speed 0.3ml/h obtains polyamic acid/butyl titanate compound submicron fiber film;
4) composite cellulosic membrane that will prepare by method of electrostatic spinning is after 80 ℃ of dryings, again this composite membrane is heat-treated: 140 ℃ of insulation 1h, 200 ℃ of insulation 1h, 280 ℃ of insulation 1h, make its imidization, form the polyimide film.
Utilize the PI/TiO of rhodamine B check preparation
2The photocatalysis performance of sub-micron fibers, the original solubility of rhodamine B is 20mg/L, tunica fibrosa macroscopic view area 20cm
2Behind the 60min, the degradation rate of rhodamine B is 55.7% under uviol lamp; Behind the 90min, the degradation rate of rhodamine B is 76.2%; Behind the 120min, the degradation rate of rhodamine B is 77.2%; Behind the 150min, the degradation rate of rhodamine B is 92.6%; Behind the 180min, the degradation rate of rhodamine B is 94.7%, (see figure 2).
Example 3
1) with 0.75g tetrabutyl titanate Ti (OC
4H
9)
4(analyzing pure) stirred down and splashed into 0.5g N-N dimethyl formamide, magnetic agitation 2h, and adding 0.2g acetylacetone,2,4-pentanedione does dispersant, makes it to be mixed into homogeneous solution;
2) at N
2Under the gas shiled, the uniform solution that step 1) is made is added drop-wise in the 5g malonamic acid solution, continues to stir 24h, obtains evenly, has the precursor solution (PAA-Ti (OC of certain viscosity
4H
9)
4);
3) above-mentioned precursor solution is packed in the plastic injector of electrostatic spinning apparatus, it is as follows to adjust the electrostatic spinning parameter: supply voltage 10KV, receive between substrate and the spinning head apart from 15cm, feeding speed 0.5ml/h obtains polyamic acid/butyl titanate compound submicron fiber film;
4) composite cellulosic membrane that will prepare by method of electrostatic spinning is heat-treated this composite membrane after 80 ℃ of dryings again: 140 ℃ of insulation 1h, and 200 ℃ of insulation 1h, 280 ℃ of insulation 1h make its imidization.Form the polyimide film.
Utilize the PI/TiO of rhodamine B check preparation
2The photocatalysis performance of sub-micron fibers, the original solubility of rhodamine B is 20mg/L, is used for the tunica fibrosa macroscopic view area 20cm of catalysis experiment
2Behind the 30min, the degradation rate of rhodamine B is 3.6% under uviol lamp; Behind the 60min, the degradation rate of rhodamine B is 37.8%; Behind the 90min, the degradation rate of rhodamine B is 75.6%; Behind the 120min, the degradation rate of rhodamine B is 94.9%; Behind the 180min, the degradation rate of rhodamine B is 96.3%, (see figure 2).
Example 4
1) with 1g tetrabutyl titanate Ti (OC
4H
9)
4(analyzing pure) splashes into 0.5g N-N dimethyl formamide, magnetic agitation 2h under stirring.And add the 0.2g acetylacetone,2,4-pentanedione and do dispersant, make it to be mixed into homogeneous solution;
2) at N
2Under the gas shiled, the uniform solution that step 1) is made is added drop-wise in the 0.3g malonamic acid solution, continues to stir 24h, obtains evenly, has the precursor solution (PAA-Ti (OC of certain viscosity
4H
9)
4);
3) above-mentioned precursor solution is packed in the plastic injector of electrostatic spinning apparatus, it is as follows to adjust the electrostatic spinning parameter: supply voltage 20KV, receive between substrate and the spinning head apart from 15cm, feeding speed 0.4ml/h obtains polyamic acid/butyl titanate compound submicron fiber film;
4) composite cellulosic membrane that will prepare by method of electrostatic spinning is heat-treated this composite membrane after 80 ℃ of dryings again: 140 ℃ of insulation 1h, and 200 ℃ of insulation 1h, 280 ℃ of insulation 1h make its imidization.Form the polyimide film.
Utilize the PI/TiO of rhodamine B check preparation
2The photocatalysis performance of sub-micron fibers, the original solubility of rhodamine B is 20mg/L, consumption 7ml is used for the tunica fibrosa macroscopic view area 20cm of catalysis experiment
2Behind the 30min, the degradation rate of rhodamine B is 59% under uviol lamp; Behind the 60min, the degradation rate of rhodamine B is 81%; Behind the 90min, the degradation rate of rhodamine B is 89%; Behind the 120min, the degradation rate of rhodamine B is 96.3%; Behind the 180min, the degradation rate of rhodamine B is 97.4%, (see figure 2).
Claims (2)
1. the preparation method of a polyimide film may further comprise the steps:
1) butyl titanate is dissolved in the N-N dimethyl formamide, the mass ratio of butyl titanate and N-N dimethyl formamide is 3: 5~2: 1, and adds acetylacetone,2,4-pentanedione as dispersant, and magnetic agitation becomes uniform solution;
2) at N
2Under the gas shiled, the drips of solution that step 1) is made is added in the polyamic acid solution, stirs into mixed solution, and wherein butyl titanate mass percent scope is 5%-20%, obtains precursor solution;
3) utilize electrostatic spinning apparatus, precursor solution is made polyamic acid/butyl titanate compound submicron fiber film, heat-treat again after the drying, make its imidization, form the polyimide film.
2. the preparation method of polyimide film according to claim 1 is characterized in that the supply voltage 10-20KV of electrostatic spinning apparatus, spinning head with receive substrate apart from 10-15cm, feeding speed 0.3-0.5ml/h.
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