CN104264368B - A kind of preparation method of the spontaneous type microorganism attachment fiber that is separated - Google Patents
A kind of preparation method of the spontaneous type microorganism attachment fiber that is separated Download PDFInfo
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- CN104264368B CN104264368B CN201410486623.4A CN201410486623A CN104264368B CN 104264368 B CN104264368 B CN 104264368B CN 201410486623 A CN201410486623 A CN 201410486623A CN 104264368 B CN104264368 B CN 104264368B
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- 244000005700 microbiome Species 0.000 title claims abstract description 24
- 239000000835 fiber Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000002269 spontaneous effect Effects 0.000 title claims abstract description 15
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 32
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 27
- 229920000889 poly(m-phenylene isophthalamide) Polymers 0.000 claims abstract description 19
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 13
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 12
- 239000004760 aramid Substances 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 11
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 10
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000006166 lysate Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 6
- 230000002209 hydrophobic effect Effects 0.000 abstract description 4
- 239000002121 nanofiber Substances 0.000 abstract description 4
- 239000013067 intermediate product Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Classifications
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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
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Materials For Medical Uses (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The present invention relates to spining technology field, the preparation method of especially a kind of spontaneous type microorganism attachment fiber that is separated, the fiber prepared by this method has dynamic, pliable and tough feature, can repeatedly recycle, and this product preparation process is simple and environmentally-friendly, manufacturing cycle is short, it is simple to industrialization promotion.The technical scheme is that to first pass through and hydroxyapatite particle is dispersed in meta-aramid (PMIA) solution, and by obtaining nanofiber intermediate product after method of electrostatic spinning blending；Then being selected mutually by parent/hydrophobic material spontaneity further and be separated and solidify operation, being formed with PMIA for core, hydroxyapatite particle is the microorganism attachment fiber of shell.
Description
Technical field
The present invention relates to is the preparation method of a kind of microorganism attachment fiber, and the preparation method of especially a kind of spontaneous type microorganism attachment fiber that is separated belongs to spining technology field.
Background technology
Hydroxyapatite is to constitute skeleton, the main material of tooth, safety non-toxic, has excellent biocompatibility, and microorganism is very easily attached to the surface of hydroxyapatite.This microorganism attachment material can, as purification of water quality use, be one of a kind of effective environment-friendly materials.Owing to hydroxyapatite is usually pulverulence, cannot reclaiming after being dispersed in water, applying so needing to be carried on carrier.But the load technology of hydroxyapatite encounters bottleneck for many years: a load can cause that on surface bond strength is not enough, it is easy to comes off；The method being blended in carrier inside then can cause that most of hydroxyapatite is greatly lowered the overall microorganism adhesion property of material owing to can not be exposed to surface.
Summary of the invention
It is an object of the invention to the deficiency overcoming prior art to exist, and the preparation method that a kind of spontaneous type microorganism attachment fiber that is separated is provided, adopt and prepare nanofiber as carrier with meta-aramid material using method of electrostatic spinning, selected mutually by spontaneity to realize surface high density load hydroxyapatite particle with phase separation principle, thus forming dynamically pliable and tough microorganism attachment fiber, reach to improve the purpose of overall microorganism adhesion property.
The present invention first passes through and is dispersed in meta-aramid (PMIA) solution by hydroxyapatite particle, and by obtaining nanofiber intermediate product after method of electrostatic spinning blending.Then being selected mutually by parent/hydrophobic material spontaneity further and be separated and solidify operation, being formed with PMIA for core, hydroxyapatite particle is the microorganism attachment fiber of shell.
It is an object of the invention to complete by following technical solution, described preparation method comprises the steps:
1) by mass fraction, 1-3 part lithium chloride (LiCl) powder is dissolved in 10 parts of N,N-dimethylacetamide (DMAC), makes lysate；
2) by mass fraction, 1-3 part meta-aramid (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 90 DEG C of-120 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 1-2 part, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.25-1 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.25-1.0ml/h, and receiving range is 10-20cm, and spinning voltage is 15-20kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 6-12 hour, dry and namely obtain end product in 8-12 hour after taking-up at 60-90 DEG C.
Currently preferred technical scheme is:
1) by mass fraction, 2 parts of lithium chloride (LiCl) powder are dissolved in 10 parts of N,N-dimethylacetamide (DMAC), make lysate；
2) by mass fraction, 2 parts of meta-aramids (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 100 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 2 parts, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.6 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.5ml/h, and receiving range is 15cm, and spinning voltage is 15kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 10 hours, dry and namely obtain end product in 10 hours after taking-up at 80 DEG C.
PMIA is high hydrophobic material, is at high temperature dissolved by DMAC/LiCl.Hydroxyapatite particle is water wetted material, for making it add a small amount of ethanol dispersed needs of PMIA solution system.In electrostatic spinning process, ethanol quickly volatilizees and makes parent/hydrophobic material spontaneity select mutually and be separated, so that PMIA is inwardly formed fiber and is extruded by hydrophilic hydroxy group hydroxyapatite particles, hydrophilic hydroxy group hydroxyapatite particles high density is finally made to be distributed in hydrophobicity PMIA fiber surface.PMIA nanofiber can be made further to solidify so that hydroxyapatite particle is firmly fixed in PMIA surface with the form of inlaying by acetone solidification liquid.
Beneficial effects of the present invention:
1) contradiction between Hydroxyapatite-Supported and activity is solved.
2) this kind of microorganism attachment fiber has dynamic, pliable and tough feature, can repeatedly recycle.
3) this product preparation process is simple and environmentally-friendly, and manufacturing cycle is short, it is simple to industrialization promotion.
Accompanying drawing explanation
Fig. 1 is one of Electronic Speculum figure of the spontaneous type microorganism attachment fiber that is separated of the present invention.
Fig. 2 is the two of the Electronic Speculum figure of the spontaneous type microorganism attachment fiber that is separated of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail: the preparation method of the spontaneous type microorganism attachment fiber that is separated of the present invention, it comprises the steps:
1) by mass fraction, 1-3 part lithium chloride (LiCl) powder is dissolved in 10 parts of N,N-dimethylacetamide (DMAC), makes lysate；
2) by mass fraction, 1-3 part meta-aramid (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 90 DEG C of-120 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 1-2 part, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.25-1 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.25-1.0ml/h, and receiving range is 10-20cm, and spinning voltage is 15-20kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 6-12 hour, dry and namely obtain end product in 8-12 hour after taking-up at 60-90 DEG C.
As shown in Figure 1 and Figure 2 for the Electronic Speculum figure of the spontaneous type microorganism attachment fiber that is separated of the present invention.
Protection scope of the present invention is not limited to following embodiment, therefore, every technical scheme formed by simple numerical value replacement etc., all constitute specific embodiments of the invention, and form protection scope of the present invention.
Embodiment 1: the preparation method of the spontaneous type microorganism attachment fiber that is separated of the present invention, it comprises the steps:
1) by mass fraction, 1 part of lithium chloride (LiCl) powder is dissolved in 10 parts of N,N-dimethylacetamide (DMAC), makes lysate；
2) by mass fraction, 1 part of meta-aramid (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 90 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 1 part, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.25 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.25ml/h, and receiving range is 10cm, and spinning voltage is 15kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 6 hours, dry and namely obtain end product in 8 hours after taking-up at 60 DEG C.
Embodiment 2: the preparation method of the spontaneous type microorganism attachment fiber that is separated of the present invention, it comprises the steps:
1) by mass fraction, 2 parts of lithium chloride (LiCl) powder are dissolved in 10 parts of N,N-dimethylacetamide (DMAC), make lysate；
2) by mass fraction, 2 parts of meta-aramids (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 100 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 1.5 parts, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.5 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.5ml/h, and receiving range is 15cm, and spinning voltage is 18kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 8 hours, dry and namely obtain end product in 10 hours after taking-up at 70 DEG C.
Embodiment 3: the preparation method of the spontaneous type microorganism attachment fiber that is separated of the present invention, it comprises the steps:
1) by mass fraction, 3 parts of lithium chloride (LiCl) powder are dissolved in 10 parts of N,N-dimethylacetamide (DMAC), make lysate；
2) by mass fraction, 3 parts of meta-aramids (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 110 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 2 parts, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.75 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.75ml/h, and receiving range is 15cm, and spinning voltage is 20kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 10 hours, dry and namely obtain end product in 10 hours after taking-up at 80 DEG C.
Embodiment 4: the preparation method of the spontaneous type microorganism attachment fiber that is separated of the present invention, it comprises the steps:
1) by mass fraction, 3 parts of lithium chloride (LiCl) powder are dissolved in 10 parts of N,N-dimethylacetamide (DMAC), make lysate；
2) by mass fraction, 3 parts of meta-aramids (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 120 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 2 parts, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 1 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 1.0ml/h, and receiving range is 20cm, and spinning voltage is 20kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 12 hours, dry and namely obtain end product in 12 hours after taking-up at 90 DEG C.
Claims (2)
1. the preparation method of the spontaneous type microorganism attachment fiber that is separated, it is characterised in that described preparation method comprises the steps:
1) by mass fraction, 1-3 part lithium chloride (LiCl) powder is dissolved in 10 parts of N,N-dimethylacetamide (DMAC), makes lysate；
2) by mass fraction, 1-3 part meta-aramid (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 90 DEG C of-120 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 1-2 part, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.25-1 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.25-1.0ml/h, and receiving range is 10-20cm, and spinning voltage is 15-20kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 6-12 hour, dry and namely obtain end product in 8-12 hour after taking-up at 60-90 DEG C.
2. the preparation method of the spontaneous type microorganism attachment fiber that is separated according to claim 1, it is characterised in that in described step:
1) by mass fraction, 2 parts of lithium chloride (LiCl) powder are dissolved in 10 parts of N,N-dimethylacetamide (DMAC), make lysate；
2) by mass fraction, 2 parts of meta-aramids (PMIA) being joined 10 parts of above-mentioned steps 1) in the solution of gained, under 100 DEG C of conditions, agitating heating is configured to mixed solution in 3 hours；
3) when stirring at normal temperature, by mass fraction 10 parts of above-mentioned steps 2) mixed solution of gained is initially charged the hydroxyapatite particle of 2 parts, it is configured to hydroxyapatite particle dispersion；Then it is added dropwise over the ethanol of 0.6 part again, obtains blend spinning liquid；
4) by above-mentioned steps 3) the blend spinning liquid of gained carries out electrostatic spinning, and fltting speed is 0.5ml/h, and receiving range is 15cm, and spinning voltage is 15kv, namely obtains uniform spinning film after spinning；
5) by above-mentioned steps 4) the spinning film of gained is soaked in acetone soln and stands 10 hours, dry and namely obtain end product in 10 hours after taking-up at 80 DEG C.
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| CN1751745A (en) * | 2005-08-02 | 2006-03-29 | 天津大学 | Apatite super-fine fiber material and its prepn. method |
| JP2008002011A (en) * | 2006-06-22 | 2008-01-10 | Toyobo Co Ltd | Polyimide nonwoven fabric and method for producing the same |
| US7879093B2 (en) * | 2007-03-26 | 2011-02-01 | University Of Connecticut | Electrospun apatite/polymer nano-composite scaffolds |
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