CN1245547C - Method for modifying high-polymer fibre material surface - Google Patents
Method for modifying high-polymer fibre material surface Download PDFInfo
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- CN1245547C CN1245547C CN 200410041289 CN200410041289A CN1245547C CN 1245547 C CN1245547 C CN 1245547C CN 200410041289 CN200410041289 CN 200410041289 CN 200410041289 A CN200410041289 A CN 200410041289A CN 1245547 C CN1245547 C CN 1245547C
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- fiber material
- polymer fiber
- shitosan
- material surface
- ultraviolet ray
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Abstract
The present invention relates to a method for the surface modification of high molecular fibre material without the need of water (as the medium), chemicals and steam. The method which omits the process of baking and the treatment of waste water has the advantages of low investment cost of apparatus, high operability, energy saving, high efficiency, no pollution, durability and resource saving, and is beneficial for environmental protection. The method comprises the modification steps as follows: a) attachments on the surface of fabrics are removed with conventional refinement methods; b) high molecular fibre material is put into gas containing oxygen and irradiated by ultraviolet rays for 5 to 30 minutes; c) the high molecular fibre material is impregnated in chitosan solution for 5 to 15 minutes, wherein the deacetylation degree of the chitosan solution is more than 80%, and the concentration is from 0.3 to 0.7VOL%; d) the solution is rolled with a roller after chitosan is attached to the surface of the high molecular fibre material so as to achieve 40 to 70% of the mangle expression; e) the solution is dried by hot air of 50 to 110 DEG C so as to combine the chitosan onto the surface of the high molecular fibre material.
Description
Technical field
The present invention is a kind of method to the polymer fiber material surface modification, the ultraviolet irradiation technique of especially a kind of usefulness carries out modification to the polymer fiber material table method.
Background technology
The modification technology on fibrous material surface mainly contains at present: methods such as alkali cleaning, strong oxidizer oxidation swelling, plasma.
Alkali cleaning is to be used for the surface-treated of polyester fiber typical case effective ways, industrial title alkali decrement method.The basic principle of alkali decrement method is a saponification, when saponification, and OH
-Cast the first stone-(C) (O)-be with δ among the O-R
+The C atom of electric charge forms addition product, ester linkage hydrolyzing fracture then, macromolecules degradation is the less molecule of molecular weight, and reaction goes on successively, leaves fiber until generating para-phthalic sodium and ethylene glycol, the weight of fabric is reduced,, claim the decrement method again so claim alkali decrement method.
The strong oxidizer oxidation be substantially since fiber under the effect of strong oxidizer, fiber surface is by the powerful oxidation agent oxidation ablation, make the cracking of polymer surfaces generation chain, crosslinked and oxidation make physical bond and chemical bond between fiber and other material make a concerted effort to strengthen, improve fiber surface activation energy and wettability, thereby improved the performance of fiber.The method of strong oxidizer oxidation has pickling, ozone oxidation and hydrogen peroxide swelling etc.
Alkali cleaning, strong oxidizer oxidation swelling etc. all are by the access of chemical treatment to the etching of fiber surface, chain cracking, group, improve polymer fiber material surface active energy and wettability, but it is difficult to the modification degree easy damaged fiber macromolecular chain inside of controlling fiber, influence fibre strength and quality, water consumption is big and the pollution problem of environment has been caused people's attention.
Plasma surface modification is to study more modification technology recently, plasma has three kinds: hot plasma, cold plasma, hybrid plasma, low temperature plasma commonly, low temperature plasma is to have high-octane ion and a molecule by what glow discharge produced under vacuum, and electron temperature reaches degree up to ten thousand (K), can cause generation high polymer free radical with the Cement Composite Treated by Plasma fiber, cracking takes place, introduce functional group, grafting, and can make the fiber surface etching.The plasma modification of fiber also is a kind of complete dry gas-solid phase dry modification processing mode, and it can avoid the pollution of waste liquid, and reaction only relates to the superficial layer of fiber, can not change the overall performance of fiber self and gives fiber new surface physical property.But in plasma modification, require to carry out under vacuum condition, that equipment requires is high, cost an arm and a leg, not too suitability for industrialized production, and exists the fiber surface modification degree is difficult to control problem.
Summary of the invention
Technical problem: the purpose of this invention is to provide the method for the ultraviolet irradiation technique of a kind of usefulness to macromolecular fibre material surface modification, this method of modifying need not water as medium, need not chemicals, steam, drying course, wastewater treatment have been saved, its equipment investment expense is low, workable, have energy-conservation, efficient, pollution-free, durability, saving resource, help environmental protection.
Technical scheme: in view of the above-mentioned problems, the present invention has developed ultraviolet irradiation technique the polymer fiber material table has been carried out method of modifying.Ultraviolet ray is the electromagnetic wave shorter than visible wavelength, and its energy is difference according to the length of its wavelength and to some extent, and the binding energy of its energy size and most organic-matter chemicals belong to same category basically.Ultraviolet ray irradiation polymer fiber material, when energy surpasses the polymer chemistry binding energy, strand produces cracking, under the atmospheric conditions of aerobic, oxygen molecule ozonize in the atmosphere, active oxygen, polymer fiber material is oxidized, and the polymer fiber material surface generates carboxyl, aldehyde radical, hydroxyl, carbonyl etc.Polymer fiber material after the UV treatment can be introduced abundant polar group, as-OH ,-NH
2Deng, thereby hydrophily, hygroscopicity, the antistatic behaviour of raising polymer fiber material.Introducing disappears smelly, antibacterial material can make polymer fiber material have smelly, the antibiotic property that disappears.
The step of the polymer fiber material surface nature being carried out modification with ultraviolet irradiation technique is:
A, remove the attachment of fabric face with the common method of baptizing,
B, polymer fiber material is placed in the oxygen containing gas, through the ultraviolet ray irradiation of wavelength in 180～330nm scope 5～30 minutes,
C, polymer fiber material be impregnated in 0.3～0.7VOL% chitosan solution of degree of deacetylation more than 80% 5～15 fens kinds in (20～50 ℃),
D, behind polymer fiber material surface attachment shitosan, use the roll mangle again, making pick-up rate is 40～70%,
E, make it dry, make the polymer fiber material surface in conjunction with shitosan with 50～110 ℃ hot blasts.
Through the polymer fiber material that shines with ultraviolet ray with method of the present invention, improved the character (antistatic behaviour, wettability, dyeability, sorptive, antibiotic property, fungus resistance) on polymer fiber material surface.Because shitosan is the form combination with ionic bond at least on the polymer fiber material surface, the character on the surface that is enhanced has good durability.Especially to the durability of hot water than without the ultraviolet ray irradiation, only flood high tens of times of the method for chitosan solution.Can bring into play the distinctive physical chemistry rerum natura of shitosan for a long time.
The ultraviolet ray irradiation can in the air of normal temperature, carry out, also can other at ozone, oxygen, carbon dioxide carries out in all gases of nitrogen etc.Regardless of which kind of gas, the existence of oxygen is essential in the gas of ultraviolet ray irradiation.The amount that contains oxygen in the gas is at least more than 10%, and is better more than 20%.Do not reach that irradiation ultraviolet radiation can not fine activation synthetic high polymer surface in the gas of 10% oxygen.Can the air of normal temperature, shine from economy and security consideration.Improve oxygen concentration cost of equipment will be increased, along with operation under the condition that is close in 100% oxygen also can produce safety issue.
When having oxygen in the air, with have than oxygen molecule (O=O) (490.4KJ/mol) ultraviolet ray that binding energy is big irradiation can shine, the oxygen molecule some becomes active oxygen (oxygen atom), undecomposed oxygen molecule combines ozonize in the part of this active oxygen and the air, oxidation synthetic high polymer surface, remaining active oxygen combines (oxidation) with the molecule of the synthetic high polymer surface molecular chain cracking that is caused by the ultraviolet ray irradiation, like this, the synthetic high polymer surface is activated, on the polymer fiber material surface, (1) produce all functional group or bioactive molecule, (2) are etched out slight concavo-convex.Only be that active oxygen also can obtain this effect, but, ozone is generated more effective.
Ultraviolet ray is the electromagnetic wave shorter than visible wavelength, its energy is difference according to the length of its wavelength and to some extent, the binding energy of its energy size and most organic-matter chemicals belongs to same category basically, ultraviolet ray irradiation polymer fiber material, when energy surpasses the polymer chemistry binding energy, strand produces cracking, under the atmospheric conditions of aerobic, oxygen molecule ozonize in the atmosphere, active oxygen, polymer fiber material is oxidized, and the polymer fiber material surface generates carboxyl, aldehyde radical, hydroxyl, carbonyl etc.Polymer fiber material after the UV treatment can be introduced abundant polar group, as-OH ,-NH
2Deng, thereby hydrophily, hygroscopicity, the antistatic behaviour of raising polymer fiber material.Introducing disappears smelly, antibacterial material can make polymer fiber material have smelly, the antibiotic property that disappears.
Main chemical bond of table 1 and binding energy
| In conjunction with | In conjunction with (cracking) energy (KJ/mol) | In conjunction with | In conjunction with (cracking) energy (KJ/mol) |
| CH 3-H CH 3-CH 3 CH 3-C 2H 5 CH 2＝CH 2 CH 2≡CH 2 | 339 417 357 718 960 | CH 3-F CH 3-CI CH 3-Br Benzene-OH Benzene-CH 3 | 452 345 291 458 417 |
Ultraviolet wavelength can not make the material molecule chain produce cracking in the ultraviolet ray of 330nm～380nm scope, and the synthetic high polymer surface is activated, and it is slight concavo-convex to be etched out.Though wavelength is that vacuum ultraviolet can reach above-mentioned effect less than 180nm, practical operation is that difficulty is accomplished.The ultraviolet wavelength that the ultraviolet ray irradiation technique adopts is in 180～330nm scope.
This method wishes to use the ultraviolet ray that can make oxygen generate the following wavelength of 254nm of ozone.
The irradiation that ultraviolet ray is excessive can make the chemical constitution of polymer surface take place to change greatly, brings local interfacial failure, the original characteristic of damage macromolecule.Exposure is with 1～100J/cm in the method
2Do not damage the ultraviolet ray irradiation of polymer fiber material characteristic degree, with 2～20J/cm
2Preferable; Owing to be to use the luminous energy higher that the fiber surface strand is split than general molecule binding energy.So can not damage the original characteristic of polymer fiber material.
All functional groups that generate during the ultraviolet ray irradiation or bioactive molecule are unstable, but make it stable with the binding energy of chitosan molecule.Again, shitosan can play the effect of diaphragm to the position that the polymer fiber material surface interface that occurs with ultraviolet ray irradiation back is destroyed, and jog has physically been strengthened the adhesion strength of shitosan.Shitosan that should the surface after the ultraviolet ray irradiation is strong bonded fully, and its surface demonstrates the characteristic of shitosan simultaneously.
Use this method, the set form on shitosan and synthetic high polymer surface is a chemical bond, the amino-NH in the shitosan of its pull-out capacity and set
2Proportional.Therefore; the shitosan degree of deacetylation that uses in this method is high more good more; degree of deacetylation is at least more than 80%; the shitosan of degree of deacetylation nearly 100% also can use; but; shitosan to nearly 100% may not be good because price height and molecular weight are low, the most handy 85% degree of deacetylation chitosan solution.Concentration is at 0.3～0.75VOL%, the most handy 0.5VOL%
Make polymer fiber material adhere to shitosan and can adopt dipping, coating (containing spraying) such as pads at method.Make polymer fiber material adhere to chitosan solution, as far as possible will be simply, give uniformly, can easily remove solvent, dry (for example water).)
Shitosan mainly is to form chemical bond on the polymer fiber material surface in this method; But, not getting rid of shitosan exists and polymer fiber material surface physics ground adhesion part.
Beneficial effect: the reaction of UV treatment textiles is the direct effect between gas phase and the solid phase, need not water as medium, need not chemicals, steam, drying course, wastewater treatment have been saved, its equipment investment expense is low, workable, have energy-conservation, efficient, pollution-free, durability, saving resource, help advantages such as environmental protection, be better than other modification technology.Ultraviolet ray is to the technology of fibre modification, and is widely applicable, and it can be applied to polyenoid system, polyester system, all aromatic system, polyvinyl chloride, polyacrylonitrile based, fluorine-containing system, polyamide-based, polypropylene-based, polyethenol series, the surface modification of synthetic high polymer fibrous materials such as polyolefin, give its moisture absorption, antibiotic, smelly, antistatic, caking property disappear.Ultraviolet ray only occurs in its surface tens to thousands of dust thickness ranges to the effect of material.Therefore, can not influence the body phasic property of material, can keep the basic physical properties and the mechanical characteristic of material, on demand modification carried out on its surface.Because shitosan is the form combination with ionic bond at least on the polymer fiber material surface, the character on the surface that is enhanced has good durability.Especially to the durability of hot water than without the ultraviolet ray irradiation, only flood high tens of times of the method for chitosan solution.Can bring into play the distinctive physical chemistry rerum natura of shitosan for a long time.
The specific embodiment
Ultraviolet ray in this method takes place, available low-pressure mercury bright lamp, deuterium lamp, xenon lamp, the ultraviolet ray generating apparatus of laser etc.
(1), ultraviolet irradiation technique carries out modification to terylene plain knit fabric surface
1, removes attachment with the common method of baptizing by the woven plain knit fabric of polyester filament surface.Cooper-Hewitt lamp in the air of normal temperature, irradiation distance 40mm, 10 minutes (exposure 10.2J/cm
2) from three plain knit fabrics of plain knit fabric irradiation.
After the irradiation; textile impregnation is modulated to pH=3 to the shitosan of degree of deacetylation 85% at the acetic acid with 1%; concentration is 10 fens kinds in the chitosan aqueous solution (25 ℃) of 0.5vol.%; use the roll mangle again; making pick-up rate is after 40%; make it dry with 50 ℃ hot blasts, again with after 30 fens kinds of the boiling hot wash of acetic acid modulation pH=3, with 50 ℃ heated-air drying.So just obtain on the surface in conjunction with the terylene plain knit fabric A of shitosan.
2, remove attachment with the common method of baptizing by the woven plain knit fabric of polyester filament surface.Without the irradiation ultraviolet; the acetic acid that three plain knit fabrics are immersed in equally with 1% is modulated to pH=3 to the shitosan of degree of deacetylation 85%; concentration is 10 fens kinds in the chitosan aqueous solution (25 ℃) of 0.5vol.%; use the roll mangle again; making pick-up rate is after 40%; make it dry with 50 ℃ hot blasts, again with after 30 fens kinds of the boiling hot wash of acetic acid modulation pH=3, with 50 ℃ heated-air drying.So just obtain on the surface in conjunction with the terylene plain knit fabric B of shitosan.
Handle the character of back fabric in order to understand ultraviolet ray irradiation shitosan, do following several test.
1, the shitosan amount of fabric face combination
Gaining in weight divided by the original weight of fabric (dry weight) of fabric calculated the shitosan amount of the fabric face combination of several different time ultraviolet ray irradiations, as table 2.
Table 2: the shitosan amount of fabric face combination
| Fabric | Irradiation time (minute) | The shitosan amount % that increases on the fabric | Mean value | ||
| B | 0 | 0.004 | |||
| A | 10 | 0.083 | 0.085 | 0.078 | 0.082 |
As known from Table 2: the binding capacity with shitosan on the textiles of ultraviolet ray irradiation in 10 minutes is 0.082% (to fibre weight), is 0.004% (to fibre weight) without the binding capacity of shitosan on the textiles of ultraviolet ray irradiation
This explanation is only flooded shitosan without the ultraviolet ray irradiation, because shitosan only is physically to be combined in textile surface, just can remove substantially with hot wash.
2, wettability test
Respectively to handling textiles through 10 minutes shitosan of ultraviolet ray irradiation and handling textile surface with its solid-liquid contact angle of water gaging of 25 ℃ without the shitosan of ultraviolet ray irradiation, its regain of test under standard atmosphere condition, carry out the wettability experiment, result of the test such as table 3.
The comparison of fabric face wettability after table 3 hot wash
| Postradiation treatment conditions | Ultraviolet ray irradiation back is in conjunction with the fabric A of shitosan | Fabric B without the ultraviolet ray irradiation | ||
| Solid-liquid contact angle | Regain % | Solid-liquid contact angle | Regain % | |
| With hot wash after 30 minutes, heated-air drying | 46.3 degree | 1.15 | 79.0 degree | 0.41 |
| With hot wash after 60 minutes, heated-air drying | 46.4 degree | 1.11 | 83.5 degree | 0.38 |
As known from Table 3, handling the textiles solid-liquid contact angle through 10 minutes shitosan of ultraviolet irradiation time is 59% (46.3./79.0) of handling the textiles solid-liquid contact angle without the shitosan of ultraviolet ray irradiation, regain is 2.8 times (1.15/0.41), the wettability that explanation is handled textiles through 10 minutes shitosan of ultraviolet irradiation time is good, moistening easily.Through the boiling hot water cleaning 30 minutes of 10 minutes shitosan of ultraviolet irradiation time processing used for textiles acetic acid modulation pH to 3 and after with 60 minutes, use heated-air drying, its wetting quality does not almost change.The boiling hot water of handling used for textiles acetic acid modulation pH to 3 without the shitosan of ultraviolet ray irradiation cleaned 30 fens and with 60 minutes after, use heated-air drying, its wettability is worse.
3, antistatic test
Measure the antistatic property that shitosan is handled fabric sample with electrostatic pressure half-life method, test result sees 4.
Table 4: shitosan is handled electrostatic pressure, the half-life of textiles.
Shine 10 without the ultraviolet ray irradiation through ultraviolet ray
Shitosan is handled a fabric minute shitosan processing and is knitted
B thing A
Electrostatic pressure KV 5.7 3.8
Half-life S 15.6 1.8
Handle fabric through the shitosan of ultraviolet ray irradiation and modulate the boiling hot water cleaning of pH to 3 after 30 minutes, with 50 ℃ heated-air drying with acetic acid.Measuring its electrostatic pressure value according to electrostatic pressure half-life assay method is 3.8KV.
Handle fabric without the shitosan of ultraviolet ray irradiation and modulate the boiling hot water cleaning of pH to 3 after 30 minutes, with 50 ℃ heated-air drying with acetic acid.Measuring its electrostatic pressure value according to electrostatic pressure half-life assay method is 5.7KV.
The ratio of their electrostatic pressures is 3.8/5.7, the shitosan processing webbing piezoelectric voltage that obtained in 10 minutes through ultraviolet irradiation time only is to handle 67% of fabric without ultraviolet ray irradiation shitosan, employing this method is handled, and the fabric of shitosan combination has good antistatic behaviour.
4, shitosan is handled the durability of textiles,
Obtained the durability that shitosan is handled textiles in 10 minutes in order to understand the ultraviolet ray irradiation, measure the residual amount of back textiles of cleaning in conjunction with shitosan.Its result is as shown in table 5.Can know clearly from table 5: the shitosan of combination on the textiles of ultraviolet ray irradiation even wash 20 times, also has 0.067% shitosan (to fibre weight) stable bond on textiles.The fabric shell glycan of not handling through ultraviolet ray irradiation shitosan has not almost had, and as can be known, the ultraviolet ray irradiation obtained shitosan processing textiles in 10 minutes good durability.
The residual quantity of shitosan after table 5 fabric washing 20 times
| Fabric shell glycan residual quantity % (fabric weight relatively) | ||
| Through ultraviolet ray irradiation (fabric A) | Not through ultraviolet ray irradiation (fabric B) | |
| Boiling hot water without acetic acid modulation pH to 3 cleaned 30 minutes | 0.232 | 0.224 |
| Boiling hot water with acetic acid modulation pH to 3 cleaned 30 minutes | 0.082 | 0.004 |
| Boiling hot water with acetic acid modulation pH to 3 cleaned 30 minutes, washed 20 times (by the decantation test requirement) again | 0.067 | ＜0.004 |
The present invention can be applicable to polyenoid system to the method for polymer fiber material surface modification, polyester system, all aromatic system, polyvinyl chloride, polyacrylonitrile based, fluorine-containing system, polyamide-based, polypropylene-based, polyethenol series, the surface modification of synthetic high polymer fibrous materials such as polyolefin.
Claims (5)
1, a kind of method to the polymer fiber material surface modification is characterized in that with the method for ultraviolet ray irradiation the polymer fiber material surface nature being carried out modification, the steps include:
A, remove the attachment of fabric face with the common method of baptizing,
B, polymer fiber material is placed in the oxygen containing gas, through ultraviolet ray irradiation 5～30 minutes,
C, polymer fiber material be impregnated in degree of deacetylation more than 80%, concentration 5～15 fens kinds in the chitosan solution of 0.3～0.7VOL%,
D, behind polymer fiber material surface attachment shitosan, use the roll mangle again, making pick-up rate is 40～70%,
E, make it dry, make the polymer fiber material surface in conjunction with shitosan with 50～110 ℃ hot blasts.
2, a kind of method to the polymer fiber material surface modification according to claim 1 is characterized in that shining the ultraviolet wavelength of usefulness in 180～330nm scope.
3, a kind of method to the polymer fiber material surface modification according to claim 1, the ultraviolet irradiation amount that it is characterized in that shining usefulness is 1～100J/cm
2
4, a kind of method to the polymer fiber material surface modification according to claim 1 is characterized in that ultraviolet irradiation can also can carry out in all gases of other oxygen containing ozone, carbon dioxide, nitrogen in air.
5, according to claim 1 or 4 described a kind of methods, it is characterized in that containing in the oxygen containing gas amount of oxygen more than 10% to the polymer fiber material surface modification.
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| CN 200410041289 CN1245547C (en) | 2004-06-16 | 2004-06-16 | Method for modifying high-polymer fibre material surface |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102978898A (en) * | 2012-12-19 | 2013-03-20 | 上海汇泉实业有限公司 | Preparation method of antibacterial non-woven fabric |
| CN105498363B (en) * | 2015-12-22 | 2017-08-11 | 苏州协泰科技有限公司 | MODIFIED PP S fiber filter material production technologies |
| CN107869048B (en) * | 2017-11-09 | 2020-05-22 | 青岛哆瑭生物科技有限公司 | Functional polysaccharide antibacterial modified natural fiber and preparation method thereof |
| CN107964778A (en) * | 2017-11-27 | 2018-04-27 | 桐乡佳车科技有限公司 | A kind of cut pile fabric afterfinish method |
| CN110172818A (en) * | 2019-01-14 | 2019-08-27 | 自然资源部第三海洋研究所 | A kind of antibacterial surface method of modifying of non-woven cloth plasma graft shell oligosaccharide derivative |
| CN113333252A (en) * | 2021-05-08 | 2021-09-03 | 上海克络蒂材料科技发展有限公司 | Pretreatment process for spray painting of fiber reinforced resin section |
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