CN103981711A - Hydrophilic modification method of PVA to polyester fiber - Google Patents
Hydrophilic modification method of PVA to polyester fiber Download PDFInfo
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- CN103981711A CN103981711A CN201410165074.0A CN201410165074A CN103981711A CN 103981711 A CN103981711 A CN 103981711A CN 201410165074 A CN201410165074 A CN 201410165074A CN 103981711 A CN103981711 A CN 103981711A
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Abstract
The invention provides a hydrophilic modification method of PVA to polyester fiber, which belongs to the high-molecular technical field. The method comprises the following steps: pretreating the polyester fiber by a sodium hydroxide solution with 3-10% of mass fraction for 1 hour, wherein the solid liquid ratio is 1: 50, flushing and drying the polyester fiber, then placing the polyester fiber in a reaction container filled with a PVA solution with 0.2-0.3% of mass fraction, then adding acetate, methanol and sulfuric acid according to volume ratio of 3: 2: 1 in the reaction container, wherein the volume fraction of acetate, methanol and sulfuric acid are 10% respectively, adding GA with 25% of mass fraction in the reaction container, wherein the mol ratio of GA to PVA is 1: 4, performing mechanical stirring and reacting for 1-2 hours under the temperature of 50-70 DEG C, washing by water after the reaction is completed, and drying. Through representation and determination, the surface of the modified polyester fiber uniformly contains PVA, the contact angle is less than 10-50 DEG, hydrophilcity of the polyester fiber is greatly improved, the effect is stable, and the polyester fiber can be widely used in the fields of regeneration resource papermaking, clothes, decoration and industry and agriculture.
Description
Technical field
The present invention relates to a kind of method of polyster fibre modification, relate in particular to the method for a kind of PVA to polyster fibre hydrophilic modifying, belong to technical field of macromolecules.
Background technology
Polyster fibre is a kind of of polyester fiber, claim again POLYESTER, it is to take fiber-forming polymer---the polyethylene terephthalate that poly terephthalic acid or dimethyl terephthalate (DMT) and ethylene glycol make through esterification or ester exchange and polycondensation reaction as raw material, the fiber of making through spinning and post processing.Having many uses of polyster fibre, in a large number for the manufacture of goods in clothing and industry.
Many physics of polyster fibre, chemical property are better than natural fabric, as high in intensity, excellent wear resistance, its goods again not yielding, do not crease easily, well-pressed, and cheap.But polyster fibre is because interior molecules is arranged closely, the intermolecular hydrophilic-structure that lacks, thereby regain is very little, and moisture pick-up properties is poor, and gas permeability is bad, and dyeability is poor, and pilling resistance is poor.Therefore the hydrophilicity that improves polyster fibre is the vital task of polyster fibre modification.
Hydrophilic modifying research for polyster fibre mainly contains two aspects: the one, and physical modification method and chemical modification, the former is physical blending, the latter uses the method for chemical graft or block to change the molecular chain structure of polyster fibre; The 2nd, the surface dressing to fiber or fabric.
But the hydrophilic finishing agent using can not fundamentally change the water-wet behavior of polyster fibre and goods thereof, toward contact, to be subject to the restriction of service condition in surface dressing.The method of at present common processing is the principle based on physical blending mostly, and certain material blend spinning by adulterating in melt spinning liquid with water-wet behavior reaches the object of hydrophilic modifying.Japanese patent application publication No. JP S5766123A, on April 22 nineteen eighty-two publication date, denomination of invention is Preparation of modified polyester fiber.This application case discloses a kind of method of physical modification terylene.This application case adopts a kind of cellulose of modification, under the effect of carrier module, joins in molten polyester, to obtain stable hydrophily, and can not damage the mechanical performance that it has.The method of this modification is set about from raw material, similarly method is well applied in factory's practice is produced, at present most of modified polyester fibre and goods thereof are all that method by physical blending obtains on the market, such as Cationic Dyeable Pet, amination modified terylene etc.The angle of producing from raw material, physical blending be a kind of with low cost, produce method of modifying efficiently, but the hydrophilic modifying for existing polyster fibre and goods thereof, mostly the principle based on chemical reaction, generates new hydrophilic radical by the original surface chemical structure of destruction PET fiber and reaches modification object.
For example, a, honeycomb capillary modified polyester fibre, have good moisture absorption, wet transmitting performance by dodging the microcellular structure Cationic Dyeable Pet fiber of quick-fried processing, and this is inseparable with the internal structure of fiber; Foot point is not the surface wettability that the crystallisation of growing nonparasitically upon another plant that ultimate strength and fracture toughness are less than ordinary polyester fiber .b, polyester fiber improves fiber, the employing crystallisation of growing nonparasitically upon another plant improves the surface and interface performance of PET fiber, forefathers' result of study shows, resin forms and crosses after crystal at fiber surface, and the interface bond strength of fiber and resin obviously strengthens.Therefore, can use grow nonparasitically upon another plant crystallisation PET fiber surface grow nonparasitically upon another plant one deck polarity or with the polymer of other resin thermodynamic compatibility, finally reach the object of improving PET fiber surface performance.C, the improvement of lipase treatment to fabrics of polyester hydrophilicity, lipase has certain denudation to polyster fibre fiber surface, and it is more coarse that fiber surface becomes, and its hydrophily significantly improves.
China Patent Publication No. CN 101367912A, February 18 2009 publication date, denomination of invention is modified dacron having excellent hydrophilic and antistatic property and preparation method thereof, this disclosure of the invention a kind of functional ion liquid modified polyester fibre and preparation method thereof, adopt and a kind ofly contain 1, the ionic liquid of 3-bis-(2-methoxyl group-2-oxygen ethyl) glyoxaline structure, react with polyster fibre fiber and goods under certain condition, and change the structure of polyster fibre fiber and goods, make it have certain hydrophily.This method effect is obvious, but operation is succinct not, and reactant is on the high side, partially complicated, is unfavorable for heavy industrialization application.China Patent Publication No. CN 101935952B, on January 4 2012 publication date, denomination of invention is a kind of method of dacron bio-modification.This application case discloses a kind of method of enzyme modified dacron.In order to open the ester bond in the large molecule of PET, thereby produce appropriate hydroxyl and carboxyl, improve the hydrophily of fabric, antistatic behaviour, the performances such as pilling, this patent adopts the terylene monomer that contains phenyl ring as inducer, and induction stosterone produces oxidizing ferment modified dacron fabric from hair monad.But the method step is various, conditional request is too high, and particularly the condition of bacterial classification cultivation and Induction Process is harsh, is not suitable for heavy industrialization application.European Patent Publication No EP 0548452A1, on June 30 1993 publication date, denomination of invention is Hydrophilic silicone-modified polyester resin and fibers and films made there from.This application case discloses a kind of preparation method of hydrophilic polyester fibers.This application case adopts a kind of aromatic dicarboxylic acid and the polysiloxane polyether copolymer esterification that contains dihydroxylic alcohols, and on organosilicon segment, contain hydrophilic group, consequent organosilicon modified polyester, has good hydrophily, is especially applicable to manufacturing hydrophilic fibre and film.The method of this modification is to introduce a kind of segment with hydrophilic radical, but course of reaction is still comparatively complicated, and the hydrophilic modifying of the polyester fiber of inapplicable structural integrity.
Summary of the invention
The object of the invention is, for the poor problem of polyster fibre hydrophilicity, provides the method for a kind of PVA to polyster fibre hydrophilic modifying.
To achieve these goals, the present invention is achieved through the following technical solutions:
The method of a kind of PVA to polyster fibre hydrophilic modifying, the method of described modification refers to that it is that the sodium hydroxide solution of 3-10% stirs preliminary treatment 1h under 70-90 ℃ of condition in stirred vessel that polyster fibre is adopted to mass fraction, mechanical agitation speed is 100-400 rev/min, the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:50, preliminary treatment finishes rear water and rinses and be dried, again dried polyster fibre is put into and filled the reaction vessel that mass fraction is the PVA solution of 0.2-3%, then to adding the acetic acid of 3:2:1 by volume in reaction vessel, methyl alcohol, sulfuric acid, acetic acid, methyl alcohol, the volume fraction of sulfuric acid is respectively 10%, to adding mass fraction in reaction vessel, be 25% GA again, the mol ratio of GA and PVA is 1:4, mechanical agitation reaction 1 ~ 2h at 50 ~ 70 ℃, mechanical agitation speed is 100-400 rev/min, after PVA finishes the graft reaction of polyster fibre, through rinsing and dry 1h under 70 ℃ of conditions, make the polyster fibre after hydrophilic modifying.
Owing to adopting above technical scheme, with the method comparison of existing polyster fibre hydrophilic modifying, the present invention has the following advantages:
1 invention needed raw material and reagent are all AR or are prepared into by AR, and as NaOH, PVA, ethanol, formic acid, sulfuric acid, GA, raw material sources are simple, and use amount is little, and cost is lower.
Reaction condition gentleness related in 2 inventions is controlled, if the temperature of polyster fibre alkali treatment is 70-90 ℃, mechanical agitation speed is 100-400 rev/min, the graft reaction temperature of polyster fibre is 50 ~ 70 ℃, mechanical agitation speed is 100-400 rev/min, and light water bath and mechanical agitator just can the required conditions of realization response.
The related graft reaction of 3 method of modifying of the present invention is to be connected and to fetch realization with terylene surface texture by the hydroxyl in PVA, and PVA itself is a kind of Biodegradable material, has biological nontoxic and biocompatibility, can not contain poisonous organic solvent.
In 4 inventions, gained modified polyester fibre adopts electron microscopic scanning mirror to characterize: in Fig. 1, from (a) to (d) is followed successively by the electron microscope scanning figure that service property (quality) mark is gained polyster fibre 0.2%, 0.8%, 1.5%, 3.0% PVA solution hydrophilic modifying, from (a) and (b), (c) with (d), can find out, in PET fiber surface, there is the stable PVA layer of one deck, increase along with PVA concentration, the PVA of PET fiber surface increases, and more even, but the mass fraction of PVA can not surpass 5%; Gained modified polyester fibre in invention is adopted to the assay method test of contact angle: the polyster fibre of above-mentioned preparation is ground, makes sheet, with CA-A type contact angle instrument, measure, test result is shown in Fig. 2, increase along with PVA mass fraction, the contact angle of modified polyester fibre diminishes gradually, owing to having introduced the oh group in PVA on polyster fibre segment, make the polyster fibre after modification obviously show good hydrophily, after measured, the contact angle of modified polyester fibre prepared by the present invention is less than 10-60 degree, and hydrophilic effect is stable.
Accompanying drawing explanation
Fig. 1 is the electron microscope scanning figure of the polyster fibre after PVA modification.
Fig. 2 is that the contact angle of the polyster fibre after PVA modification is with the variation tendency of PVA concentration.
The specific embodiment
Below in conjunction with drawings and Examples, the present invention is described in further details.
The method of a kind of PVA to polyster fibre hydrophilic modifying, described method refers to first carries out NaOH preliminary treatment to polyster fibre, accurately take a certain amount of sodium hydrate solid, add deionized water to be mixed with the sodium hydroxide solution that mass fraction is 3-10%, again the sodium hydroxide solution preparing is put into stirred vessel, then polyster fibre is immersed in the solution in stirred vessel, under 70-90 ℃ of condition, in stirred vessel, stir preliminary treatment 1h, mechanical agitation speed is 100-400 rev/min, the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:50, after reaction finishes, polyster fibre is taken out, water rinses and to remain in PET fiber surface and inner sodium hydroxide solution, after rinsing well, put into baking oven inner drying, accurately take a certain amount of PVA solid, add deionized water under 70 ℃ of conditions, to be mixed with the PVA solution that mass fraction is 0.2-3%, this is conducive to the dissolving of PVA solid, carries out mechanical agitation simultaneously and is beneficial to PVA solute and is uniformly distributed in solution, get volume fraction and be respectively 10% acetic acid, methyl alcohol, sulfuric acid solution, by the volume ratio of 3:2:1, mix, the PVA solution preparing is put into reaction vessel, then dried polyster fibre is immersed in the PVA solution in reaction vessel, under 50 ~ 70 ℃ of conditions, carry out mechanical agitation, simultaneously to having added the acetic acid that 3:2:1 mixes by volume in reaction vessel, methyl alcohol, sulfuric acid mixed solution, with pipettor, to adding mass fraction in reaction vessel, be 25% GA solution again, GA and PVA's mole is than 1:4, mechanical agitation reaction 1 ~ 2h at 50 ~ 70 ℃, mechanical agitation speed is 100-400 rev/min, sealed reaction vessel in course of reaction, after reaction finishes, polyster fibre is taken out, water rinses and remains in PET fiber surface and inner acetic acid, methyl alcohol, sulfuric acid, GA solution, there is no the PVA solution crosslinked with polyster fibre, other issuable impurity, after rinsing well, polyster fibre is put into baking oven, dry 1h under 70 ℃ of conditions, be dried rear taking-up, it is exactly the polyster fibre after hydrophilic modifying, in order to characterize the crosslinked PVA monomer of having gone up of PET fiber surface, polyster fibre after hydrophilic modifying is spun under electronic scanner microscope to large 2000 times and observe its surface state, in order to test the hydrophily of the polyster fibre after modification, again it is carried out the test of contact angle, polyster fibre after the modification of above-mentioned preparation is ground, makes sheet, with CA-A type contact angle instrument, measure.
Specific embodiment
embodiment 1
1 accurately takes 3g sodium hydrate solid, adding 97ml water to be mixed with mass fraction is 3% sodium hydroxide solution, and contain in stirred vessel, then container is added to 2g polyster fibre, under 70 ℃ of conditions, stir preliminary treatment 1h in reaction vessel, mechanical agitation speed is 100 revs/min, and the solid-to-liquid ratio of polyster fibre and reaction solution is 1:50, after reaction finishes, water rinses and is dried polyster fibre.
2 use electronics weighing devices accurately take 1.0gPVA, add 499ml deionized water, under 70 ℃ of conditions, dissolve, and are mixed with mass fraction and are 0.2% PVA solution, and solute is uniformly distributed in solution.
3 put into reaction vessel by above-mentioned dried polyster fibre and the PVA solution that the mass fraction configuring is 0.2%, then reaction vessel is added to 30ml acetic acid, 20ml methyl alcohol, 10ml sulfuric acid, the volume fraction of acetic acid, methyl alcohol, sulfuric acid is respectively 10%, with pipettor, reaction vessel is added to 0.057gGA solution again, the mol ratio of GA and PVA is 1:4, the molecular weight of PVA is pressed mean molecule quantity 1750 and is calculated, the molecular weight of GA is 100, the mass fraction of GA is 25%, stirring reaction 1h at 50 ℃, mechanical agitation speed is 100 revs/min.
After 4 reactions finish, rinse and dry reagent contained, obtain the polyster fibre after hydrophilic modifying.
The hydrophilicity test of 5 modified polyester fibres: adopt the assay method of contact angle, the polyster fibre of above-mentioned preparation is ground, makes sheet, measure with CA-A type contact angle instrument, the contact angle of modified polyester fibre prepared by the present invention is below 45 degree.
embodiment 2
1 accurately takes 5g sodium hydrate solid, adding 95ml water to be mixed with mass fraction is 5% sodium hydroxide solution, and contain in stirred vessel, then container is added to 2g polyster fibre, under 70 ℃ of conditions, stir preliminary treatment 1h in reaction vessel, mechanical agitation speed is 250 revs/min, and the solid-to-liquid ratio of polyster fibre and reaction solution is 1:50, after reaction finishes, water rinses and is dried polyster fibre.
2 use electronics weighing devices accurately take 2.0gPVA, add 98ml deionized water, under 70 ℃ of conditions, dissolve, and are mixed with mass fraction and are 2% PVA solution, and solute is uniformly distributed in solution.
3 put into reaction vessel by above-mentioned dried polyster fibre and the PVA solution that the mass fraction configuring is 2%, then reaction vessel is added to 30ml acetic acid, 20ml methyl alcohol, 10ml sulfuric acid, the volume fraction of acetic acid, methyl alcohol, sulfuric acid is respectively 10%, with pipettor, reaction vessel is added to 0.114gGA solution again, the mol ratio of GA and PVA is 1:4, the molecular weight of PVA is pressed mean molecule quantity 1750 and is calculated, the molecular weight of GA is 100, the mass fraction of GA is 25%, stirring reaction 1.5h at 60 ℃, mechanical agitation speed is 250 revs/min.
After 4 reactions finish, rinse and dry reagent contained, obtain the polyster fibre after hydrophilic modifying.
The hydrophilicity test of 5 modified polyester fibres: adopt the assay method of contact angle, the polyster fibre of above-mentioned preparation is ground, makes sheet, measure with CA-A type contact angle instrument, the contact angle of modified polyester fibre prepared by the present invention is below 30 degree.
embodiment 3
1 accurately takes 10g sodium hydrate solid, adding 90ml water to be mixed with mass fraction is 10% sodium hydroxide solution, and contain in stirred vessel, then container is added to 2g polyster fibre, under 70 ℃ of conditions, stir preliminary treatment 1h in reaction vessel, mechanical agitation speed is 400 revs/min, and the solid-to-liquid ratio of polyster fibre and reaction solution is 1:50, after reaction finishes, water rinses and is dried polyster fibre.
2 use electronics weighing devices accurately take 3.0gPVA, add 97ml deionized water, under 70 ℃ of conditions, dissolve, and are mixed with mass fraction and are 3% PVA solution, and solute is uniformly distributed in solution.
3 put into reaction vessel by above-mentioned dried polyster fibre and the PVA solution that the mass fraction configuring is 3%, then reaction vessel is added to 30ml acetic acid, 20ml methyl alcohol, 10ml sulfuric acid, the volume fraction of acetic acid, methyl alcohol, sulfuric acid is respectively 10%, with pipettor, reaction vessel is added to 0.171gGA solution again, the mol ratio of GA and PVA is 1:4, the molecular weight of PVA is pressed mean molecule quantity 1750 and is calculated, the molecular weight of GA is 100, the mass fraction of GA is 25%, stirring reaction 2h at 70 ℃, mechanical agitation speed is 400 revs/min.
After 4 reactions finish, rinse and dry reagent contained, obtain the polyster fibre after hydrophilic modifying.
The hydrophilicity test of 5 modified polyester fibres: adopt the assay method of contact angle, the polyster fibre of above-mentioned preparation is ground, makes sheet, measure with CA-A type contact angle instrument, the contact angle of modified polyester fibre prepared by the present invention is below 10 degree.
Claims (1)
1. the PVA method to polyster fibre hydrophilic modifying, it is characterized in that: the method for described modification refers to that it is that the sodium hydroxide solution of 3-10% stirs preliminary treatment 1h under 70-90 ℃ of condition in stirred vessel that polyster fibre is adopted to mass fraction, mechanical agitation speed is 100-400 rev/min, the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:50, preliminary treatment finishes rear water and rinses and be dried, again dried polyster fibre is put into and filled the reaction vessel that mass fraction is the PVA solution of 0.2-3%, then to adding the acetic acid of 3:2:1 by volume in reaction vessel, methyl alcohol, sulfuric acid, acetic acid, methyl alcohol, the volume fraction of sulfuric acid is respectively 10%, to adding mass fraction in reaction vessel, be 25% GA again, the mol ratio of GA and PVA is 1:4, mechanical agitation reaction 1 ~ 2h at 50 ~ 70 ℃, mechanical agitation speed is 100-400 rev/min, after PVA finishes the graft reaction of polyster fibre, through rinsing and being dried under 70 ℃ of conditions, make the polyster fibre after hydrophilic modifying.
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Cited By (7)
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| CN105088761A (en) * | 2015-09-17 | 2015-11-25 | 福建师范大学泉港石化研究院 | Method for hydrophilic modification of polyester fibers by amphiphilic triazine monomer |
| CN105544193A (en) * | 2016-01-25 | 2016-05-04 | 苏州印丝特纺织数码科技有限公司 | Hydrophilic modification method for polyester fibers with bromoethane and PVA |
| CN105908507A (en) * | 2016-05-26 | 2016-08-31 | 张家港鸿运织标有限公司 | Process for producing polyester warp knitted fabric crown-covering strip |
| CN106637977A (en) * | 2016-12-16 | 2017-05-10 | 池州方达科技有限公司 | Polyester fiber treating agent prepared from hydroxyethyl methylacrylate |
| CN108951176A (en) * | 2018-06-27 | 2018-12-07 | 阜南美凯服饰有限公司 | A kind for the treatment of process improving dacron hydrophilic |
| CN108978269A (en) * | 2018-06-27 | 2018-12-11 | 阜南美凯服饰有限公司 | A kind of processing method improving dacron dyefastness |
| CN109403037A (en) * | 2018-11-09 | 2019-03-01 | 安徽农业大学 | A kind of modified polyester fibre and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088761A (en) * | 2015-09-17 | 2015-11-25 | 福建师范大学泉港石化研究院 | Method for hydrophilic modification of polyester fibers by amphiphilic triazine monomer |
| CN105088761B (en) * | 2015-09-17 | 2017-03-22 | 福建师范大学泉港石化研究院 | Method for hydrophilic modification of polyester fibers by amphiphilic triazine monomer |
| CN105544193A (en) * | 2016-01-25 | 2016-05-04 | 苏州印丝特纺织数码科技有限公司 | Hydrophilic modification method for polyester fibers with bromoethane and PVA |
| CN105544193B (en) * | 2016-01-25 | 2017-11-28 | 苏州印丝特纺织数码科技有限公司 | The hydrophilic modification method of a kind of bromoethane and PVA to polyester fiber |
| CN105908507A (en) * | 2016-05-26 | 2016-08-31 | 张家港鸿运织标有限公司 | Process for producing polyester warp knitted fabric crown-covering strip |
| CN106637977A (en) * | 2016-12-16 | 2017-05-10 | 池州方达科技有限公司 | Polyester fiber treating agent prepared from hydroxyethyl methylacrylate |
| CN108951176A (en) * | 2018-06-27 | 2018-12-07 | 阜南美凯服饰有限公司 | A kind for the treatment of process improving dacron hydrophilic |
| CN108978269A (en) * | 2018-06-27 | 2018-12-11 | 阜南美凯服饰有限公司 | A kind of processing method improving dacron dyefastness |
| CN109403037A (en) * | 2018-11-09 | 2019-03-01 | 安徽农业大学 | A kind of modified polyester fibre and preparation method thereof |
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| CN103981711B (en) | 2016-09-14 |
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