CN105113209A - Preparation method of PPS fibers with self-extinguishment and free of molten drops - Google Patents
Preparation method of PPS fibers with self-extinguishment and free of molten drops Download PDFInfo
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- CN105113209A CN105113209A CN201510631820.5A CN201510631820A CN105113209A CN 105113209 A CN105113209 A CN 105113209A CN 201510631820 A CN201510631820 A CN 201510631820A CN 105113209 A CN105113209 A CN 105113209A
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Abstract
The invention discloses a preparation method of PPS fibers with self-extinguishment and free of molten drops. The preparation method comprises the following steps: soaking a pure polyphenylene sulfide fiber serving as a raw material into an oxidant solution, controlling the soaking temperature and the soaking time by selecting the type of an oxidant, adjusting the oxidization degree of sulfur atoms on the surface of the fiber, performing solvent separation after an reaction, and washing and drying the PPS fibers. The preparation method is simple and feasible, and a complicated fiber modification method is eliminated; the performances, such as oxidization resistance, high-temperature resistance, creep resistance and molten drop resistance, of the prepared PPS fibers are greatly improved.
Description
Technical field
The present invention relates to the technology of preparing of PPS fiber, be specially a kind of preparation method with self-extinguishment and the PPS fiber without molten drop.The method utilizes oxidant to be sulfone (SO by polyphenylene sulfide fibre surface sulphur atom (S) partial oxidation
2), the PPS fiber of the selective oxidation of generation has without molten drop and creep resisting feature.
Background technology
Polyphenylene sulfide (be called for short PPS) be with phenyl ring to on link sulphur atom and the stiff backbone that formed, owing to there being the existence of a large amount of π key in structure, so its performance is more stable.The maximum feature of PPS fiber is exactly Long-Time Service under higher temperatures and extremely severe working environment, is mainly used in heat filtering material.Along with the development of high-tech research and application, people have higher requirement to exotic material.The serviceability temperature of PPS fiber is about 180 DEG C, and the exhaust temperature of plant emissions often reaches 190-220 DEG C, and under this hot environment, fibres show creep causes web contraction, and causes PPS fibrous mechanical property to reduce and life-span minimizing.PPS belongs to middle high section filtering material, and not resistance to oxidation, exploitation PPS is the high temperature resistant of matrix and oxidation resistant fiber, makes its high temperature resistant grade section of reaching a high temperature, can at 280-300 DEG C of Long-Time Service.Because PPS vitrification point and fusing point are not very high, cause this kind of easy creep of fiber and easy molten drop, if the vitrification point of MODIFIED PP S is brought up to more than 300 DEG C, the preparation without molten drop and the PPS high-temperature fibre without creep will be realized completely.This modified fibre can be widely used as protective articles, as fire-entry suit, stokehold Work Clothes, electric welding Work Clothes, special uniform, fireproof felt, fire screen and fireproof glove etc.
While maintenance PPS its excellent properties, tackle it and carry out structure and composition carries out modification.Blended is make up PPS defect the most effectively and one of the simplest method.By the mode of modification, overcome the above-mentioned shortcoming of PPS fiber, improve the combination property of PPS fiber.The copolymers such as usual employing polyamide, polyolefin, polytetrafluoroethylene (PTFE) carry out co-blended spinning, and in PPS resin, add the stuffing such as calcium carbonate, nano imvite, CNT, silica or organo-mineral complexing antioxidant carry out modification to PPS fiber.Compared with PPS fiber, PPS/SiO
2fibrous mechanical property improves, and heat resisting temperature can improve 50 DEG C.On the other hand, due to SiO
2/ PPS fiber increases at the post crystallization degree that is heated, and make PPS aggregated structure more stable, therefore its percent thermal shrinkage significantly reduces.PPS fiber surface modification is also the important means promoting its performance; PTFE dispersion liquid is applied in the Final finishing of PPS filtrate; PTFE is formed on fiber coating; filtrate is played a protective role; intercept the infringement of oxidisability and corrosive goods confrontation filtrate, improve the performance of filtrate, make filtrate have better filter efficiency; more easy-to-clean ash, and increase the service life.Sol-gel process is utilized to be coated with on the surface of conventional PPS fiber with SiO
2, SiC, BN and TiO
2be the protective layer of main body Deng ceramic material, effectively can extend the service time of fiber under high-temperature oxygen-enriched condition, can further improve fire-retardant, acidproof, the resistance to oxidation of fiber and the performance such as high temperature resistant.In addition, plasma processing techniques is utilized also can to carry out surface modification to PPS fiber.But current method of modifying technique is more complicated, difficult control, and cost is also relatively high, is unfavorable for that industrialization is produced.
Summary of the invention
For the deficiencies in the prior art, the technical problem that quasi-solution of the present invention is determined is, a kind of preparation method with self-extinguishment and the PPS fiber without molten drop is provided, this preparation method for raw material, is impregnated in oxidizing agent solution with pure polyphenylene sulfide fibre, by selective oxidation agent kind, control dipping temperature and dip time, the degree of oxidation of regulation and control fiber surface sulphur atom, reacts complete by separated from solvent, and by PPS fiber wash and drying.This preparation method is simple, eliminates the method for complicated fibre modification, and the performances such as anti-oxidant, high temperature resistant, the creep resistant of prepared PPS fiber and anti-dropping improve greatly.
The technical scheme that the present invention solve the technical problem is, provides a kind of preparation method with self-extinguishment and the PPS fiber without molten drop, it is characterized in that described preparation method comprises the following steps:
(1) configure oxidizing agent solution: be dissolved or dispersed in by oxidant in solvent, forming mass concentration is the oxidizing agent solution of 0.5-40wt%;
(2) dipping washing is dry: by PPS fiber impregnation in oxidizing agent solution, the quality of PPS fiber accounts for the 10-40wt% of PPS fiber and oxidizing agent solution gross mass, and dipping temperature is 60-140 DEG C, and dip time is 10min-12h; By separated from solvent, washing and dry step, vacuumize temperature is 60-180 DEG C, and drying time is 1-48h, obtains having self-extinguishment and the PPS fiber without molten drop;
Above-mentioned steps (1), (2) are in normal pressure to a 30 normal atmosphere pressure reaction;
Described oxidant is KMnO
4, K
2cr
2o
7, MnO
2, FeCl
3, HClO, H
2o
2, Na
2o
2, NO
2, HNO
3, O
3, peracetic acid, performic acid, dicumyl peroxide, benzoyl peroxide, methyl ethyl ketone peroxide, cyclohexanone peroxide, tertbutanol peroxide or tertiary butyl perbenzoate at least one;
Described solvent is at least one of water, benzene, toluene, ketone compounds, Organic Alcohol, amide compound, dimethyl sulfoxide (DMSO), oxolane, ether, dimethyl ether, cyclohexane, n-hexane, organic acid or halogenated hydrocarbons.
Compared with prior art, beneficial effect of the present invention is:
1. utilize PPS fiber for raw material, by simple solution impregnation and surface oxidation technology, by polyphenylene sulfide fibre surface portion sulphur atom (S) optionally partial oxidation be sulfone (SO
2), to have prepared cortex be polyether sulfone and sandwich layer is the composite fibre of PPS, and PPS fibrous outer surfaces introduces polarity conjugation group SO
2, make its outer surface become noncrystallizable polymer, the PPS fiber of this surperficial selective oxidation compensate for PPS vitrification point and melting temperature is not high, poor toughness and the large shortcoming of fragility.
2, the vitrification point of PPS fiber prepared of this method is high, under high temperature, fiber occurs without molten drop with without creep, compensate for PPS vitrification point and melting temperature is not high, poor toughness, fragility are large and easily produce electrostatic, monofilament cohesive force is poor, strand is loose, coefficient of friction is large, cannot carry out the shortcoming of aft-loaded airfoil.Fiber prepared by this method has the feature of preferably creep resistant and anti-dropping, and excellent mechanical property, by improving the performance of PPS fiber surface, improve its wettability and caking property, improve its electric conductivity, thus reduce the lousiness of fiber in process, broken end etc., improve tensile property and the aftertreatment performance of fiber, make it smoothly by each road manufacturing procedure.This fiber can be used for protective articles, as fire-entry suit, stokehold Work Clothes, electric welding Work Clothes, special uniform, fire screen, fireproof felt and fireproof glove etc.Can be used for high-end filtering material, as high-temperature flue dedusting filtering bag and chemical industry filter cloth etc.
Detailed description of the invention
The invention provides a kind of preparation method with self-extinguishment and the PPS fiber without molten drop, described preparation method comprises the following steps:
(1) configure oxidizing agent solution: be dissolved or dispersed in by oxidant in solvent, forming mass concentration is the oxidizing agent solution of 0.5-40wt%; Preferred oxidant concentration of polymer solution is 5% ~ 15%.
(2) dipping washing is dry: by PPS fiber impregnation in oxidizing agent solution, the quality of PPS fiber accounts for the 10-40wt% of PPS fiber and oxidizing agent solution gross mass, and preferred mass mark is 15 ~ 25%; Dipping temperature is 60-140 DEG C, and preferred dipping temperature is 65 ~ 90 DEG C; Dip time is 10min-12h, and preferred dip time is 0.5 ~ 2h; By separated from solvent, washing and dry step, vacuumize temperature is 60-180 DEG C, and preferred baking temperature is 80 ~ 120 DEG C; Drying time is 1-48h, and preferred drying time is 6 ~ 12h, obtains having self-extinguishment and the PPS fiber without molten drop.
Above-mentioned steps (1), (2) are in normal pressure to a 30 normal atmosphere pressure reaction.
Described oxidant is KMnO
4, K
2cr
2o
7, MnO
2, FeCl
3, HClO, H
2o
2, Na
2o
2, NO
2, HNO
3, O
3, peracetic acid, performic acid, dicumyl peroxide, benzoyl peroxide, methyl ethyl ketone peroxide, cyclohexanone peroxide, tertbutanol peroxide or tertiary butyl perbenzoate at least one.
Described solvent is Organic Alcohol, the N such as the ketone compounds such as the aromatic solvent such as water, Benzene and Toluene, acetone and butanone, methyl alcohol and ethanol, the organic acids such as the alkane such as the alkyl ethers such as the amide compounds such as N-dimethylacetylamide and 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), oxolane, ether and dimethyl ether, cycloalkanes or aryl ether, cyclohexane and n-hexane, acetic acid and formic acid or the halogenated hydrocarbons such as tetrachloroethanes and chloroform etc., these solvents can be mutually composite.
Provide specific embodiments of the invention below.
Embodiment 1
By 3L10%H
2o
2with 500gPPS fiber (TENSILE STRENGTH 3.9CN/dt, elongation at break 20%), be heated to 60 DEG C under mechanical agitation, then keep 10 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fiber deionized water washes 3 times respectively, 140 DEG C of vacuum dryings 12 hours, namely obtain that there is self-extinguishment and the PPS fiber without molten drop.
The PPS fiber of made preparation, the oxidized sulfur atom on surface 22% is sulfone, has self-extinguishment and without molten drop phenomenon, vitrification point reaches 165 DEG C, tensile strength of fiber 3.8CN/dt, elongation at break 21%.
Embodiment 2
By 10%KMnO
43L and 600gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 60 DEG C under mechanical agitation, then keep 10 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 140 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.
The oxidized sulfur atom of made PPS fiber surface 28% is sulfone, has self-extinguishment and without molten drop phenomenon, vitrification point reaches 176 DEG C, tensile strength of fiber 4.0CN/dt, elongation at break 23%.
Embodiment 3
By 3L5%HClO and 400gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 80 DEG C under mechanical agitation, then keep 20 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 160 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.
The oxidized sulfur atom of made PPS fiber surface 19% is sulfone, and PPS fiber has self-extinguishment and without molten drop phenomenon, vitrification point reaches 156 DEG C, tensile strength of fiber 4.1CN/dt, elongation at break 24%.
Embodiment 4
By 3L10%HNO
3with 500gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 40 DEG C under mechanical agitation, then keep 20 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 150 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.
The oxidized sulfur atom of made PPS fiber surface 23% is sulfone, and PPS fiber has self-extinguishment and without molten drop phenomenon, vitrification point reaches 170 DEG C, tensile strength of fiber 4.1CN/dt, elongation at break 23%.
Embodiment 5
By the benzole soln of 3L10% benzoyl peroxide and 400gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 60 DEG C under mechanical agitation, then keep 40 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 150 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.
The oxidized sulfur atom of made PPS fiber surface 24% is sulfone, and PPS fiber has self-extinguishment and without molten drop phenomenon, vitrification point reaches 172 DEG C, tensile strength of fiber 4.2CN/dt, elongation at break 25%.
Embodiment 6
By the benzole soln of 3L10% cyclohexanone peroxide and 400gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 60 DEG C under mechanical agitation, then keep 40 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 150 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.
The oxidized sulfur atom of made PPS fiber surface 20% is sulfone, and PPS fiber has self-extinguishment and without molten drop phenomenon, vitrification point reaches 160 DEG C, tensile strength of fiber 4.2CN/dt, elongation at break 25%.
Embodiment 7
By the N of 3L10% cyclohexanone peroxide, N-dimethylacetamide solution and 400gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 70 DEG C under mechanical agitation, then keep 40 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 150 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.
The oxidized sulfur atom of PPS fiber surface 18% is sulfone, and PPS fiber has self-extinguishment and without molten drop phenomenon, vitrification point reaches 158 DEG C, tensile strength of fiber 4.2CN/dt, elongation at break 25%.
Embodiment 8
By the acetic acid solution of 3L10% cyclohexanone peroxide and 400gPPS fiber (TENSILE STRENGTH 4.2CN/dt, elongation at break 25%), be heated to 70 DEG C under mechanical agitation, then keep 40 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fibrous ion water washes 3 times respectively, 150 DEG C of vacuum dryings 12 hours, obtain that there is self-extinguishment and the PPS fiber without molten drop.The oxidized sulfur atom of PPS fiber surface 19% is sulfone,
PPS fiber has self-extinguishment and without molten drop phenomenon, vitrification point reaches 145 DEG C, tensile strength of fiber 4.2CN/dt, elongation at break 25%.
Embodiment 9
By 3L15%H
2o
2with 500gPPS fiber (TENSILE STRENGTH 3.9CN/dt, elongation at break 20%), be heated to 80 DEG C under mechanical agitation, then keep 20 minutes, utilize 200 ~ 400 order steel wire filtering solutions, after PPS fiber deionized water washes 3 times respectively, 140 DEG C of vacuum dryings 12 hours, namely obtain that there is self-extinguishment and the PPS fiber without molten drop.
The PPS fiber of made preparation, the oxidized sulfur atom on surface 85% is sulfone, has self-extinguishment and without molten drop phenomenon, vitrification point reaches 300 DEG C, tensile strength of fiber 3.7CN/dt, elongation at break 16.5%.
Claims (5)
1. there is a preparation method for self-extinguishment and the PPS fiber without molten drop, it is characterized in that described preparation method comprises the following steps:
(1) configure oxidizing agent solution: be dissolved or dispersed in by oxidant in solvent, forming mass concentration is the oxidizing agent solution of 0.5-40wt%;
(2) dipping washing is dry: by PPS fiber impregnation in oxidizing agent solution, the quality of PPS fiber accounts for the 10-40wt% of PPS fiber and oxidizing agent solution gross mass, and dipping temperature is 60-140 DEG C, and dip time is 10min-12h; By separated from solvent, washing and dry step, vacuumize temperature is 60-180 DEG C, and drying time is 1-48h, obtains having self-extinguishment and the PPS fiber without molten drop;
Above-mentioned steps (1), (2) are in normal pressure to a 30 normal atmosphere pressure reaction;
Described oxidant is KMnO
4, K
2cr
2o
7, MnO
2, FeCl
3, HClO, H
2o
2, Na
2o
2, NO
2, HNO
3, O
3, peracetic acid, performic acid, dicumyl peroxide, benzoyl peroxide, methyl ethyl ketone peroxide, cyclohexanone peroxide, at least one in tertbutanol peroxide or tertiary butyl perbenzoate;
Described solvent is at least one in water, benzene, toluene, ketone compounds, Organic Alcohol, amide compound, dimethyl sulfoxide (DMSO), oxolane, ether, dimethyl ether, cyclohexane, n-hexane, organic acid or halogenated hydrocarbons.
2. the preparation method with self-extinguishment and the PPS fiber without molten drop according to claim 1, is characterized in that in described step (1), oxidizing agent solution mass concentration is 5 ~ 15%.
3. the preparation method with self-extinguishment and the PPS fiber without molten drop according to claim 1, is characterized in that the quality of PPS fiber in described step (2) accounts for 15 ~ 25% of PPS fiber and oxidizing agent solution gross mass.
4. the preparation method with self-extinguishment and the PPS fiber without molten drop according to claim 1, is characterized in that in described step (2), dipping temperature is 65 ~ 90 DEG C; Dip time is 0.5 ~ 2h; Baking temperature is 80 ~ 120 DEG C; Drying time is 6 ~ 12h.
5. the preparation method with self-extinguishment and the PPS fiber without molten drop according to claim 1, is characterized in that described ketone compounds is acetone or butanone; Described Organic Alcohol is methyl alcohol or ethanol; Described amide compound is DMA or 1-METHYLPYRROLIDONE; Described organic acid is acetic acid or formic acid; Halogenated hydrocarbons is tetrachloroethanes or chloroform.
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Cited By (9)
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CN105544183A (en) * | 2015-12-22 | 2016-05-04 | 苏州协泰科技有限公司 | A PPS fiber modification process |
CN110184811A (en) * | 2019-04-25 | 2019-08-30 | 四川安费尔高分子材料科技有限公司 | A kind of polyphenylene sulfide fibre and preparation method thereof of the anti-shrink under ignition |
CN111286836A (en) * | 2020-03-11 | 2020-06-16 | 山东星宇手套有限公司 | Flame-retardant anti-cutting yarn based on modified polyphenylene sulfide, preparation method and glove |
CN111349240A (en) * | 2018-12-24 | 2020-06-30 | 上海钱丰纺织品有限公司 | Modified polyphenylene sulfide with high glass transition temperature and preparation method thereof |
CN111364138A (en) * | 2020-03-11 | 2020-07-03 | 山东星宇手套有限公司 | Composite yarn for manufacturing high-temperature operation protective articles, preparation method and high-temperature operation protective gloves |
CN112080930A (en) * | 2020-09-24 | 2020-12-15 | 福州大学 | Method for rapidly preparing polyphenylene sulfone sulfoxide fiber through liquid-phase oxidation at normal temperature and normal pressure |
CN113481626A (en) * | 2021-07-14 | 2021-10-08 | 天津工业大学 | Preparation method of polyphenylene sulfide sulfone ketone fiber |
CN115637582A (en) * | 2022-10-26 | 2023-01-24 | 清源创新实验室 | Method for preparing polyphenylene sulfone sulfoxide fiber by ozone-hydrogen peroxide synergistic heterogeneous oxidation |
CN116556046A (en) * | 2023-05-30 | 2023-08-08 | 山东明化新材料有限公司 | Method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and product thereof |
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Cited By (10)
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CN105544183A (en) * | 2015-12-22 | 2016-05-04 | 苏州协泰科技有限公司 | A PPS fiber modification process |
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CN110184811A (en) * | 2019-04-25 | 2019-08-30 | 四川安费尔高分子材料科技有限公司 | A kind of polyphenylene sulfide fibre and preparation method thereof of the anti-shrink under ignition |
CN111286836A (en) * | 2020-03-11 | 2020-06-16 | 山东星宇手套有限公司 | Flame-retardant anti-cutting yarn based on modified polyphenylene sulfide, preparation method and glove |
CN111364138A (en) * | 2020-03-11 | 2020-07-03 | 山东星宇手套有限公司 | Composite yarn for manufacturing high-temperature operation protective articles, preparation method and high-temperature operation protective gloves |
CN112080930A (en) * | 2020-09-24 | 2020-12-15 | 福州大学 | Method for rapidly preparing polyphenylene sulfone sulfoxide fiber through liquid-phase oxidation at normal temperature and normal pressure |
CN113481626A (en) * | 2021-07-14 | 2021-10-08 | 天津工业大学 | Preparation method of polyphenylene sulfide sulfone ketone fiber |
CN115637582A (en) * | 2022-10-26 | 2023-01-24 | 清源创新实验室 | Method for preparing polyphenylene sulfone sulfoxide fiber by ozone-hydrogen peroxide synergistic heterogeneous oxidation |
CN116556046A (en) * | 2023-05-30 | 2023-08-08 | 山东明化新材料有限公司 | Method for simply and conveniently preparing high-temperature-resistant antioxidant polyphenylene sulfide fibers and product thereof |
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