CN109778335A - A kind of modified polypropylene fiber and preparation method - Google Patents
A kind of modified polypropylene fiber and preparation method Download PDFInfo
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- CN109778335A CN109778335A CN201910192616.6A CN201910192616A CN109778335A CN 109778335 A CN109778335 A CN 109778335A CN 201910192616 A CN201910192616 A CN 201910192616A CN 109778335 A CN109778335 A CN 109778335A
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Abstract
The present invention relates to modified polypropylene fiber fields, and in particular to a kind of modified polypropylene fiber and preparation method.The present invention reacts graphene oxide and alkyl mercaptoamine, obtain sulfhydryl modified graphene oxide, sulfydryl-alkene clicking chemistry is carried out with vinyl POSS again to react, obtain vinyl POSS modified graphene oxide, sulfydryl-alkene clicking chemistry is carried out with alkyl hydrosulfide again to react, then redox graphene obtains POSS/ graphene composite material;POSS/ graphene composite material is added to melt pelletization in PP GRANULES and obtains modified polypropylene agglomerate, then with PP GRANULES melt spinning, obtain modified polypropylene fiber.The modified polypropylene fiber that the present invention obtains has preferable electric conductivity, thermal conductivity, anti-flammability and mechanical property, can apply in weaving.
Description
Technical field
The present invention relates to modified polypropylene fiber fields, and in particular to a kind of modified polypropylene fiber and preparation method.
Background technique
Cage modle polysilsesquioxane, abbreviation POSS have general structure (RSiO1.5)n, it is the silicon alternately connected by Si-O
The inorganic kernel of oxygen skeleton composition, the group R that Si atom is connected on its apex angle are reactivity or inertia group.The three of POSS
Size is tieed up between 1.3nm, wherein the distance between Si atom is 0.5nm, and the distance between R group is 1.5nm, belongs to nanometer
Compound.POSS through being added in polymer frequently as additive so that modified polymer heat-resistant, mechanical property plus
Work performance, anti-flammability can be improved effectively.
The Chinese invention of publication No. CN101724982A, which is applied for a patent, discloses that a kind of POSS modified polypropylene melt-blown is non-to be knitted
Cloth and preparation method thereof is made, POSS is first added to polypropylene and prepares polypropylene functional agglomerate, then prepares poly- third containing POSS
Alkene melt-blow nonwoven.
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit forms the two dimension that hexangle type is in honeycomb lattice
Carbon nanomaterial.Since 2004 are found, graphene have excellent optics, electricity, mechanical characteristic, materialogy,
Micro-nano technology, the energy, biomedicine and drug delivery etc. are with important application prospects, it is considered to be a kind of future revolution
The material of property.Graphene is added to the thermal conductivity, electric conductivity, mechanical strength etc. that polymer can be improved in polymer.
Application of the graphene in weaving is mainly the surface by being added in polymer or being adsorbed on fiber, is formed
Modified fibre have the function of conductive, thermally conductive etc..The Chinese invention granted patent of publication No. CN103966844B discloses one kind
The preparation method of graphene conductive composite fibre, by fiber surface with KH-560 it is silane coupler modified after, be immersed in graphene
It is handled in dispersion, obtains graphene conductive composite fibre, there is preferable electric conductivity.
Finishing agent containing POSS or graphene is applied to the final finishing of fabric, and POSS or graphene pass through chemical graft or object
Reason is adsorbed onto the surface of fabric.But this method has the disadvantage that the POSS for being fabric surface or graphene are being washed, used
It can gradually decrease in the process, cause effect more and more weaker.Another kind into fibre-forming polymer, obtains POSS or graphene dispersion
Functional fiber can have longer action time.
In view of the performance of POSS and graphene, it is to play simultaneously that POSS and graphene are added to purpose in fiber together
The function of POSS and graphene, but both materials, which are added separately in fiber, only can respectively play a role, or even can be mutual
Mutually hinder.
POSS and graphene formed after compound be then added in fiber be it is a kind of can collaboration play POSS and graphene
The method of energy.The Chinese invention of publication No. CN107385542A, which is applied for a patent, proposes a kind of POSS grafted graphene oxide modification
Nylon compound resin and its preparation method of fiber the POSS containing amino or hydroxyl and graphite oxide alkene reaction are obtained
POSS grafted graphene oxide, then mixed with lactam monomers, it then reacts, it is in-situ modified to obtain POSS grafted graphene oxide
Nylon compound resin slice, obtain modified nylon fiber after melt spinning.
Sulfydryl-alkene clicking chemistry reaction is a kind of " green " chemical reaction, is had without removing water deoxygenation, reaction condition temperature
With the advantages that reaction time is short, reaction conversion ratio is high, reaction product is with high purity, in hydrogel, film, lithographic printing and biology
Material Field has a wide range of applications.
Summary of the invention
(1) the technical issues of solving used
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of modified polypropylene fibers, have preferable
Electric conductivity, thermal conductivity, mechanical strength and flame retardant property, and graphene/cage modle polysilsesquioxane composite material is in additive amount
It is larger that (mass fraction is more than 5%, or even close to 10%) all with preferable mechanical property.
It is another object of the present invention to provide a kind of preparation methods of modified polypropylene fiber.
(2) technical solution
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that,
A kind of modified polypropylene fiber is made of by weight percentage following components, and 0.1~10% graphene/cage modle is poly-
Silsesquioxane (graphene/POSS) composite material, 90~99.9% polypropylene.
Preferably, it is made of by weight percentage following components, 0.5~5% graphene/POSS composite material, 95~
99.5% polypropylene.
Preferably, the graphene/POSS composite material preparation method includes the following steps,
S1: according to parts by weight, 1~10 part of graphene oxide is added to 20~30 points of ultrasound in 1000 parts of dehydrated alcohols
Clock, addition general structure are HS (CH2)nNH2Alkyl mercaptoamine and 0.5 times of alkyl mercaptoamine weight of 1- (3- dimethylamino third
Base) -3- ethyl carbodiimide (EDC), it is warming up to the micro- reflux of system under stirring, reacts 0.5~2 hour, filtering removes filtrate,
It filters out solid washes of absolute alcohol 5 times, dries in vacuum drying oven to constant weight, obtain sulfhydryl modified graphene oxide;Wherein n
=2,3,4;
S2: according to parts by weight, the sulfhydryl modified graphene oxide in 5~20 parts of step S1 is added to 1000 parts of acetic acid
Ultrasound 20~30 minutes in ethyl ester, are added octavinyl-POSS and 0.01 times of POSS weight of dimethoxybenzoin, under stirring,
Dominant wavelength 365nm irradiates 5~30 minutes under the ultraviolet light of 20~200W/cm of light intensity;Alkyl hydrosulfide is added, under stirring, in main wave
Long 365nm continues irradiation 5~30 minutes under the ultraviolet light of 20~200W/cm of light intensity;Reducing agent is added, is warming up to system micro- time
Stream reacts 2~4 hours, and filtering removes filtrate, filters out solid washes of absolute alcohol 5 times, dries in vacuum drying oven to perseverance
Weight, obtains graphene/POSS composite material.
It is furthermore preferred that the weight ratio of graphene oxide described in step S1 and alkyl mercaptoamine is 1:0.4~2.
Graphene oxide is that crystalline flake graphite is made using strong oxidizer oxidation, Hummers method or improvement Hummers legal system
Standby graphene oxide is the method that wherein reaction condition is comparatively gentle.
Periodical literature " Study on adsorption properties of the sulfhydrylation graphene to Pb in water (II) " (" chemistry notification " 2017 the 80th
Rolled up for the 4th 361-366 pages of phase) report the side that sulfhydryl modified graphene oxide is prepared using mercaptoethylmaine and graphite oxide alkene reaction
Method.
The Chinese invention of publication No. CN108084528A, which is applied for a patent, to be disclosed using sulfydryl-amino-compound and oxidation stone
The method that black alkene reaction prepares sulfhydrylation graphene.
It is furthermore preferred that the molal quantity of sulfydryl and octavinyl-POSS in sulfhydryl modified graphene oxide described in step S2
Mole ratio is 1~3:1.
Periodical literature " synthesis and characterization of eight vinyl polyhedral oligomeric silsesquioxanes " (" China Synthetic Rubber Industry " 2009
The 2nd 105-108 pages of the phase of volume 32 year) report vinyltrimethoxysilane eight ethylene of hydrolytic condensation preparation in acidic environment
The method of base POSS.
It is further preferred that the molal quantity of sulfydryl and mole of octavinyl-POSS in the sulfhydryl modified graphene oxide
Number is than being 2:1.
It is furthermore preferred that alkyl hydrosulfide described in step S2 is selected from positive stearylmercaptan, positive 16 mercaptan, positive tetradecanylthioalcohol, just
One or more of lauryl mercaptan and n octylmercaptan.
It is furthermore preferred that the molar ratio of octavinyl-POSS described in step S2 and alkyl hydrosulfide is 1:2~4.
It is furthermore preferred that reducing agent described in step S2 is selected from sodium borohydride, vitamin C, hydrazine hydrate, Dimethylhydrazine and Vitamin C
One or more of acid, the usage amount of the reducing agent are 2~3 times of sulfhydryl modified graphene oxide weight.
A kind of preparation method of modified polypropylene fiber described in any of the above-described embodiment, includes the following steps,
S3: according to parts by weight, by graphene described in 5~20 parts of any of the above-described embodiments/POSS composite material and
80~95 parts of PP GRANULESs carry out melt pelletization, obtain modified polypropylene agglomerate;
S4: according to parts by weight, by the modified polypropylene agglomerate and 50~98 parts of PP GRANULESs in 2~50 parts of step S3
Melt spinning is carried out, modified polypropylene fiber is obtained.
Application of the modified polypropylene fiber in weaving described in a kind of any of the above-described embodiment.
The present invention utilizes the epoxy group of surface of graphene oxide, carboxyl, hydroxyl isoreactivity group, using alkyl mercaptoamine
On amino and the epoxy group of surface of graphene oxide and carboxyl react, obtain sulfhydryl modified graphene oxide.Utilize second
The sulfydryl of alkenyl and sulfydryl-alkene clicking chemistry reaction, so that after sulfhydryl modified graphene oxide and octavinyl-POSS reaction, not
The vinyl continuation of reaction is reacted with alkyl hydrosulfide, and graphene/POSS composite material is obtained after redox graphene.Graphite
Alkene/POSS composite material due to being grafted with alkyl segment, improve with polyacrylic compatibility so that modified poly- third
Alkene fiber has preferable electric conductivity, thermal conductivity, ultraviolet-resistent property, washability and improves anti-flammability.
(3) beneficial effect
Compared to the prior art, the invention has the benefit that (1) provides the stone for being grafted with alkyl group on a kind of POSS
Black alkene/modified filler of the POSS composite material as polypropylene fibre;(2) graphene/POSS composite material is added to polypropylene
In there is preferable dispersibility, additive amount, which reaches, does not all influence mechanical property close to 10% (mass fraction);(3) stone is added
The modified polypropylene fiber obtained after black alkene/POSS composite material has preferable electric conductivity, thermal conductivity, ultraviolet-resistent property, washable
Property and improve anti-flammability.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, by embodiment to the present invention carry out into
One step elaborates, but is not intended to limit the present invention.
If not specified, the number in embodiment below is all parts by weight.
Prepare sulfhydryl modified graphene oxide
With stirring rod, thermometer and reflux condensing tube container in be added 1 part of Hummers method graphene oxide and
1000 parts of dehydrated alcohols, ultrasound 20 minutes, are added 0.4 part of mercaptoethylmaine and 0.2 part of EDC, the micro- reflux of system are warming up under stirring,
Reaction 2 hours, filtering remove filtrate, filter out solid washes of absolute alcohol 5 times, dry in vacuum drying oven to constant weight, obtain
Sulfhydryl modified graphene oxide 1.Titration is used to measure the content of sulfydryl in product as 0.13mol/100g.FT-IR analysis is aobvious
Show, product is in 1585cm-1Sharp middle Qiang Feng, be the characteristic absorption peak of-NHCO-, in 3410cm-1Broad peak, be-OH and-
The absorption overlap of peaks of NH- causes.
With stirring rod, thermometer and reflux condensing tube container in be added 10 parts of Hummers method graphene oxides and
1000 parts of dehydrated alcohols, ultrasound 30 minutes, are added 20 parts of mercaptopropylamines and 10 parts of EDC, the micro- reflux of system are warming up under stirring, instead
It answers 0.5 hour, filters, remove filtrate, filter out solid washes of absolute alcohol 5 times, dry in vacuum drying oven to constant weight, obtain
Sulfhydryl modified graphene oxide 2.Titration is used to measure the content of sulfydryl in product as 0.12mol/100g.
Prepare graphene/POSS composite material
5 parts of sulfhydryl modified graphene oxide 1 and 1000 part ethyl acetate are added in a reservoir, ultrasound 20 minutes is added 4.1
Part octavinyl-POSS and 0.04 part of dimethoxybenzoin, under stirring, at dominant wavelength 365nm, the ultraviolet light of light intensity 20W/cm
Irradiation 30 minutes;3.72 parts of n-octadecane base mercaptan are added, under stirring, at dominant wavelength 365nm, the ultraviolet light of light intensity 20W/cm
Continue irradiation 30 minutes;10 parts of hydrazine hydrates are added, are warming up to the micro- reflux of system, react 4 hours, filtering removes filtrate, filters out solid
Body is dried to constant weight in vacuum drying oven with washes of absolute alcohol 5 times, is obtained graphene/POSS composite material 1.FT-IR analysis
It has been shown that, product is in 1110cm-1There is a sharp strong peak, is the characteristic absorption peak of Si-O-Si on POSS, in 1630cm-1Have one
A weak absorption peak is the vinyl that unreacted is complete on POSS, 1585cm-1Sharp middle Qiang Feng, the feature for being-NHCO- inhales
Peak is received, in 3412cm-1Broad peak, cause for the absorption overlap of peaks of-OH and-NH-, in 1218cm-1There is a weak peak, is C-
The absorption peak of S-C, in 2570cm-1The absorption peak of sulfydryl is not belonged to nearby.
10 parts of sulfhydryl modified graphene oxide 1 and 1000 part ethyl acetate are added in a reservoir, ultrasound 20 minutes is added
8.2 parts of octavinyl-POSSs and 0.08 part of dimethoxybenzoin, under stirring, in dominant wavelength 365nm, light intensity 100W/cm's is ultraviolet
It is irradiated 15 minutes under light;3.94 parts of n-dodecyl mercaptans are added, under stirring, in dominant wavelength 365nm, the purple of light intensity 100W/cm
Continue irradiation 15 minutes under outer light;25 parts of sodium borohydrides are added, are warming up to the micro- reflux of system, react 3 hours, filtering removes filter
Liquid filters out solid washes of absolute alcohol 5 times, dries in vacuum drying oven to constant weight, obtains graphene/POSS composite material 2.
20 parts of sulfhydryl modified graphene oxide 2 and 1000 part ethyl acetate are added in a reservoir, ultrasound 30 minutes is added
7.6 parts of octavinyl-POSSs and 0.076 part of dimethoxybenzoin, under stirring, in dominant wavelength 365nm, light intensity 200W/cm's is ultraviolet
It is irradiated 5 minutes under light;4.64 parts of n octylmercaptans are added, under stirring, at dominant wavelength 365nm, the ultraviolet light of light intensity 200W/cm
Continue irradiation 5 minutes;60 parts of vitamin Cs are added, are warming up to the micro- reflux of system, react 2 hours, filtering removes filtrate, filters out solid
Body is dried to constant weight in vacuum drying oven with washes of absolute alcohol 5 times, is obtained graphene/POSS composite material 3.
Embodiment 1
5 parts of graphenes/POSS composite material 1 and 95 part PP GRANULES is subjected to melt pelletization, obtains modified polypropene
Master batch 1.
1 part of modified polypropylene agglomerate 1 and 29 part PP GRANULES is subjected to melt spinning, obtains modified polypropylene fiber 1.
Melt-spinning technology: 240 DEG C of spinning temperature, draw ratio 4, spinning speed 800m/min.
Embodiment 2
10 parts of graphenes/POSS composite material 2 and 90 part PP GRANULES is subjected to melt pelletization, obtains modified polypropene
Master batch 2.
5 parts of modified polypropylene agglomerate 2 and 95 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber 2.
Melt-spinning technology is same as Example 1.
Embodiment 3
15 parts of graphenes/POSS composite material 3 and 85 part PP GRANULES is subjected to melt pelletization, obtains modified polypropene
Master batch 3.
15 parts of modified polypropylene agglomerate 3 and 85 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
3.Melt-spinning technology is same as Example 1.
Embodiment 4
20 parts of graphenes/POSS composite material 1 and 80 part PP GRANULES is subjected to melt pelletization, obtains modified polypropene
Master batch 4.
5 parts of modified polypropylene agglomerate 4 and 95 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber 4.
Melt-spinning technology is same as Example 1.
Embodiment 5
20 parts of graphenes/POSS composite material 2 and 80 part PP GRANULES is subjected to melt pelletization, obtains modified polypropene
Master batch 5.
20 parts of modified polypropylene agglomerate 5 and 80 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
5.Melt-spinning technology is same as Example 1.
Embodiment 6
20 parts of graphenes/POSS composite material 3 and 80 part PP GRANULES is subjected to melt pelletization, obtains modified polypropene
Master batch 6.
48 parts of modified polypropylene agglomerate 6 and 52 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
6.Melt-spinning technology is same as Example 1.
Comparative example 1
10 parts of sulfhydrylation graphene oxide 1 and 90 part PP GRANULESs are subjected to melt pelletization, obtain modified polypropene mother
Grain 7.
10 parts of modified polypropylene agglomerate 7 and 90 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
7.Melt-spinning technology is same as Example 1.
Comparative example 2
10 parts of octavinyl-POSSs and 90 parts of PP GRANULESs are subjected to melt pelletization, obtain modified polypropylene agglomerate 8.
10 parts of modified polypropylene agglomerate 8 and 90 part PP GRANULESs are subjected to melt spinning, obtain modified polypropylene fiber
8.Melt-spinning technology is same as Example 1.
Performance test
Electric conductivity: referring to GB/T 12703.4-2010 " the 4th part of evaluation of textile antistatic property: resistivity ", test
The resistivity of sample to be tested.Concrete outcome is as shown in table 1.
Thermal conductivity: ASTM D1518-2014 method is referred to, the thermal coefficient of sample to be tested is tested.Concrete outcome such as 1 institute of table
Show.
Ultraviolet-resistent property: referring to GB/T 18830-2009 " evaluation of ultraviolet resistance of fabric ", sample to be tested is tested
Ultraviolet-resistent property.UPF value is higher, and uvioresistant performance is better.Concrete outcome is as shown in table 1.
Anti-flammability: referring to the resistance of GB/T 5454-1997 " textile combustion performance test oxygen index method " test sample to be tested
Combustion property.Oxygen index (OI) is higher, and anti-flammability is better.Concrete outcome is as shown in table 1.
Washability: by sample to be tested after standard wash 50 times, testing its electric conductivity and thermal conductivity, compare electric conductivity and
The variation of thermal conductivity.Concrete outcome is as shown in table 2.
1 sample to be tested the performance test results of table
As can be known from the results of Table 1, the modified polypropylene fiber that the present invention obtains has preferable electric conductivity, thermal conductivity, resistance
Combustion property, mechanical property and ultra-violet resistance.
2 sample to be tested washability test result of table
As can be known from the results of Table 2, modified polypropylene fiber of the invention has preferable washability, by 50 standards
After washing, resistivity improves an order of magnitude, and thermal coefficient changes less than 20%.
Therefore, the poly- third class fiber of modification of the invention has preferable thermal conductivity, electric conductivity, mechanical property, ultraviolet-resistent property
And washability, oxygen index (OI) with higher, it can be applied to some special workplaces.
It should be noted that embodiment disclosed above only embodies and illustrates technical solution of the present invention, rather than it is used to limit this
The protection scope of invention, although explaining in detail referring to preferred embodiment to the present invention, any those skilled in the art is answered
Work as understanding, modify within the scope of technical solution of the present invention or various change, equivalent replacement not departing from, this all should belong to
The protection scope of invention.
Claims (10)
1. a kind of modified polypropylene fiber, it is characterised in that: be made of by weight percentage following components, 0.1~10% graphite
Alkene/cage modle polysilsesquioxane composite material, 90~99.9% polypropylene.
2. modified polypropylene fiber according to claim 1, it is characterised in that: by following components group by weight percentage
At, 0.5~5% graphene/cage modle polysilsesquioxane composite material, 95~99.5% polypropylene.
3. modified polypropylene fiber according to claim 1 or 2, it is characterised in that: the poly- sesquialter silicon of graphene/cage modle
The preparation method of oxygen alkane composite material includes the following steps,
S1: according to parts by weight, being added to ultrasound 20~30 minutes in 1000 parts of dehydrated alcohols for 1~10 part of graphene oxide,
Addition general structure is HS (CH2)nNH2Alkyl mercaptoamine and 0.5 times of alkyl mercaptoamine weight of 1- (3- dimethylamino third
Base) -3- ethyl carbodiimide, it is warming up to the micro- reflux of system under stirring, reacts 0.5~2 hour, filtering removes filtrate, filters out solid
Body is dried to constant weight in vacuum drying oven with washes of absolute alcohol 5 times, is obtained sulfhydryl modified graphene oxide;Wherein n=2,3,
4;
S2: according to parts by weight, the sulfhydryl modified graphene oxide in 5~20 parts of step S1 is added to 1000 parts of ethyl acetate
Middle ultrasonic 20~30 minutes, eight ethenyl cage model polysilsesquioxanes and eight ethenyl cage model polysilsesquioxane weight are added
0.01 times of dimethoxybenzoin under stirring, irradiates 5~30 at dominant wavelength 365nm, the ultraviolet light of 20~200W/cm of light intensity
Minute;Alkyl hydrosulfide is added, under stirring, continues irradiation 5~30 at dominant wavelength 365nm, the ultraviolet light of 20~200W/cm of light intensity
Minute;Reducing agent is added, is warming up to the micro- reflux of system, reacts 2~4 hours, filtering removes filtrate, filters out solid with anhydrous second
Alcohol cleans 5 times, dries in vacuum drying oven to constant weight, obtains graphene/cage modle polysilsesquioxane composite material.
4. modified polypropylene fiber according to claim 3, it is characterised in that: graphene oxide described in step S1 and mercapto
The weight ratio of pheynylalkylamine is 1:0.4~2.
5. modified polypropylene fiber according to claim 3, it is characterised in that: sulfhydryl modified oxidation stone described in step S2
The mole ratio of the molal quantity of sulfydryl and eight ethenyl cage model polysilsesquioxanes is 1~3:1 in black alkene.
6. modified polypropylene fiber according to claim 3, it is characterised in that: alkyl hydrosulfide described in step S2 is selected from just
One or more of stearylmercaptan, positive 16 mercaptan, positive tetradecanylthioalcohol, n- dodecyl mereaptan and n octylmercaptan.
7. modified polypropylene fiber according to claim 3, it is characterised in that: eight ethenyl cage models described in step S2 are poly-
The molar ratio of silsesquioxane and alkyl hydrosulfide is 1:2~4.
8. modified polypropylene fiber according to claim 3, it is characterised in that: reducing agent described in step S2 is selected from boron hydrogen
Change one or more of sodium, vitamin C, hydrazine hydrate, Dimethylhydrazine and ascorbic acid, the usage amount of the reducing agent changes for sulfydryl
2~3 times of property graphene oxide weight.
9. a kind of preparation method of any one of claim 1-8 modified polypropylene fiber, it is characterised in that: including following step
Suddenly,
S3: according to parts by weight, the described in any item graphenes of 5~20 parts of claim 1-8/cage modle polysilsesquioxane is answered
Condensation material and 80~95 parts of PP GRANULESs carry out melt pelletization, obtain modified polypropylene agglomerate;
S4: according to parts by weight, by 2~50 parts of step S3 modified polypropylene agglomerate and 50~98 parts of PP GRANULESs carry out
Melt spinning obtains modified polypropylene fiber.
10. a kind of application of any one of claim 1-8 modified polypropylene fiber in weaving.
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