CN109943902A - A kind of modified polyester fiber and preparation method - Google Patents

A kind of modified polyester fiber and preparation method Download PDF

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CN109943902A
CN109943902A CN201910192596.2A CN201910192596A CN109943902A CN 109943902 A CN109943902 A CN 109943902A CN 201910192596 A CN201910192596 A CN 201910192596A CN 109943902 A CN109943902 A CN 109943902A
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polyester fiber
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polyester
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vinyl
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CN109943902B (en
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刘云剑
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FUJIAN GALAXY APPAREL Co Ltd
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FUJIAN GALAXY APPAREL Co Ltd
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Abstract

The present invention relates to the modification fields of polyester fiber, and in particular to a kind of modified polyester fiber and preparation method.The present invention is reacted by graphene oxide and containing vinyl silicane coupling agent, obtain vinyl modified graphene oxide, sulfydryl-alkene clicking chemistry is carried out with eight (3- mercaptopropyi) POSS again to react, it is restored after being reacted later with allyl alcohol, obtain hydroxyl modification POSS/ graphene composite material, ring-opening reaction is carried out in catalyst with 6-caprolactone, obtains polyester/graphite alkene/cage modle polysilsesquioxane particle.Polyester/graphite alkene/cage modle polysilsesquioxane particle and polyester slice carry out melt spinning, obtain modified polyester fiber.The modified polyester fiber that the present invention obtains has preferable electric conductivity, thermal conductivity, anti-flammability and mechanical property, can apply in weaving.

Description

A kind of modified polyester fiber and preparation method
Technical field
The present invention relates to the modification fields of polyester fiber, and in particular to a kind of modified polyester fiber and preparation method.
Background technique
Polyester fiber is commonly called as " terylene ", is that the polyester as made of organic dibasic acid and organic diol polycondensation is obtained through spinning The synthetic fibers arrived, abbreviation PET fiber.Its four wrinkle resistance of biggest advantage and conformality are fine, intensity with higher and bullet Property recovery capability, therefore use weaving is upper a large amount of.
As people's living standard is higher and higher, the requirement to dress is also higher and higher, and not only clothing color is various, and Require some special performances, such as antistatic property, ultraviolet-resistent property etc..Antistatic property is usually to be added in textile fabric Some antistatic agents or conductive agent, or in final finishing with some hydrophilic finishing agents, ultraviolet-resistent property is usually to weave Some anti ultraviolet agents are added in fiber or in final finishing with some finishing agents with uvioresistant function.It wherein will be antistatic The modifying agent such as agent, conductive agent or anti ultraviolet agent are added in fibre spinning molding, and modifying agent disperses in the fibre, and washability is good, It is able to maintain the more long functionality time.
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.
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.And dispersion of the graphene in fibre-forming polymer an important factor for being also an influence modified effect, if dispersion It is bad, it will lead to some performances decline of fiber instead.
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 polyester fibers, have and preferably lead Electrical property, thermal conductivity, mechanical strength and flame retardant property, and graphene/cage modle polysilsesquioxane composite material additive amount compared with (mass fraction is more than 5%, or even close to 10%) all with preferable mechanical property greatly.
It is another object of the present invention to provide a kind of preparation methods of modified polyester 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 polyester fiber is made of following raw material by weight percentage, 1~50% polyester/graphite alkene/POSS Particle and 50~99% polyester.
Preferably, by weight percentage, it is made of following raw material, 5~20% polyester/graphite alkene/POSS and 80~95% Polyester.
It is furthermore preferred that the preparation method of the polyester/graphite alkene/POSS particle 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 is added and contains vinyl silicane coupling agent, and the micro- reflux of system is warming up under stirring, reacts 1~2 hour, and filtering removes filtrate, It filters out solid washes of absolute alcohol 5 times, dries in vacuum drying oven to constant weight, obtain vinyl modified graphene oxide;
S2: according to parts by weight, the vinyl modified graphene oxide in 5~20 parts of step S1 is added to 1000 parts of second Eight (3- mercaptopropyi) cage modle polysilsesquioxanes (HS-POSS) and HS-POSS weight are added in ultrasound 20~30 minutes in acetoacetic ester 0.01 times of dimethoxybenzoin of amount, under stirring, irradiate 5 at dominant wavelength 365nm, the ultraviolet light of 20~200W/cm of light intensity~ 30 minutes;Allyl alcohol 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 hydroxyl modification POSS/ graphene composite material;
S3: according to parts by weight, the hydroxyl modification POSS/ graphene composite material in 1 part of step S2 is added to 5~50 In part 6-caprolactone, ultrasonic disperse 30 minutes, the dibutyl tin dilaurate of 6-caprolactone weight 0.1% is added, is risen after stirring evenly Temperature is reacted 2 hours to 70 DEG C, is warming up to 140 DEG C, is reacted 6 hours, is decompressed to -0.099MPa hereinafter, removing low-boiling-point substance, is cooled down, It is granulated, obtains polyester/graphite alkene/POSS particle.
It is furthermore preferred that being selected from vinyltriethoxysilane, vinyl containing vinyl silicane coupling agent described in step S1 One or more of trimethoxy silane, vinyl methyl dimethoxysilane and vinyl methyl diethoxy silane, institute It states graphene oxide and the weight ratio containing vinyl silicane coupling agent is 1:0.5~1.5.
It is furthermore preferred that the molal quantity and HS-POSS of vinyl modified graphene oxide medium vinyl described in step S2 Mole ratio is 1:1.
It is furthermore preferred that the molar ratio of HS-POSS described in step S2 and allyl alcohol is 1:8~10.
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 vinyl modified graphene oxide weight.
The preparation method of modified polyester fiber described in a kind of any of the above-described embodiment, according to parts by weight, by 1~50 part Polyester described in any of the above-described embodiment/POSS/ graphene particles and 50~99 parts of polyester slices carry out melt spinning, obtain To modified polyester fiber.
Application of the modified polyester 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 silicon containing vinyl Alkane coupling agent is reacted with the active group of surface of graphene oxide, obtains vinyl modified graphene oxide.Utilize ethylene The sulfydryl of base and sulfydryl-alkene clicking chemistry reaction, so that after vinyl modified graphene oxide and HS-POSS reaction, unreacted Sulfydryl continuation reacted with allyl alcohol, hydroxyl modification POSS/ graphene/composite material is obtained after redox graphene.It utilizes Hydroxyl on hydroxyl modification POSS/ graphene/composite material causes 6-caprolactone ring-opening polymerisation as initiator under catalyst, Obtain polyester/graphite alkene/POSS particle.Polyester/graphite alkene/POSS particle is preferable compatible since polyester and polyester fiber have Property, therefore graphene/POSS can be made preferably to be dispersed in polyester fiber, it obtains having preferably conductive, thermally conductive, washable, anti- Ultraviolet, flame retardant property modified polyester fiber.
(3) beneficial effect
Compared to the prior art, the invention has the benefit that (1) provide be grafted on a kind of POSS the polyester of polyester/ Graphene/modified material of the POSS composite material as polyester fiber;(2) polyester/graphite alkene/POSS composite material is added to poly- There is preferable dispersibility, additive amount, which reaches, does not all influence mechanical property close to 10% (mass fraction) in ester;(3) it adds The modified polyester fiber obtained after polyester/graphite alkene/POSS composite material have preferable electric conductivity, thermal conductivity, ultraviolet-resistent property, Washability and raising 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 vinyl modified graphene oxide
With stirring rod, thermometer and reflux condenser container in be added 1 part of Hummers method graphene oxide and 1000 parts of dehydrated alcohols, ultrasound 20 minutes, are added 0.5 part of vinyltrimethoxysilane, 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, are dried in 60 DEG C of vacuum drying ovens to constant weight, Obtain vinyl modified graphene oxide 1.Titration is used to measure product medium vinyl content as 0.204mol/100g.FT-IR Analysis, in 1080cm-1There is a high-intensitive spike, is the characteristic absorption peak of Si-O-Si, in 1607cm-1And 1441cm-1In Equicohesive spike is the characteristic absorption peak of vinyl.
With stirring rod, thermometer and reflux condenser container in be added 5 parts of Hummers method graphene oxides and 1000 parts of dehydrated alcohols, ultrasound 25 minutes, are added 5 parts of vinyltriethoxysilane, the micro- reflux of system are warming up under stirring, instead It answers 1.5 hours, filters, remove filtrate, filter out solid washes of absolute alcohol 5 times, dried in 60 DEG C of vacuum drying ovens to constant weight, Obtain vinyl modified graphene oxide 2.Titration is used to measure product medium vinyl content as 0.207mol/100g.FT-IR Analysis, in 1082cm-1There is a high-intensitive spike, is the characteristic absorption peak of Si-O-Si, in 1605cm-1And 1443cm-1In Equicohesive spike is the characteristic absorption peak of vinyl.
With stirring rod, thermometer and reflux condenser container in be added 10 parts of Hummers method graphene oxides and 1000 parts of dehydrated alcohols, ultrasound 30 minutes, are added 15 parts of vinyl methyl dimethoxysilanes, are warming up under stirring system micro- time Stream reacts 1 hour, and filtering removes filtrate, filters out solid washes of absolute alcohol 5 times, dries in 70 DEG C of vacuum drying ovens to perseverance Weight, obtains vinyl modified graphene oxide 3.Titration is used to measure product medium vinyl content as 0.206mol/100g.
Prepare hydroxyl modification POSS/ graphene composite material
5 parts of 1 and of vinyl modified graphene oxide are added in the container with stirring rod, thermometer and reflux condenser 1000 parts of ethyl acetate, ultrasound 20 minutes, are added 10.4 parts of HS-POSS and 0.1 part of dimethoxybenzoins, under stirring, in main wave Long 365nm irradiates 30 minutes under the ultraviolet light of light intensity 20W/cm;4.74 parts of allyl alcohols are added, under stirring, in dominant wavelength 365nm, Continue irradiation 30 minutes under the ultraviolet light of light intensity 20W/cm;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 washes of absolute alcohol 5 times, dries in 50 DEG C of vacuum drying ovens to constant weight, obtains hydroxyl and change Property POSS/ graphene composite material 1.FT-IR analysis shows that, product is in 1110cm-1There is a sharp strong peak, is on POSS The characteristic absorption peak of Si-O-Si, in 1630cm-1There is no absorption peak nearby, illustrates that the vinyl in reaction raw materials substantially reacts Completely, in 2570cm-1There is no absorption peak nearby, illustrates the sulfydryl substantially fully reacting on POSS, in 3420cm-1Broad peak, For the absorption peak of-OH, in 1218cm-1There is a weak peak, is the absorption peak of C-S-C.
10 parts of vinyl modified graphene oxides 2 are added in the container with stirring rod, thermometer and reflux condenser With 1000 parts of ethyl acetate, 21.03 parts of HS-POSS and 0.21 part of dimethoxybenzoins are added in ultrasound 25 minutes, under stirring, Dominant wavelength 365nm irradiates 5 minutes under the ultraviolet light of light intensity 200W/cm;10.82 parts of allyl alcohols are added, under stirring, in dominant wavelength 365nm continues irradiation 5 minutes under the ultraviolet light of light intensity 200W/cm;25 parts of sodium borohydrides are added, are warming up to the micro- reflux of system, instead It answers 3 hours, filters, remove filtrate, filter out solid washes of absolute alcohol 5 times, dry in 60 DEG C of vacuum drying ovens to constant weight, obtain To hydroxyl modification POSS/ graphene composite material 2.
20 parts of vinyl modified graphene oxides 3 are added in the container with stirring rod, thermometer and reflux condenser With 1000 parts of ethyl acetate, 41.86 parts of HS-POSS and 0.41 part of dimethoxybenzoins are added in ultrasound 30 minutes, under stirring, Dominant wavelength 365nm irradiates 15 minutes under the ultraviolet light of light intensity 100W/cm;23.93 parts of allyl alcohols are added, under stirring, in dominant wavelength 365nm continues irradiation 18 minutes under the ultraviolet light of light intensity 100W/cm;60 parts of vitamin Cs are added, are warming up to the micro- reflux of system, instead It answers 2 hours, filters, remove filtrate, filter out solid washes of absolute alcohol 5 times, dry in 60 DEG C of vacuum drying ovens to constant weight, obtain To hydroxyl modification POSS/ graphene composite material 3.
Prepare polyester/graphite alkene/POSS particle
1 part of hydroxyl modification POSS/ graphene composite material 1 is added in 5 parts of 6-caprolactones, ultrasonic disperse 60 minutes, 0.005 part of dibutyl tin dilaurate is added, 70 DEG C are warming up to after stirring evenly, reacts 2 hours, is warming up to 140 DEG C, reacts 6 hours, - 0.099MPa is decompressed to hereinafter, removing low-boiling-point substance, cooling, granulation obtains polyester/graphite alkene/POSS particle 1.By 1 part of polyester/ Graphene/POSS particle 1 is added in 100 parts of ethyl acetate ultrasonic disperse 30 minutes, forms the translucent liquid of homogeneity brownish black Body, filtering, filters out solid and is cleaned 3 times with ethyl acetate, dry in 50 DEG C of vacuum drying oven, obtain solid-like particle, Prove that polyester segment is to form chemical bonding with graphene/POSS.
1 part of hydroxyl modification POSS/ graphene composite material 2 is added in 20 parts of 6-caprolactones, ultrasonic disperse 60 minutes, 0.02 part of dibutyl tin dilaurate is added, 70 DEG C are warming up to after stirring evenly, reacts 2 hours, is warming up to 140 DEG C, reacts 6 hours, - 0.099MPa is decompressed to hereinafter, removing low-boiling-point substance, cooling, granulation obtains polyester/graphite alkene/POSS particle 2.
1 part of hydroxyl modification POSS/ graphene composite material 3 is added in 50 parts of 6-caprolactones, ultrasonic disperse 60 minutes, 0.05 part of dibutyl tin dilaurate is added, 70 DEG C are warming up to after stirring evenly, reacts 2 hours, is warming up to 140 DEG C, reacts 6 hours, - 0.099MPa is decompressed to hereinafter, removing low-boiling-point substance, cooling, granulation obtains polyester/graphite alkene/POSS particle 3.
Embodiment 1
1 part of polyester/graphite alkene/POSS particle 1 and 99 part polyester slice is subjected to melt spinning, obtains modified polyester fiber 1.Melt-spinning technology: 275 DEG C of spinning temperature, using side-blown cooling technique, temperature of drying is 18 DEG C, and cold air blast velocity is 0.4m/s is handled with the winding speed winding of 3000m/s, and stretching, thermal finalization, oils, coiling and molding at twisting, is obtained modified poly- Ester fiber 1.
Embodiment 2
10 parts of polyester/graphite alkene/POSS particle 2 and 90 part polyester slice is subjected to melt spinning, obtains modified poly ester fibre Dimension 2.Melt-spinning technology is consistent in embodiment 1.
Embodiment 3
20 parts of polyester/graphite alkene/POSS particle 3 and 80 part polyester slice is subjected to melt spinning, obtains modified poly ester fibre Dimension 3.Melt-spinning technology is consistent in embodiment 1.
Embodiment 4
30 parts of polyester/graphite alkene/POSS particle 1 and 70 part polyester slice is subjected to melt spinning, obtains modified poly ester fibre Dimension 4.Melt-spinning technology is consistent in embodiment 1.
Embodiment 5
40 parts of polyester/graphite alkene/POSS particle 2 and 60 part polyester slice is subjected to melt spinning, obtains modified poly ester fibre Dimension 5.Melt-spinning technology is consistent in embodiment 1.
Embodiment 6
50 parts of polyester/graphite alkene/POSS particle 3 and 50 part polyester slice is subjected to melt spinning, obtains modified poly ester fibre Dimension 6.Melt-spinning technology is consistent in embodiment 1.
Embodiment 7
50 parts of polyester/graphite alkene/POSS particle 1 and 50 part polyester slice is subjected to melt spinning, obtains modified poly ester fibre Dimension 7.Melt-spinning technology is consistent in embodiment 1.
Comparative example
The polyester fiber obtained using unmodified polyester slice melt spinning is comparative example.Melt-spinning technology and embodiment 1 In it is consistent.
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.
Mechanical property: referring to GB/T14344-2008 " chemical fiber filament Erichsen test method ", uses at 25 DEG C YG (B) 021H type chemical-fibres filaments electronics strength machine test sample to be tested of Wenzhou Darong Textile Instrument Co., Ltd.'s production breaks Resistance to spalling, elongation at break and initial modulus.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 polyester fiber that the present invention obtains has preferable electric conductivity, thermal conductivity, fire-retardant Property, ultra-violet resistance and mechanical strength.
2 sample to be tested washability test result of table
As can be known from the results of Table 2, modified polyester fiber of the invention has preferable washability, washes by 50 standards After washing, resistivity improves an order of magnitude, and thermal coefficient changes less than 0.1W/mK.
Therefore, modified polyester fiber of the invention have preferable thermal conductivity, electric conductivity, ultraviolet-resistent property, mechanical property and Washability, oxygen index (OI) with higher 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 (9)

1. a kind of modified polyester fiber, it is characterised in that: by weight percentage, be made of following raw material, 1~50% polyester/stone Black alkene/cage modle polysilsesquioxane particle and 50~99% polyester.
2. modified polyester fiber according to claim 1, it is characterised in that: by weight percentage, it is made of following raw material, 5~20% polyester/graphite alkene/cage modle polysilsesquioxane particle and 80~95% polyester.
3. modified polyester fiber according to claim 1 or 2, it is characterised in that: poly- times of the polyester/graphite alkene/cage modle The preparation method of half siloxane particles 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, It is added and contains vinyl silicane coupling agent, the micro- reflux of system is warming up under stirring, react 1~2 hour, filtering removes filtrate, filters out Solid is dried to constant weight in vacuum drying oven with washes of absolute alcohol 5 times, is obtained vinyl modified graphene oxide;
S2: according to parts by weight, the vinyl modified graphene oxide in 5~20 parts of step S1 is added to 1000 parts of acetic acid second Eight (3- mercaptopropyi) cage modle polysilsesquioxanes and poly- times of eight (3- mercaptopropyi) cage modles are added in ultrasound 20~30 minutes in ester The dimethoxybenzoin of half 0.01 times of siloxanes weight, under stirring, in dominant wavelength 365nm, the ultraviolet light of 20~200W/cm of light intensity Lower irradiation 5~30 minutes;Allyl alcohol is added, under stirring, continues at dominant wavelength 365nm, the ultraviolet light of 20~200W/cm of light intensity Irradiation 5~30 minutes;Reducing agent is added, is warming up to the micro- reflux of system, reacts 2~4 hours, filtering removes filtrate, filters out solid With washes of absolute alcohol 5 times, dries in vacuum drying oven to constant weight, obtain hydroxyl modification cage modle polysilsesquioxane/graphene Composite material;
S3: according to parts by weight, hydroxyl modification cage modle polysilsesquioxane/graphene composite material in 1 part of step S2 is added Enter into 5~50 parts of 6-caprolactones, ultrasonic disperse 30 minutes, the dibutyl tin dilaurate of 6-caprolactone weight 0.1% be added, It is warming up to 70 DEG C after stirring evenly, reacts 2 hours, is warming up to 140 DEG C, reacts 6 hours, is decompressed to -0.099MPa hereinafter, removing low boiling Object, it is cooling, it is granulated, obtains polyester/graphite alkene/cage modle polysilsesquioxane particle.
4. modified polyester fiber according to claim 3, it is characterised in that: be coupled described in step S1 containing vinyl silanes Agent is selected from vinyltriethoxysilane, vinyltrimethoxysilane, vinyl methyl dimethoxysilane and vinyl first One or more of base diethoxy silane, the graphene oxide and the weight ratio containing vinyl silicane coupling agent are 1:0.5~1.5.
5. modified polyester fiber according to claim 3, it is characterised in that: vinyl modified described in step S2 aoxidizes stone The mole ratio of the molal quantity of black alkene medium vinyl and eight (3- mercaptopropyi) cage modle polysilsesquioxanes is 1:1.
6. modified polyester fiber according to claim 3, it is characterised in that: (3- mercaptopropyi) cage eight described in step S2 The molar ratio of type polysilsesquioxane and allyl alcohol is 1:8~10.
7. modified polyester fiber according to claim 3, it is characterised in that: reducing agent described in step S2 is selected from hydroboration The usage amount of one or more of sodium, vitamin C, hydrazine hydrate, Dimethylhydrazine and ascorbic acid, the reducing agent changes for vinyl 2~3 times of property graphene oxide weight.
8. a kind of preparation method of any one of claim 1-7 modified polyester fiber, it is characterised in that: in parts by weight Meter, by 1~50 part of polyester of any of claims 1-7/cage modle polysilsesquioxane/graphene particles and 50~99 Part polyester slice carries out melt spinning, obtains modified polyester fiber.
9. a kind of application of any one of claim 1-7 modified polyester fiber in weaving.
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CN112870764A (en) * 2021-02-25 2021-06-01 福州大学 Functional micro-extraction probe with polysiloxane-modified graphene polymeric coating and preparation method thereof
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