CN107151829A - A kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene - Google Patents

A kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene Download PDF

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Publication number
CN107151829A
CN107151829A CN201710343974.3A CN201710343974A CN107151829A CN 107151829 A CN107151829 A CN 107151829A CN 201710343974 A CN201710343974 A CN 201710343974A CN 107151829 A CN107151829 A CN 107151829A
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China
Prior art keywords
terylene
graphene
automatically cleaning
prepared
composite fibre
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CN201710343974.3A
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Chinese (zh)
Inventor
李林泽
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Nantong Kai Da Textile Co Ltd
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Nantong Kai Da Textile Co Ltd
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Priority to CN201710343974.3A priority Critical patent/CN107151829A/en
Publication of CN107151829A publication Critical patent/CN107151829A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/106Radiation shielding agents, e.g. absorbing, reflecting agents
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters

Abstract

The invention provides a kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene, terephthalic acid (TPA) is mixed with ethylene glycol, slurry is prepared;Graphite oxide prepared by improved Hummers methods is added in distilled water, ultrasound, obtains graphene oxide dispersion;The graphene oxide dispersion is added in the slurry, magnetic agitation, TiO2 colloidal sols is added while stirring, then composite fibre is obtained through dry spinning;The composite fibre is reduced with hydroiodic acid, then by the aqueous solution containing aliphatic diamine chain extender, cleaning is dried, obtains flexible terylene graphene composite fibre;Twisting, weaving obtain antibacterial uvioresistant automatically cleaning and are combined work(type terylene.Terylene prepared by the inventive method has excellent anti-microbial property, uv resistance energy and self-cleaning performance etc., and good application prospect is shown in function textile field.

Description

A kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene
Technical field
The invention belongs to textile technology field, and in particular to a kind of preparation side of antibacterial uvioresistant automatically cleaning composite-type terylene Method.
Background technology
In daily life, clothes can be stained with the spots such as oil, coffee, dust unavoidably.These spots are the normal of influence clothes Use, the environment of breeding is also provided for microorganism.So with the quickening pace of modern life, and pursue wanting for high-quality life Ask, the textile with automatical cleaning ability arises at the historic moment.
The physical and mechanical properties of polyester fiber such as strength, wearability, resilience and dimensional stability can preferably be met respectively The need for planting purposes.But polyester fiber is a kind of typical hydrophobic fibre, regain only has 0.4%, is used as skintight suit material Material, its snugness of fit is very poor, in high humidity, the condition of high temperature, and the clothes that people wear synthetic fibers have feeling of oppression and heat, and mood is tired of Hot-tempered uneasiness;Under humid tropical condition, human body increases with check room frictional force, and sense of heaviness increase, psychology and physiological change to people are produced Raw not very big influence.Meanwhile, polyester fiber hydrophily is very poor, also carrys out a series of problems to woven strip.Such as easy accumulation electrostatic, easily Inhale dust, go the stain difficulty etc. that degreases.
So-called graphene textile, refers to that grapheme material is effectively combined with flat textile product, is keeping textile every While basic performance, with graphene is a certain or textile product of several peculiar properties.Graphene textile is conductive, anti- There is huge application prospect in the fields such as radiation, UV resistance, thermoelectricity, special protection and smart fabric, at present, graphene textile Preparation method mainly includes directly preparation method and finishing method.Research on graphene fiber material is concentrated mainly on graphene The preparation of fiber and the mechanical property for how improving graphene fiber, by the excellent electricity of graphene nano lamella, calorifics and Optical property assigns macroscopical graphene fiber, and less on the research of graphene fiber spinnability.The graphene prepared Although fiber excellent combination property, fiber spinnability is poor, limits graphene fiber in civilian textile garment field Further develop.
At present, the method for function textile is prepared by blending and intertexture in textile industry extensive use, such as in the market Common stockinette and exposure suit etc., and prepare graphene through spinning and weaving on graphene fiber both at home and abroad and knit The research of thing is still rarely reported.Although graphene fiber preparation method is various, graphene fiber mechanical performance and feature are excellent, But, the spinnability of the graphene fiber prepared is poor, limits it in tradition spinning and the application in weaving field.
Therefore, it is necessary to improve the method researched and developed at present terylene being combined Self-cleaning fabric with graphene, terylene is lifted Performance, should effectively improve automatically cleaning effect, ensure environmental protection again, it is harmless.
The content of the invention
Technical problem:It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of antibacterial uvioresistant from clear The preparation method of clean composite-type terylene, lifts the performance of terylene, both effective to improve automatically cleaning effect, ensures environmental protection again, It is harmless.
Technical scheme:To achieve the above object, the present invention provides following technical scheme:
A kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene of the present invention, it is concretely comprised the following steps:
The first step:Terephthalic acid (TPA) is mixed with ethylene glycol, slurry is prepared;
Second step:Graphite oxide prepared by improved Hummers methods is added in distilled water, ultrasound, obtains aoxidizing stone Black alkene dispersion liquid;The concentration of graphene oxide dispersion is 10~20mg/mL;
3rd step:Graphene oxide dispersion obtained by second step is added into the first step to obtain in slurry, magnetic agitation, side Stir side and add TiO2 colloidal sols, stir 8-15 hours, then composite fibre is obtained through dry spinning;The graphite oxide, to benzene two The mol ratio of formic acid, ethylene glycol and TiO2 colloidal sols is (0.55-0.75):(4.0-4.45):(5.80-9.75):(0.2-0.3);
4th step:The composite fibre that 3rd step is obtained reduces 0.5~1h with hydroiodic acid, then by expanding containing aliphatic diamine The aqueous solution of chain agent, cleaning, dries, obtains flexible terylene-graphene composite fibre;Wherein, the quality of hydroiodic acid is dense Spend for 55%;
5th step:The terylene that 4th step is obtained-graphene composite fibre twisting carries out weaving processing and obtains the anti-purple of antibacterial Outer automatically cleaning is combined work(type terylene.
Heretofore described TiO2 colloidal sols are prepared using following methods:
Mass fraction is mixed for 70%-99% tetraisopropyl titanate, diethanol amine and absolute ethyl alcohol, stirred at room temperature 0.5-1.5 hours, volume fraction is then added as 60-90% alcohol using 2~3 drops/sec of speed again, 0.5- is stirred at room temperature 1.5 hours, form TiO2 colloidal sols.
Preferably, the mol ratio of the graphite oxide, terephthalic acid (TPA), ethylene glycol and TiO2 colloidal sols is (0.55-0.75): (5.80-5.85):(0.2-0.3)。
Preferably, the time ultrasonic in the second step is 3~5h.
Beneficial effect:Compared with prior art, the beneficial effects of the invention are as follows:
(1) the inventive method by graphene powder by being prepared into graphene oxide dispersion, and is added to terylene spinning In stoste, make modified terylene-graphene composite fibre that there is the special performance of two kinds of materials of graphene and terylene, can be very well Ground improves the mechanical property and heat resistance of terylene-graphene composite fibre, while graphene dispersing solution can be with the ester in terylene Base is had an effect, promote it is organic with it is inorganic between crosslinking, improve inorganic material dispersiveness in the composite.
(2) terylene prepared by the inventive method, being handled using TiO2 colloidal sols increases the functional group of fiber surface, strengthens nanometer The binding strength of particle and fiber, improves the automatically cleaning efficiency and automatically cleaning persistence of fabric.And because of graphene, TiO2 colloidal sols Adding has excellent anti-microbial property, uv resistance energy and self-cleaning performance etc., and both, which combine, makes fabric prolonged endurable, in function Textile field shows good application prospect.
(3) terylene prepared by the inventive method outstanding toughness is kept while rigidity is significantly reduced, it is tearing strength, anti- Edge-rolling and self-cleaning performance.Using the inventive method can prepare high-tech, high antibiotic property pure cotton fabric, expanded graphite Development field of the alkene in textile limit.
Embodiment
In order to deepen the understanding of the present invention, with reference to embodiment, the invention will be further described, and the embodiment is only For explaining the present invention, it is not intended to limit the scope of the present invention..
TiO in the present invention2The preparation of colloidal sol:Tetraisopropyl titanate, 4ml diethanol amine by 8ml mass fractions for 97% With the mixing of 24ml absolute ethyl alcohols, stirred 1 hour, then added again with 2 drops/sec of speed with 800rmp mixing speed at room temperature 14ml volume fraction is 75% alcohol, and the TiO for forming stable transparent for 1 hour is stirred at room temperature2Colloidal sol;
Embodiment 1
The first step:Slurry is prepared first:By terephthalic acid (TPA) and ethylene glycol according to 4.0:5.80 mol ratio is mixed, Prepare slurry;
Second step:Prepare graphene oxide dispersion:At room temperature, the oxygen prepared with improved Hummers methods is weighed Graphite 200mg, is placed in 100mL beaker, then adds deionized water 20mL and is made into the dispersion liquid that concentration is 10mg/mL, Then it is graphene oxide beaker to be put into ultrasonic pond and handle 3h by graphite oxide stripping, obtains dispersed graphite oxide Alkene solution;
3rd step:Graphene oxide dispersion obtained by second step is added into the first step to obtain in slurry, magnetic agitation, side Stir side and add TiO2Colloidal sol, is stirred 8 hours, then obtain composite fibre through dry spinning;The graphite oxide, terephthaldehyde Acid, ethylene glycol and TiO2The mol ratio of colloidal sol is 0.55:4.0:5.80:0.2;
4th step:The composite fibre that 3rd step is obtained reduces 0.5h with hydroiodic acid, then by containing aliphatic diamine chain extension The aqueous solution of agent, cleaning, dries, obtains flexible terylene-graphene composite fibre;Wherein, the mass concentration of hydroiodic acid For 55%;
5th step:The terylene that 4th step is obtained-graphene composite fibre twisting carries out weaving processing and obtains the anti-purple of antibacterial Outer automatically cleaning is combined work(type terylene.
The compound work(type terylene fracture strength of antibacterial uvioresistant automatically cleaning has reached 24.5 g deniers in the present embodiment, and fracture is stretched Long rate has reached 70, and in mass loss 10%, corresponding temperature has reached 418 DEG C.
Antibacterial uvioresistant automatically cleaning in the present embodiment is combined work(type terylene and presses GB/T 20944-2007 standards, with absorption Method is tested the bacteriostasis rate of sample, bacteriostasis rate>99.9%.UPF UPF>90, and UVA transmitance T (UVA) AV < 5%.
Embodiment 2
The first step:Slurry is prepared first:By terephthalic acid (TPA) and ethylene glycol according to 4.0:9.75 mol ratio is mixed, Prepare slurry;
Second step:Prepare graphene oxide dispersion:At room temperature, the oxygen prepared with improved Hummers methods is weighed Graphite 200mg, is placed in 100mL beaker, then adds deionized water 20mL and is made into the dispersion liquid that concentration is 10mg/mL, Then it is graphene oxide beaker to be put into ultrasonic pond and handle 4h by graphite oxide stripping, obtains dispersed graphite oxide Alkene solution;
3rd step:Graphene oxide dispersion obtained by second step is added into the first step to obtain in slurry, magnetic agitation, side Stir side and add TiO2Colloidal sol, is stirred 10 hours, then obtain composite fibre through dry spinning;The graphite oxide, terephthaldehyde Acid, ethylene glycol and TiO2The mol ratio of colloidal sol is 0.65:4.35:6.95:0.25;
4th step:The composite fibre that 3rd step is obtained reduces 1h with hydroiodic acid, then by containing aliphatic diamine chain extender The aqueous solution, cleaning, dry, obtain flexible terylene-graphene composite fibre;Wherein, the mass concentration of hydroiodic acid is 55%;
5th step:The terylene that 4th step is obtained-graphene composite fibre twisting carries out weaving processing and obtains the anti-purple of antibacterial Outer automatically cleaning is combined work(type terylene.
The compound work(type terylene fracture strength of antibacterial uvioresistant automatically cleaning has reached 35.5 g deniers in the present embodiment, and fracture is stretched Long rate has reached 90%, and in mass loss 10%, corresponding temperature has reached 450 DEG C.
Antibacterial uvioresistant automatically cleaning in the present embodiment is combined work(type terylene and presses GB/T 20944-2007 standards, with absorption Method is tested the bacteriostasis rate of sample, bacteriostasis rate>99.9%.UPF UPF>91, and UVA transmitance T (UVA) AV < 5%.
Embodiment 3
The first step:Slurry is prepared first:By terephthalic acid (TPA) and ethylene glycol according to 4.45:8.75 mol ratio is mixed Close, prepare slurry;
Second step:Prepare graphene oxide dispersion:At room temperature, the oxygen prepared with improved Hummers methods is weighed Graphite 200mg, is placed in 100mL beaker, then adds deionized water 20mL and is made into the dispersion liquid that concentration is 10mg/mL, Then it is graphene oxide beaker to be put into ultrasonic pond and handle 4h by graphite oxide stripping, obtains dispersed graphite oxide Alkene solution;
3rd step:Graphene oxide dispersion obtained by second step is added into the first step to obtain in slurry, magnetic agitation, side Stir side and add TiO2Colloidal sol, is stirred 15 hours, then obtain composite fibre through dry spinning;The graphite oxide, terephthaldehyde Acid, ethylene glycol and TiO2The mol ratio of colloidal sol is 0.65:4.35:6.95:0.25;
4th step:The composite fibre that 3rd step is obtained reduces 1h with hydroiodic acid, then by containing aliphatic diamine chain extender The aqueous solution, cleaning, dry, obtain flexible terylene-graphene composite fibre;Wherein, the mass concentration of hydroiodic acid is 55%;
5th step:The terylene that 4th step is obtained-graphene composite fibre twisting, weaving obtain antibacterial uvioresistant automatically cleaning Compound work(type terylene.
The compound work(type terylene fracture strength of antibacterial uvioresistant automatically cleaning has reached 35 g deniers, extension at break in the present embodiment Rate has reached 80%, and in mass loss 10%, corresponding temperature has reached 450 DEG C.
Antibacterial uvioresistant automatically cleaning in the present embodiment is combined work(type terylene and presses GB/T 20944-2007 standards, with absorption Method is tested the bacteriostasis rate of sample, bacteriostasis rate>99.9%.UPF UPF>90, and UVA transmitance T (UVA) AV < 5%.
Terylene nanometer composite material prepared by the present invention has excellent mechanical property and heat resistance, and fracture strength reaches To 24.5~35.5 g deniers, elongation at break has reached 70~90%, and in mass loss 10%, corresponding temperature reaches 418~450 DEG C, the application of terylene is widened.

Claims (4)

1. a kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene, it is characterised in that:It is concretely comprised the following steps:
The first step:Terephthalic acid (TPA) is mixed with ethylene glycol, slurry is prepared;
Second step:Graphite oxide prepared by improved Hummers methods is added in distilled water, ultrasound, obtains graphene oxide Dispersion liquid;The concentration of graphene oxide dispersion is 10~20mg/mL;
3rd step:Graphene oxide dispersion obtained by second step is added into the first step to obtain in slurry, magnetic agitation, side stirring Side adds TiO2Colloidal sol, is stirred 8-15 hours, then obtain composite fibre through dry spinning;The graphite oxide, terephthalic acid (TPA), Ethylene glycol and TiO2The mol ratio of colloidal sol is (0.55-0.75):(4.0-4.45):(5.80-9.75):(0.2-0.3);
4th step:The composite fibre that 3rd step is obtained reduces 0.5~1h with hydroiodic acid, then by containing aliphatic diamine chain extender The aqueous solution, cleaning, dry, obtain flexible terylene-graphene composite fibre;Wherein, the mass concentration of hydroiodic acid is 55%;
5th step:The terylene that 4th step is obtained-graphene composite fibre twisting carries out weaving processing and obtains antibacterial uvioresistant certainly The compound work(type terylene of cleaning.
2. the preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene according to claim 1, it is characterised in that described TiO2Colloidal sol is prepared using following methods:
Mass fraction is mixed for 70%-99% tetraisopropyl titanate, diethanol amine and absolute ethyl alcohol, 0.5- is stirred at room temperature 1.5 hours, alcohol of the volume fraction as 60-90% is then added using 2 ~ 3 drops/sec of speed again, 0.5-1.5 is stirred at room temperature small When, form TiO2Colloidal sol.
3. the preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene according to claim 1, it is characterised in that described Graphite oxide, terephthalic acid (TPA), ethylene glycol and TiO2The mol ratio of colloidal sol is (0.55-0.75):(5.80-5.85):(0.2- 0.3)。
4. the preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene according to claim 1, it is characterised in that described The ultrasonic time is 3~5h in second step.
CN201710343974.3A 2017-05-16 2017-05-16 A kind of preparation method of antibacterial uvioresistant automatically cleaning composite-type terylene Pending CN107151829A (en)

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CN108085770A (en) * 2017-12-06 2018-05-29 胡旺 A kind of antibacterial polyester fiber of photocatalysis and preparation method thereof
CN108409951A (en) * 2018-01-23 2018-08-17 浙江省现代纺织工业研究院 A kind of preparation method of function and service PTA
CN108866673A (en) * 2018-05-28 2018-11-23 泽塔纳米科技(苏州)有限公司 A kind of haze fiber and preparation method thereof with photocatalysis effect

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN108085770A (en) * 2017-12-06 2018-05-29 胡旺 A kind of antibacterial polyester fiber of photocatalysis and preparation method thereof
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Application publication date: 20170912