CN103981591B - Antibacterial polyester fibre of a kind of copper modification and preparation method thereof - Google Patents
Antibacterial polyester fibre of a kind of copper modification and preparation method thereof Download PDFInfo
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- CN103981591B CN103981591B CN201410212281.7A CN201410212281A CN103981591B CN 103981591 B CN103981591 B CN 103981591B CN 201410212281 A CN201410212281 A CN 201410212281A CN 103981591 B CN103981591 B CN 103981591B
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Abstract
The invention discloses antibacterial polyester fibre of a kind of copper modification and preparation method thereof, copper particle containing 1 ~ 30wt% in described polyester fiber, preparation method comprises the following steps: (1) is mixed in BTA solution after being pulverized by metallic copper and soaks 20 ~ 90min, then the copper particle after immersion is dry, obtain the Modified Cu particle of surface anti-oxidation modification.(2) in polyester slice with high viscosity, add Modified Cu particle, melt pelletization obtains copper modified poly ester master batch.(3) mixed with polyester slice by copper modified poly ester master batch, it is even to add dispersant and mix lubricant, and under vacuum state, drying obtains blend spinning raw material.(4) by blend spinning raw material, be 270 ~ 295 DEG C of melt spinnings in melt temperature, the antibacterial polyester fibre of obtained copper modification.Compared to existing technology, be not only easier to apply, and production cost is lower, production technology is simple in the present invention.
Description
Technical field
The present invention relates to the preparing technical field of functional polyester fiber, be specifically related to a kind of technology of preparing of antibacterial polyester fibre of copper modification.
Background technology
In daily life, various textiles is the ground of the good existence of microorganism, is also the important propagating source of disease.Along with improving constantly of industrial boom and living standards of the people, antibacterial problem more and more causes the great attention of people.Anti-bacterial fibre greatly increases the surcharge of textiles, and while develop high-tech textiles, the textiles that exploitation has antibacterial functions is also one of important development direction.
The exploitation of existing antibacterial polyester fibers, adopt adds nano-metal-oxide class antiseptic more, obtains through co-blended spinning.In the synthesis of terephthalic acid 1,2-propylene glycol ester, Nano titanium dioxide (TiO2) 3 ~ 5% and cupric oxide (CuO) 3 ~ 6% is added as antiseptic as the number of patent application patent document that is 200910152448.4 discloses.Number of patent application is that the patent document of 200910196831.X discloses the complex antimicrobials and polyester blend that adopt nano zine oxide, titanium dioxide, obtained antibacterial polyester fibre.Number of patent application be 200910152476.6 patent document disclose and in the synthesis of polyester, to add Nano titanium dioxide 3 ~ 5% and silver oxide 3 ~ 6% as antiseptic, obtain antibacterial degradable polyester fibre.When adopting nano-metal-oxide in prior art as antiseptic, although metal oxide nano particles has the antibacterial effect of bigger serface and excellence, due to the relation in size, dispersion effect is poor, cause the antiseptic in anti-bacterial fibre to disperse uneven, thus affect antibacterial effect.Therefore, how to be effectively dispersed in each base material by metal oxide antiseptic, be the problem of puzzlement anti-bacterial fibre suitability for industrialized production always.
And when utilizing metal in prior art as preparation of antimicrobial fiber or antimicrobial yarn, plate metal film coatings on the surface at macromolecular fibre, as metal and metal mixture films thereof such as silver, platinum, copper, the fiber plating metallic film is twisted antibacterial yarn with other fiber again.Metal film coatings method production process is numerous and diverse, and cost is high, and meanwhile, metallic particles can detract gradually because of the generation of clean, wiping and collision, causes antibiotic effect to reduce gradually, shortens the term of validity of goods anti-microbial property.A kind of method is also had to be in macromolecular fibre, be mixed into part metals fiber, as metal fibres such as silver, copper.Because metal fibre price is high, make its cost high, application is also very limited.
Summary of the invention
First technical problem to be solved by this invention is: the deficiency existed for prior art, the antibacterial polyester fibre of the copper particle modification providing a kind of excellent antibacterial performance, production cost low.
Second technical problem to be solved by this invention is: the deficiency existed for prior art, a kind of preparation method of antibacterial polyester fibre of copper particle modification is provided, the method overcomes in prior art and use metal oxide as difficulties in dispersion during antiseptic and use metal coating and the high technical problem of metal fibre cost.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
An antibacterial polyester fibre for copper modification, the copper particle containing 1 ~ 30wt% in described polyester fiber, the antibacterial effect of described polyester fiber is: white reads coccus >=99%, Escherichia coli >=99%, staphylococcus aureus >=99%.
Preferably, median particle diameter D50≤0.5 μm of described copper particle.
As further preferred, the maximum gauge of described copper particle is 0.9 μm.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
A preparation method for the antibacterial polyester fibre of copper modification, comprises the following steps:
(1) the anti-oxidation modification of copper particle: metallic copper is pulverized the copper particle for median particle diameter D50≤0.5 μm, being mixed into concentration is mix in the BTA solution of 0.1 ~ 1.0g/l, and soak 20 ~ 90min, then the copper particle after immersion is dry at 80 ~ 150 DEG C, obtain the Modified Cu particle of surface anti-oxidation modification.
(2) copper modified poly ester master batch is prepared: in polyester slice with high viscosity, add the Modified Cu particle that step (1) obtains, the addition of described Modified Cu particle is 20 ~ 30wt% of described polyester slice, and melt pelletization obtains copper modified poly ester master batch.
(3) combination drying: the copper modified poly ester master batch obtain step (2) and polyester slice are according to the weight ratio of 5 ~ 100:95 ~ 0, add dispersant again and lubricant is uniformly mixed, dry more than 12h under vacuum state, obtains blend spinning raw material.
(4) melt spinning: by described blend spinning raw material, enter double screw extruder is 270 ~ 295 DEG C of melt spinnings in melt temperature, the antibacterial polyester fibre of obtained copper modification.
Preferably, in the mixed solution in step (1), the weight ratio of BTA and copper particle is 0.25 ~ 1:1.
Preferably, the maximum particle diameter of described copper particle is no more than 0.9 μm.
Preferably, in step (2), the viscosity >=0.8mpas of described polyester slice with high viscosity.
Preferably, in step (3), described dispersant is calgon, and the addition of described calgon is 0.2 ~ 0.5% of copper modified poly ester master batch and polyester slice mixed weight; Described lubricant is odium stearate, and the addition of described odium stearate is 0.1 ~ 0.3% of copper modified poly ester master batch and polyester slice mixed weight.
Wherein, the antibacterial polyester fibre of described copper modification is the short silk of polyester fiber or polyester filaments.
Owing to have employed technique scheme, the invention has the beneficial effects as follows:
Antibacterial polyester fibre of the present invention adopts copper minuteness particle as antiseptic, the antibacterial polyester fibre that prepare copper modification blended with polyester slice, the reunion that when to overcome in prior art using metal oxide as antiseptic, nanometer metal oxide particle brings, the problems such as difficulties in dispersion, and the cost being mixed into metal fibre technology in metal film coatings technology and macromolecular fibre is high, the drawback problems such as production process is numerous and diverse, the anti-microbial property of the anti-bacterial fibre prepared reaches: white reads coccus >=99%, Escherichia coli >=99%, the antibacterial effect of staphylococcus aureus >=99%, and there is promotion microcirculation function.
Compared to existing technology, be not only easier to apply, and production cost is lower, production technology is simple in the present invention.
Detailed description of the invention
Specifically the present invention is set forth below in conjunction with specific embodiment.
Embodiment 1
An antibacterial polyester fibre for copper modification, the copper particle containing 5wt% in described polyester fiber, the antibacterial effect of described polyester fiber is: white reads coccus >=99.1%, Escherichia coli >=99%, staphylococcus aureus >=99.5%.
Embodiment 2
A kind of antibacterial polyester fibre of copper modification, copper particle containing 10wt% in described polyester fiber, the median particle diameter D50 of described copper particle is 0.5 μm, and the antibacterial effect of described polyester fiber is: white reads coccus >=99.2%, Escherichia coli >=99.3%, staphylococcus aureus >=99.2%.
Embodiment 3
A kind of antibacterial polyester fibre of copper modification, copper particle containing 18wt% in described polyester fiber, the median particle diameter D50 of described copper particle is 0.3 μm, the maximum gauge of described copper particle is 0.6 μm, the antibacterial effect of described polyester fiber is: white reads coccus >=99.3%, Escherichia coli >=99.35%, staphylococcus aureus >=99.41%.
Embodiment 4
A kind of antibacterial polyester fibre of copper modification, copper particle containing 26wt% in described polyester fiber, the median particle diameter D50 of described copper particle is 0.45 μm, the maximum gauge of described copper particle is 0.9 μm, the antibacterial effect of described polyester fiber is: white reads coccus >=99.43%, Escherichia coli >=99.55%, staphylococcus aureus >=99.56%.
Embodiment 5
A preparation method for the antibacterial polyester fibre of copper modification, comprises the following steps:
(1) the anti-oxidation modification of copper particle: metallic copper is pulverized for median particle diameter D50 is the copper particle of 0.5 μm, being mixed into concentration is mix in the BTA solution of 0.5g/l, and soak 80min, then the copper particle after immersion is dry at 100 DEG C, obtain the Modified Cu particle of surface anti-oxidation modification.
(2) prepare copper modified poly ester master batch: in polyester slice with high viscosity, add the Modified Cu particle that step (1) obtains, the addition of described Modified Cu particle is the 22wt% of described polyester slice, and melt pelletization obtains copper modified poly ester master batch.
(3) combination drying: the copper modified poly ester master batch obtain step (2) and polyester slice according to the weight ratio of 50:50, then add dispersant and lubricant is uniformly mixed, and dry more than 12h under vacuum state, obtains blend spinning raw material.
(4) melt spinning: by described blend spinning raw material, enter double screw extruder is 275 DEG C of melt spinnings in melt temperature, cuts off and cool the antibacterial polyester fibre staple fibre of obtained copper modification.The antibacterial effect of the polyester fiber prepared is: white reads coccus >=99.53%, Escherichia coli >=99.45%, staphylococcus aureus >=99.51%.
Embodiment 6
A preparation method for the antibacterial polyester fibre of copper modification, comprises the following steps:
(1) the anti-oxidation modification of copper particle: metallic copper is pulverized for median particle diameter D50 is the copper particle of 0.45 μm, being mixed into concentration is mix in the BTA solution of 0.6g/l, in mixed solution, the weight ratio of BTA and copper particle is 0.35:1, soak 60min, then the copper particle after immersion is dry at 120 DEG C, obtain the Modified Cu particle of surface anti-oxidation modification.
(2) copper modified poly ester master batch is prepared: in the polyester slice with high viscosity of viscosity 0.8mpas, add the Modified Cu particle that step (1) obtains, the addition of described Modified Cu particle is the 25wt% of described polyester slice, and melt pelletization obtains copper modified poly ester master batch.
(3) combination drying: the copper modified poly ester master batch obtain step (2) and polyester slice are according to the weight ratio of 30:70, add sodium hexametaphosphate dispersant and lubricant stearic acid sodium again, the addition of calgon is 0.3% of copper modified poly ester master batch and polyester slice mixed weight, the addition of odium stearate is 0.15% of copper modified poly ester master batch and polyester slice mixed weight, be uniformly mixed, dry 48h under vacuum state, obtains blend spinning raw material.
(4) melt spinning: by described blend spinning raw material, enter double screw extruder is 270 ~ 295 DEG C of melt spinnings in melt temperature, the antibacterial polyester fibre long filament of obtained copper modification.The antibacterial effect of the polyester fiber prepared is: white reads coccus >=99.42%, Escherichia coli >=99.38%, staphylococcus aureus >=99.53%.
Embodiment 7
A preparation method for the antibacterial polyester fibre of copper modification, comprises the following steps:
(1) the anti-oxidation modification of copper particle: metallic copper is pulverized for median particle diameter D50 is the copper particle of 0.3 μm, the maximum particle diameter of copper particle 0.8 μm, being mixed into concentration is mix in the BTA solution of 1.0g/l, BTA solution is the ethanolic solution of BTA, in mixed solution, the weight ratio of BTA and copper particle is 0.85:1, soak 25min, then the copper particle after immersion is dry at 80 ~ 100 DEG C, obtain the Modified Cu particle of surface anti-oxidation modification.
(2) copper modified poly ester master batch is prepared: in the polyester slice with high viscosity of viscosity 0.8mpas, add the Modified Cu particle that step (1) obtains, the addition of described Modified Cu particle is the 28wt% of described polyester slice, and melt pelletization obtains copper modified poly ester master batch.
(3) combination drying: the copper modified poly ester master batch obtain step (2) and polyester slice are according to the weight ratio of 20:80, add sodium hexametaphosphate dispersant and lubricant stearic acid sodium again, the addition of calgon is 0.45% of copper modified poly ester master batch and polyester slice mixed weight, the addition of odium stearate is 0.25% of copper modified poly ester master batch and polyester slice mixed weight, be uniformly mixed, dry 32h under vacuum state, obtains blend spinning raw material.
(4) melt spinning: by described blend spinning raw material, enter double screw extruder is 280 ~ 295 DEG C of melt spinnings in melt temperature, cuts off the antibacterial polyester fibre staple fibre that granulation obtains copper modification.The antibacterial effect of the polyester fiber prepared is: white reads coccus >=99.45%, Escherichia coli >=99.47%, staphylococcus aureus >=99.42%.
Embodiment 8
A preparation method for the antibacterial polyester fibre of copper modification, comprises the following steps:
(1) the anti-oxidation modification of copper particle: metallic copper is pulverized for median particle diameter D50 is the copper particle of 0.4 μm, the maximum particle diameter of copper particle 0.7 μm, being mixed into concentration is mix in the BTA solution of 0.5g/l, in mixed solution, the weight ratio of BTA and copper particle is 0.5:1, soak 50min, then the copper particle after immersion is dry at 120 ~ 130 DEG C, obtain the Modified Cu particle of surface anti-oxidation modification.
(2) copper modified poly ester master batch is prepared: in the polyester slice with high viscosity of viscosity 0.8mpas, add the Modified Cu particle that step (1) obtains, the addition of described Modified Cu particle is the 30wt% of described polyester slice, and melt pelletization obtains copper modified poly ester master batch.
(3) combination drying: the copper modified poly ester master batch obtain step (2) and polyester slice are according to the weight ratio of 10:90, add sodium hexametaphosphate dispersant and lubricant stearic acid sodium again, the addition of calgon is 0.25% of copper modified poly ester master batch and polyester slice mixed weight, the addition of odium stearate is 0.15% of copper modified poly ester master batch and polyester slice mixed weight, be uniformly mixed, dry 24h under vacuum state, obtains blend spinning raw material.
(4) melt spinning: by described blend spinning raw material, enter double screw extruder is 275 ~ 285 DEG C of melt spinnings in melt temperature, cuts off the antibacterial polyester fibre staple fibre that granulation obtains copper modification.The antibacterial effect of the polyester fiber prepared is: white reads coccus >=99.19%, Escherichia coli >=99.25%, staphylococcus aureus >=99.36%.
Claims (5)
1. a preparation method for the antibacterial polyester fibre of copper modification, is characterized in that comprising the following steps:
(1) the anti-oxidation modification of copper particle: metallic copper is pulverized the copper particle for median particle diameter D50≤0.5 μm, being mixed into concentration is mix in the BTA solution of 0.1 ~ 1.0g/l, and soak 20 ~ 90min, then the copper particle after immersion is dry at 80 ~ 150 DEG C, obtain the Modified Cu particle of surface anti-oxidation modification;
(2) copper modified poly ester master batch is prepared: in polyester slice with high viscosity, add the Modified Cu particle that step (1) obtains, the addition of described Modified Cu particle is 20 ~ 30wt% of described polyester slice, and melt pelletization obtains copper modified poly ester master batch;
(3) combination drying: the copper modified poly ester master batch obtain step (2) and polyester slice are according to the weight ratio of 5 ~ 100:95 ~ 0, add dispersant again and lubricant is uniformly mixed, dry more than 12h under vacuum state, obtains blend spinning raw material; Described dispersant is calgon, and the addition of described calgon is 0.2 ~ 0.5% of copper modified poly ester master batch and polyester slice mixed weight; Described lubricant is odium stearate, and the addition of described odium stearate is 0.1 ~ 0.3% of copper modified poly ester master batch and polyester slice mixed weight;
(4) melt spinning: by described blend spinning raw material, enter double screw extruder is 270 ~ 295 DEG C of melt spinnings in melt temperature, the antibacterial polyester fibre of obtained copper modification.
2. the preparation method of the antibacterial polyester fibre of a kind of copper modification as claimed in claim 1, is characterized in that: in the mixed solution in step (1), the weight ratio of BTA and copper particle is 0.25 ~ 1:1.
3. the preparation method of the antibacterial polyester fibre of a kind of copper modification as claimed in claim 1, it is characterized in that: in step (1), the maximum particle diameter of described copper particle is no more than 0.9 μm.
4. the preparation method of the antibacterial polyester fibre of a kind of copper modification as claimed in claim 1, is characterized in that: in step (2), the viscosity >=0.8mPa ﹒ s of described polyester slice with high viscosity.
5. the preparation method of the antibacterial polyester fibre of a kind of copper modification as described in claim as arbitrary in Claims 1-4, is characterized in that: the antibacterial polyester fibre of described copper modification is the short silk of polyester fiber or polyester filaments.
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| WO2018017147A1 (en) * | 2016-07-19 | 2018-01-25 | Cupron Inc. | Processes for producing an antimicrobial masterbatch and products therefrom |
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