CN110230119A - A kind of preparation method of antibiotic polyester fiber - Google Patents

A kind of preparation method of antibiotic polyester fiber Download PDF

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Publication number
CN110230119A
CN110230119A CN201910598686.1A CN201910598686A CN110230119A CN 110230119 A CN110230119 A CN 110230119A CN 201910598686 A CN201910598686 A CN 201910598686A CN 110230119 A CN110230119 A CN 110230119A
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China
Prior art keywords
silver powder
polyester fiber
terylene
added
antibiotic polyester
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Pending
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CN201910598686.1A
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Chinese (zh)
Inventor
魏丽娟
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Qingdao Yinyuan Textile Technology Co Ltd
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Qingdao Yinyuan Textile Technology Co Ltd
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Priority to CN201910598686.1A priority Critical patent/CN110230119A/en
Publication of CN110230119A publication Critical patent/CN110230119A/en
Pending legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/103—Agents inhibiting growth of microorganisms
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent 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
    • D01F6/92—Monocomponent 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 belongs to chemical fibre processing technique fields, and in particular to a kind of preparation method of antibiotic polyester fiber, comprising the following steps: (1) carry out cladding processing to silver powder, used silver powder partial size is 1-15 microns；(2) it is dried, terylene chips is dried using vacuum oven, drying temperature is set as 100 DEG C, makes the water content 110ppm of terylene chips；(3) prepared by antibacterial functions particle, and the terylene particle of doping silver powder is made；(4) spinning；(5) it post-processes: long filament obtained is subjected to drawing-off, winding and doffing.By having carried out cladding processing to the silver powder used, reduce the reunion of silver powder, make to produce that polyester fiber antibacterial effect is more preferable, and the silver powder in polyester fiber is not easily to fall off.

Description

A kind of preparation method of antibiotic polyester fiber
Technical field:
The invention belongs to chemical fibre processing technique fields, and in particular to a kind of preparation method of antibiotic polyester fiber utilizes silver The characteristic of ion sterilizing prepares the polyester fiber with antibacterial functions.
Background technique:
Polyester fiber has many advantages, such as high-strength, Gao Mo, high-elastic and good conformality and heat resistance, it has also become purposes is most Extensively, the maximum fiber species of consumption.Due to good wearability, polyester fiber is widely used in garment industry.With Social development and the improvement of people's living standards, traditional textile garment can not meet what people wore daily life It is required that.Therefore, functional textile garment just comes into being in recent years.The textile with antibacterial functions is worn, people can be made Trip and activity it is safer, people also increasingly pay close attention to the anti-microbial property of clothes.
In research both domestic and external, using it is most be the doping nano-Ag into textile fabric.Application No. is 201710710557.8 Chinese invention patent discloses a kind of processing technology of long acting antibiotic polyester filament, including following step It is rapid: a, thermoplastic polyurethane to be sliced after cleaned drying to mix to be added in screw extruder with antibacterial agent and melted, be kneaded； B, the metering section of extruder or after extruder, into crosslinking agent is added before mixer；C, melt-spun material through spinneret spray, Spinning and coiling and molding, finally obtain finished product.The technological process of production are as follows: slice cleaning-drying-extrusion-mixing-spinneret- Drawing-off is-cooling-oil-to wind.Antibacterial agent is silver powder, and silver powder is nano-scale silver powder.Application No. is 201310088508.7 Chinese invention patent discloses a kind of production method of anti-bacterial fibre, includes the following steps: A, self-control antibacterial matrices comprising: Nano-silver powder is distributed in solvent, polypropylene chip is added after being uniformly dispersed and is made it dissolve；It is heated to reflux polypropylene/Nano silver System, the solvent in removal system are pulverized after dry；Polypropylene/Nano silver powder and resin are mixed, squeezed by screw rod Out, polypropylene antibacterial master batch is prepared；B, antibacterial matrices made from step A are mutually mixed by 2-10% with fibrous raw material, passes through high speed Batch mixer mixing, squeezes out wire drawing, obtains anti-bacterial fibre.The above technologic material uses nano silver, although this technique plays Antibacterial effect, but be likely to cause falling off for nano silver simultaneously in the dress and washing process for being made into clothes, with skin contact Harm is generated to human body afterwards.Since the partial size of nano-silver powder is smaller, it is easier to enter human body, when contacting a large amount of nano silver particles There is a possibility that causing damages to liver, and studies have shown that nano silver has toxicity to many aquatiles, and can be in food chain Middle accumulation.Meanwhile being added that the fiber of the nano silver nano silver after multiple washing is easy to fall off, and anti-microbial property, which has, significantly to drop It is low.
Summary of the invention:
It is an object of the invention to overcome disadvantage of the existing technology, for the weaving of doping nano-Ag in the prior art Fiber harm health and environment and the unabiding disadvantage of anti-microbial property, under the premise of keeping polyester fiber excellent mechanical performances, A kind of preparation method of antibiotic polyester fiber is sought in design, and polyester fiber is made to have anti-microbial property and Durability of antimicrobial effect.
In order to achieve the above-mentioned object of the invention, the preparation method of antibiotic polyester fiber of the present invention, comprising the following steps:
(1) cladding processing is carried out to silver powder, used silver powder partial size is 1-15 microns；
(2) it is dried: terylene chips being dried using vacuum oven, drying temperature is set as 100 DEG C, makes to wash The water content of synthetic fibre slice is in 110ppm；
(3) prepared by antibacterial functions particle: the silver powder using the addition of output syringe pump by surface cladding processing is cut with terylene Screw extruder is added in piece mixing, and the solution of mixed melting is squeezed out by spinneret orifice, cooling by circulator bath, using drum It air-dries dry, removes the moisture on surface, the terylene particle of doping silver powder is made through pelleter；
(4) spinning: the dry water content for making the terylene particle for adulterating the silver powder by surface cladding processing is lower than 25ppm, Screw Extrusion spinning machine is added in terylene particle, is extruded after melting from spinneret orifice, is frozen into silk；
(5) it post-processes: long filament obtained is subjected to drawing-off, winding and doffing.
The present invention relates to the step of (3) in by surface cladding processing silver powder and terylene chips weight ratio be (0.05- 8): 100, screw extruder melting temperature is 250 DEG C -300 DEG C.
The present invention relates to the step of (3) in control mixture inherent viscosity be 0.5-0.9dL/g, water content 110- 150ppm。
The present invention relates to the step of (4) in the extruder temperature of Screw Extrusion spinning machine be 250 DEG C -280 DEG C, temperature in manifold Degree is 260 DEG C -290 DEG C.
The present invention relates to the step of (5) in, draw ratio is 2-7 times when drawing-off, and circular blow air temperature is 10-30 DEG C, circular blow Wind wind speed is 5-20m/s.
The present invention relates to the step of (1) in silver powder surface coat processing method are as follows:
(1) it is mixed 1-5 minutes with neopelex powder and silver powder, reduces the electrostatic force between silver powder, Prevent the generation of silver powder agglomeration；
(2) mixed silver powder is added in the ethanol solution for the ethyl orthosilicate that weight percent concentration is 5% simultaneously The NaOH aqueous solution that molar concentration is 1.0mol/L is added dropwise in quickly stirring, so that solution ph is greater than 7, the reaction time is that 0.5-5 is small When, reaction product is filtered, is dried, the silver powder of coated with silica is obtained；
(3) silver powder of coated with silica is placed in reactor, N-Methyl pyrrolidone is added, divided under ultrasound condition It dissipates 10-60 minutes, in N2Silane coupling agent is added under atmosphere, the reaction time is 0.5-5 hours；
(4) sediment is filtered, is dried under the conditions of 40-80 DEG C to get to by surface cladding processing Silver powder.
The weight of neopelex powder and silver powder described in cladding process method step (1) of the present invention Amount is than being (0.5-2): 100.
The weight ratio of N-Methyl pyrrolidone and silver powder described in cladding process method step (3) of the present invention is (0.2-1): 100, silane coupling agent and silver powder weight ratio are (0.5-5): 100；
Compared with prior art, the present invention its process simple and effective for preparing antibiotic polyester fiber, by using Silver powder carried out cladding processing, reduce the reunion of silver powder, it is more preferable to make to produce polyester fiber antibacterial effect, and polyester fiber In silver powder it is not easily to fall off, obtain excellent anti-microbial property and Durability of antimicrobial effect using lower cost, design principle is reliable, Automation of Manufacturing Process degree is high, and good product quality can be promoted the use of.
Specific embodiment:
Below by embodiment, the invention will be further described.
Embodiment 1:
The preparation method for the antibiotic polyester fiber that the present embodiment is related to, includes the following steps:
(1) it is mixed 1-5 minutes with neopelex powder and silver powder, reduces the electrostatic force between silver powder, The generation of silver powder agglomeration is prevented, used silver powder partial size is 1-10 microns, neopelex powder and silver powder Weight ratio be 0.5:100；
(2) mixed silver powder is added in the ethanol solution for the ethyl orthosilicate that weight percent concentration is 5% simultaneously The NaOH aqueous solution that molar concentration is 1.0mol/L is added dropwise in quickly stirring, so that solution ph is greater than 7, the reaction time is 0.5 small When, reaction product is filtered, is dried, the silver powder of coated with silica is obtained；
(3) silver powder of coated with silica is placed in reactor, N-Methyl pyrrolidone is added, divided under ultrasound condition It dissipates 60 minutes, in N2Silane coupling agent is added under atmosphere, the reaction time is 0.5 hour；The N-Methyl pyrrolidone and silver of addition The weight ratio of powder is 0.2:100, and silane coupling agent and silver powder weight ratio are 0.5:100；Silane coupling agent can enhance at cladding Dispersibility and bonding force of the silver powder in terylene after reason, keeps silver powder not easily to fall off；
(4) sediment is filtered, is dried under the conditions of 40 DEG C 1 hour and is handled to get to by surface cladding Silver powder.
(5) terylene chips are dried using vacuum oven, drying temperature is set as 100 DEG C, makes terylene chips Water content is 110ppm；
(6) prepared by antibacterial functions particle: the silver powder using the addition of output syringe pump by surface cladding processing is cut with terylene Piece mixes according to a certain percentage is added screw extruder, and the solution of mixed melting is squeezed out by spinneret orifice, passes through recirculated water Bath cooling, using forced air drying, removes the moisture on surface, and the terylene particle of doping silver powder is made through pelleter；By surface The weight ratio of the silver powder and terylene chips that coat processing is 0.05:100, and screw extruder melting temperature is set as 260 DEG C；Control The inherent viscosity of mixture is 0.5dL/g, water content 110ppm；
(7) spinning: the dry water content for making the terylene particle for adulterating the silver powder by surface cladding processing is lower than 25ppm, Screw Extrusion spinning machine is added in terylene particle, is extruded after melting from spinneret orifice, is frozen into silk；Wherein Screw Extrusion spinning machine Extruder temperature is 280 DEG C, and spinning the temperature inside the box is 290 DEG C；
(8) it post-processes: long filament obtained is subjected to drawing-off, winding and doffing, wherein draw ratio is 2 times when drawing-off, ring Temperature of drying is 20 DEG C, and circular blow wind wind speed is 7m/s.
Embodiment 2:
The preparation method for the antibiotic polyester fiber that the present embodiment is related to, includes the following steps:
(1) it is mixed 1-5 minutes with neopelex powder and silver powder, reduces the electrostatic force between silver powder, The generation of silver powder agglomeration is prevented, used silver powder partial size is 10-15 microns, neopelex powder and silver powder Weight ratio be 2:100；
(2) mixed silver powder is added in the ethanol solution for the ethyl orthosilicate that weight percent concentration is 5% simultaneously The NaOH aqueous solution that molar concentration is 1.0mol/L is added dropwise in quickly stirring, so that solution ph is greater than 7, the reaction time is 0.5 small When, reaction product is filtered, is dried, the silver powder of coated with silica is obtained；
(3) silver powder of coated with silica is placed in reactor, N-Methyl pyrrolidone is added, divided under ultrasound condition It dissipates 30 minutes, in N2Silane coupling agent is added under atmosphere, the reaction time is 3 hours；The N-Methyl pyrrolidone and silver powder of addition Weight ratio be 0.5:100, silane coupling agent and silver powder weight ratio are 4:100；After silane coupling agent can enhance cladding processing Dispersibility and bonding force of the silver powder in terylene, keep silver powder not easily to fall off；
(4) sediment is filtered, is dried under the conditions of 80 DEG C 1 hour and is handled to get to by surface cladding Silver powder.
(5) terylene chips are dried using vacuum oven, drying temperature is set as 100 DEG C, makes terylene chips Water content is 130ppm；
(6) prepared by antibacterial functions particle: the silver powder using the addition of output syringe pump by surface cladding processing is cut with terylene Piece mixes according to a certain percentage is added screw extruder, and the solution of mixed melting is squeezed out by spinneret orifice, passes through recirculated water Bath cooling, using forced air drying, removes the moisture on surface, and the terylene particle of doping silver powder is made through pelleter；By surface The weight ratio of the silver powder and terylene chips that coat processing is 8:100, and screw extruder melting temperature is set as 270 DEG C；Control is mixed The inherent viscosity for closing material is 0.5dL/g, water content 110ppm；
(7) spinning: the dry water content for making the terylene particle for adulterating the silver powder by surface cladding processing is lower than 25ppm, Screw Extrusion spinning machine is added in terylene particle, is extruded after melting from spinneret orifice, is frozen into silk；Wherein Screw Extrusion spinning machine Extruder temperature is 265 DEG C, and spinning the temperature inside the box is 270 DEG C；
(8) it post-processes: long filament obtained is subjected to drawing-off, winding and doffing, wherein draw ratio is 4 times when drawing-off, ring Temperature of drying is 20 DEG C, and circular blow wind wind speed is 10m/s.
Embodiment 3:
The preparation method for the antibiotic polyester fiber that the present embodiment is related to, includes the following steps:
(1) it is mixed 1-5 minutes with neopelex powder and silver powder, reduces the electrostatic force between silver powder, The generation of silver powder agglomeration is prevented, used silver powder partial size is 10-15 microns, neopelex powder and silver powder Weight ratio be 1:100；
(2) mixed silver powder is added in the ethanol solution for the ethyl orthosilicate that weight percent concentration is 5% simultaneously The NaOH aqueous solution that molar concentration is 1.0mol/L is added dropwise in quickly stirring, and solution ph is made to be greater than 7, and the reaction time is 2 hours, Reaction product is filtered, is dried, the silver powder of coated with silica is obtained；
(3) silver powder of coated with silica is placed in reactor, N-Methyl pyrrolidone is added, divided under ultrasound condition It dissipates 10 minutes, in N2Silane coupling agent is added under atmosphere, the reaction time is 5 hours；The N-Methyl pyrrolidone and silver powder of addition Weight ratio be 1:100, silane coupling agent and silver powder weight ratio are 5:100；Silane coupling agent can enhance cladding, and treated Dispersibility and bonding force of the silver powder in terylene, keep silver powder not easily to fall off；
(4) sediment is filtered, is dried under the conditions of 80 DEG C 1 hour and is handled to get to by surface cladding Silver powder.
(5) terylene chips are dried using vacuum oven, drying temperature is set as 100 DEG C, makes terylene chips Water content is 150ppm；
(6) prepared by antibacterial functions particle: the silver powder using the addition of output syringe pump by surface cladding processing is cut with terylene Piece mixes according to a certain percentage is added screw extruder, and the solution of mixed melting is squeezed out by spinneret orifice, passes through recirculated water Bath cooling, using forced air drying, removes the moisture on surface, and the terylene particle of doping silver powder is made through pelleter；By surface The weight ratio of the silver powder and terylene chips that coat processing is 4:100, and screw extruder melting temperature is set as 300 DEG C；Control is mixed The inherent viscosity for closing material is 0.5dL/g, water content 150ppm；
(7) spinning: the dry water content for making the terylene particle for adulterating the silver powder by surface cladding processing is lower than 25ppm, Screw Extrusion spinning machine is added in terylene particle, is extruded after melting from spinneret orifice, is frozen into silk；Wherein Screw Extrusion spinning machine Extruder temperature is 250 DEG C, and spinning the temperature inside the box is 260 DEG C；
(8) it post-processes: long filament obtained is subjected to drawing-off, winding and doffing, wherein draw ratio is 4 times when drawing-off, ring Temperature of drying is 20 DEG C, and circular blow wind wind speed is 20m/s.

Claims (8)

1. a kind of preparation method of antibiotic polyester fiber, which comprises the following steps:
(1) cladding processing is carried out to silver powder, used silver powder partial size is 1-15 microns；
(2) it is dried: terylene chips being dried using vacuum oven, drying temperature is set as 100 DEG C, cuts terylene The water content of piece is 110ppm；
(3) prepared by antibacterial functions particle: the silver powder using the addition of output syringe pump by surface cladding processing, mixed with terylene chips It closes and screw extruder is added, the solution of mixed melting is squeezed out by spinneret orifice, it is cooling by circulator bath, it is dry using air blast It is dry, the moisture on surface is removed, the terylene particle of doping silver powder is made through pelleter；
(4) spinning: the water content of the dry terylene particle for making to adulterate the silver powder by surface cladding processing will be washed lower than 25ppm Screw Extrusion spinning machine is added in synthetic fibre particle, extrudes after melting from spinneret orifice, is frozen into silk；
(5) it post-processes: long filament obtained is subjected to drawing-off, winding and doffing.
2. the preparation method of antibiotic polyester fiber according to claim 1, it is characterised in that: in step (3), by surface The weight ratio of the silver powder and terylene chips that coat processing is (0.05-8): 100, screw extruder melting temperature is 250 DEG C -300 ℃。
3. the preparation method of antibiotic polyester fiber according to claim 1, it is characterised in that: in step (3), control mixing The inherent viscosity of material is 0.5-0.9dL/g, water content 110-150ppm.
4. the preparation method of antibiotic polyester fiber according to claim 1, it is characterised in that: in step (4), Screw Extrusion The extruder temperature of spinning machine is 250 DEG C -280 DEG C, and spinning the temperature inside the box is 260 DEG C -290 DEG C.
5. the preparation method of antibiotic polyester fiber according to claim 1, it is characterised in that: in step (5), when drawing-off is drawn Stretching multiple is 2-7 times, and circular blow air temperature is 10-30 DEG C, and circular blow wind wind speed is 5-20m/s.
6. the preparation method of antibiotic polyester fiber according to claim 1, it is characterised in that: silver powder surface in step (1) Coat processing method are as follows:
(1) it is mixed 1-5 minutes with neopelex powder and silver powder, reduces the electrostatic force between silver powder, prevent The generation of silver powder agglomeration；
(2) mixed silver powder is added in the ethanol solution for the ethyl orthosilicate that weight percent concentration is 5% and quick The NaOH aqueous solution that molar concentration is 1.0mol/L is added dropwise in stirring, and solution ph is made to be greater than 7, and the reaction time is 0.5-5 hours, Reaction product is filtered, is dried, the silver powder of coated with silica is obtained；
(3) silver powder of coated with silica is placed in reactor, N-Methyl pyrrolidone is added, disperses under ultrasound condition 10-60 minutes, in N2Silane coupling agent is added under atmosphere, the reaction time is 0.5-5 hours；
(4) sediment is filtered, is dried 1 hour under the conditions of 40-80 DEG C to get to by surface cladding processing Silver powder.
7. the preparation method of antibiotic polyester fiber according to claim 6, it is characterised in that: cladding process method step (1) weight ratio of neopelex powder and silver powder described in is (0.5-2): 100.
8. the preparation method of antibiotic polyester fiber according to claim 6, it is characterised in that: cladding process method step (3) weight ratio of N-Methyl pyrrolidone and silver powder described in is (0.2-1): 100, silane coupling agent is with silver powder weight ratio (0.5-5): 100.
CN201910598686.1A 2019-07-04 2019-07-04 A kind of preparation method of antibiotic polyester fiber Pending CN110230119A (en)

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CN110644069A (en) * 2019-10-18 2020-01-03 青岛银原素纺织科技有限公司 Preparation method of moisture-absorbing sweat-releasing antibacterial polyamide filament
CN110670167A (en) * 2019-10-18 2020-01-10 青岛银原素纺织科技有限公司 Preparation method of antibacterial polyester staple fibers
CN110699777A (en) * 2019-10-18 2020-01-17 青岛银原素纺织科技有限公司 Preparation method of skin-core structure antibacterial chinlon
CN110714238A (en) * 2019-10-18 2020-01-21 青岛银原素纺织科技有限公司 Preparation method of skin-core structure antibacterial polyester
CN112267162A (en) * 2020-10-16 2021-01-26 浙江银瑜新材料股份有限公司 Preparation method of polyester fiber with zinc oxide deposited on surface of titanium dioxide

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110644069A (en) * 2019-10-18 2020-01-03 青岛银原素纺织科技有限公司 Preparation method of moisture-absorbing sweat-releasing antibacterial polyamide filament
CN110670167A (en) * 2019-10-18 2020-01-10 青岛银原素纺织科技有限公司 Preparation method of antibacterial polyester staple fibers
CN110699777A (en) * 2019-10-18 2020-01-17 青岛银原素纺织科技有限公司 Preparation method of skin-core structure antibacterial chinlon
CN110714238A (en) * 2019-10-18 2020-01-21 青岛银原素纺织科技有限公司 Preparation method of skin-core structure antibacterial polyester
CN112267162A (en) * 2020-10-16 2021-01-26 浙江银瑜新材料股份有限公司 Preparation method of polyester fiber with zinc oxide deposited on surface of titanium dioxide

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