CN107761188A - The preparation method of copper zinc composite antibacterial polyester fiber - Google Patents
The preparation method of copper zinc composite antibacterial polyester fiber Download PDFInfo
- Publication number
- CN107761188A CN107761188A CN201711192688.8A CN201711192688A CN107761188A CN 107761188 A CN107761188 A CN 107761188A CN 201711192688 A CN201711192688 A CN 201711192688A CN 107761188 A CN107761188 A CN 107761188A
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- CN
- China
- Prior art keywords
- preparation
- copper
- temperature
- polyester fiber
- antibacterial
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
-
- 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
-
- 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 present invention relates to synthetic fiber industry technical field, and in particular to a kind of preparation method of copper zinc composite antibacterial polyester fiber.A kind of preparation method of copper zinc composite antibacterial polyester fiber, comprises the following steps：（1）The preparation of copper zinc oxide composite antibiosis agent；（2）The preparation of antibacterial modified poliester chip；（3）The preparation of antibacterial modified pet fiber.Copper zinc composite antibacterial polyester fiber made of the present invention is respectively 91.2% and 93.2% to the bacteriostasis rate of Escherichia coli and staphylococcus aureus, has good antibacterial effect.
Description
Technical field
The present invention relates to synthetic fiber industry technical field, and in particular to a kind of preparation of copper zinc composite antibacterial polyester fiber
Method.
Background technology
Polyester fiber is the first big kind of current synthetic fibers.Fiber is taken various, polyester fiber and other conjunctions
Compare into fiber, with acceptable, the good spinnability and resource exploitability of its consumer, widely should obtain
With.
With people's living environment and horizontal continuous improvement, consumer also changes therewith to the demand of textile garment.From
Most start by cover body, it is warming for the purpose of primary demand, by now to the aesthetic requirements of the elements such as fashion, prevalence while, people
Pursuit also begin to be intended to environmental protection, the textile material of health.Textile is advantageous to microorganism and bacterial adhesion in fabric table
Face, and then propagate, it is detrimental to health.People can be infected with many human secretions when wearing clothes on fabric, this is micro- life
Thing provides nutrition, turns into it and lives away from home ground.For textile into the important carrier of transmission, this causes people to focus more on its safety
Health.Anti-bacterial fibre can suppress flourish of the bacterium on fabric, improve the living environment of people.Anti-bacterial fibre is ground
Study carefully and be valued by people with exploitation, it is believed that each field will be widely used in from now on.
Antiseptic mainly has natural class, organic and an inorganic at present, and wherein inorganic antiseptic is because its is excellent resistance to
Hot conduct polyester fiber class antiseptic preferably compared with other two classes antiseptics uses.In inorganic antiseptic, nano zine oxide
With nontoxic, tasteless, intrinsic colour is white, cheap while again non-stimulated to skin, and has high thermal stability,
The many merits such as do not decompose, never degenerate.Although zinc oxide has efficient antibacterial effect, due to being limited by energy gap
Make, it is general that only there is obvious suppression and killing action under ultraviolet light to bacterium, microorganism etc..However, reaching in ground
In the sunshine of ball, the accounting of ultraviolet light is only 5%~7%, irradiation condition of the single nano zine oxide in Weak ultraviolet
Lower anti-microbial property is relatively low.Therefore, its photoresponse scope is widened to improve anti-microbial property be very necessary.Pass through ion doping
Mode can introduce more oxygen vacancies in the lattice of nano zine oxide or introduce the defects of more, be photooxidation
Reaction provides more avtive spots, or by introducing impurity energy level, expands the absorption orientation to light, strengthen the suction of visible ray
Receipts ability.The ionic radius of copper ion is 0.073nm, and the ionic radius of zinc ion is 0.074 nm, and difference is smaller so that copper
Ion is easier to be incorporated into the lattice of zinc oxide, so as to improve the photocatalytic activity of nano zine oxide.
The content of the invention
It is contemplated that in view of the above-mentioned problems, propose a kind of preparation method of copper zinc composite antibacterial polyester fiber.
Technical program of the present invention lies in：
A kind of preparation method of copper zinc composite antibacterial polyester fiber, comprises the following steps：
（1）The preparation of copper-zine oxide complex antimicrobials；
（2）The preparation of antibacterial modified poliester chip；
（3）The preparation of antibacterial modified pet fiber.
The preparation detailed process of described copper-zine oxide complex antimicrobials is：Weigh zinc nitrate and copper nitrate is dissolved in 200m
L distilled water, magnetic agitation is placed in three-necked flask to clear solution；Citric acid magnetic agitation is added to dissolve to abundant, its
The mol ratio of middle zinc nitrate and citric acid is 1：1.3；It is 8 with constant pressure titration dripping ammonification water regulation pH value；In 80 DEG C of constant temperature
Water-bath evaporation moisture forms wet gel, then dries 24h until constant weight, obtains xerogel in 80 DEG C of vacuum drying chambers；Will be dry solidifying
Glue at 600 DEG C, calcines 2h, naturally cools to room temperature, copper-zine oxide nano composite antibacterial is obtained after grinding in air atmosphere
Agent.
The preparation detailed process that described bacterium is modified poliester chip is：By load weighted essence to benzene
Dioctyl phthalate, ethylene glycol and catalyst glycol antimony, stabilizer triphenyl phosphate and anti-ether agent zinc acetate input 5L polymeric kettles
In, the first esterification is carried out under the conditions of 240~250 DEG C and 0.3~0.4MPa；When the reception of the first reaction kettle of the esterification reclaimed water
When amount reaches theoretical value 95%, reaction terminates, normal pressure esterification 30min or so；Into the second esterification stage, copper-oxygen is added
Change zinc composite nano germicide；Polycondensation phase, temperature is gradually risen, start simultaneously at and be slowly evacuated to below 100Pa, control is anti-
Answering temperature, the polycondensation time is 2h at 275~283 DEG C, vacuum 50Pa, and reaction terminates that antibacterial modified poly terephthalic acid is made
Glycol ester is cut into slices.
The preparation detailed process of described antibacterial modified pet fiber is：Obtained antibacterial is changed
Property poliester chip 24h is dried in vacuo under the conditions of 140 DEG C, to section carry out melt spinning, obtain pre-
It is orientated silk；The temperature of screw rod is respectively 280 ~ 290 DEG C, and metering pump temperature is 289 DEG C, and assembly temperature is 290 DEG C, return bend temperature
For 290 DEG C, spinneret temperature is 290 DEG C, spinning speed 800m/min.As-spun fibre is stretched, heater temperature is
80 DEG C, temperature of heat plate is 160 DEG C.
Described zinc nitrate and the mol ratio of copper nitrate are 1：0.05.
The mass fraction 25%~28% of described ammoniacal liquor.
The technical effects of the invention are that：
Copper zinc composite antibacterial polyester fiber is respectively to the bacteriostasis rate of Escherichia coli and staphylococcus aureus made of the present invention
91.2% and 93.2%, there is good antibacterial effect.
Embodiment
A kind of preparation method of copper zinc composite antibacterial polyester fiber, comprises the following steps：
（1）The preparation of copper-zine oxide complex antimicrobials；
（2）The preparation of antibacterial modified poliester chip；
（3）The preparation of antibacterial modified pet fiber.
The preparation detailed process of described copper-zine oxide complex antimicrobials is：Weigh zinc nitrate and copper nitrate is dissolved in 200m
L distilled water, magnetic agitation is placed in three-necked flask to clear solution；Citric acid magnetic agitation is added to dissolve to abundant, its
The mol ratio of middle zinc nitrate and citric acid is 1：1.3；It is 8 with constant pressure titration dripping ammonification water regulation pH value；In 80 DEG C of constant temperature
Water-bath evaporation moisture forms wet gel, then dries 24h until constant weight, obtains xerogel in 80 DEG C of vacuum drying chambers；Will be dry solidifying
Glue at 600 DEG C, calcines 2h, naturally cools to room temperature, copper-zine oxide nano composite antibacterial is obtained after grinding in air atmosphere
Agent.
The preparation detailed process that described bacterium is modified poliester chip is：By load weighted essence to benzene
Dioctyl phthalate, ethylene glycol and catalyst glycol antimony, stabilizer triphenyl phosphate and anti-ether agent zinc acetate input 5L polymeric kettles
In, the first esterification is carried out under the conditions of 240~250 DEG C and 0.3~0.4MPa；When the reception of the first reaction kettle of the esterification reclaimed water
When amount reaches theoretical value 95%, reaction terminates, normal pressure esterification 30min or so；Into the second esterification stage, copper-oxygen is added
Change zinc composite nano germicide；Polycondensation phase, temperature is gradually risen, start simultaneously at and be slowly evacuated to below 100Pa, control is anti-
Answering temperature, the polycondensation time is 2h at 275~283 DEG C, vacuum 50Pa, and reaction terminates that antibacterial modified poly terephthalic acid is made
Glycol ester is cut into slices.
The preparation detailed process of described antibacterial modified pet fiber is：Obtained antibacterial is changed
Property poliester chip 24h is dried in vacuo under the conditions of 140 DEG C, to section carry out melt spinning, obtain pre-
It is orientated silk；The temperature of screw rod is respectively 280 ~ 290 DEG C, and metering pump temperature is 289 DEG C, and assembly temperature is 290 DEG C, return bend temperature
For 290 DEG C, spinneret temperature is 290 DEG C, spinning speed 800m/min.As-spun fibre is stretched, heater temperature is
80 DEG C, temperature of heat plate is 160 DEG C.
Wherein, the mol ratio of described zinc nitrate and copper nitrate is 1：0.05.The mass fraction 25% of described ammoniacal liquor~
28%.
Claims (6)
- A kind of 1. preparation method of copper zinc composite antibacterial polyester fiber, it is characterised in that：Comprise the following steps：（1）The preparation of copper-zine oxide complex antimicrobials；（2）The preparation of antibacterial modified poliester chip；（3）The preparation of antibacterial modified pet fiber.
- 2. the preparation method of copper zinc composite antibacterial polyester fiber according to claim 1, it is characterised in that：Described copper- The preparation detailed process of zinc oxide composite antibiosis agent is：Weigh zinc nitrate and copper nitrate is dissolved in 200mL distilled water, be placed in three mouthfuls Magnetic agitation is to clear solution in flask；Citric acid magnetic agitation is added to abundant dissolving, wherein zinc nitrate and citric acid Mol ratio is 1：1.3；It is 8 with constant pressure titration dripping ammonification water regulation pH value；Formed in 80 DEG C of water bath with thermostatic control evaporation moisture wet Gel, then 24h is dried until constant weight, obtains xerogel in 80 DEG C of vacuum drying chambers；By xerogel 600 DEG C in air atmosphere Under, 2h is calcined, room temperature is naturally cooled to, copper-zine oxide composite nano germicide is obtained after grinding.
- 3. the preparation method of copper zinc composite antibacterial polyester fiber according to claim 2, it is characterised in that：Described bacterium changes The preparation detailed process of property poliester chip is：By load weighted p-phthalic acid, ethylene glycol and Catalyst glycol antimony, stabilizer triphenyl phosphate and anti-ether agent zinc acetate input 5L polymeric kettles in, at 240~250 DEG C and The first esterification is carried out under the conditions of 0.3~0.4MPa；When the reception amount of the first reaction kettle of the esterification reclaimed water reaches theoretical value 95% When, reaction terminates, normal pressure esterification 30min or so；Into the second esterification stage, copper-zine oxide nano composite antibacterial is added Agent；Polycondensation phase, temperature is gradually risen, start simultaneously at and be slowly evacuated to below 100Pa, controlling reaction temperature is 275~283 DEG C, vacuum 50Pa, the polycondensation time is 2h, and reaction terminates that antibacterial modified poliester chip is made.
- 4. the preparation method of copper zinc composite antibacterial polyester fiber according to claim 3, it is characterised in that：Described antibacterial The preparation detailed process of modified pet fiber is：The antibacterial modified poly terephthalic acid second two by made from Alcohol ester section is dried in vacuo 24h under the conditions of 140 DEG C, carries out melt spinning to section, obtains preoriented yarn；The temperature of screw rod point Wei not be 280 ~ 290 DEG C, metering pump temperature is 289 DEG C, and assembly temperature is 290 DEG C, and return bend temperature is 290 DEG C, spinneret temperature For 290 DEG C, spinning speed 800m/min；As-spun fibre is stretched, heater temperature is 80 DEG C, temperature of heat plate 160 ℃。
- 5. the preparation method of copper zinc composite antibacterial polyester fiber according to claim 4, it is characterised in that：Described nitric acid The mol ratio of zinc and copper nitrate is 1：0.05.
- 6. the preparation method of copper zinc composite antibacterial polyester fiber according to claim 5, it is characterised in that：Described ammoniacal liquor Mass fraction 25%~28%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711192688.8A CN107761188A (en) | 2017-11-24 | 2017-11-24 | The preparation method of copper zinc composite antibacterial polyester fiber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711192688.8A CN107761188A (en) | 2017-11-24 | 2017-11-24 | The preparation method of copper zinc composite antibacterial polyester fiber |
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| Publication Number | Publication Date |
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| CN107761188A true CN107761188A (en) | 2018-03-06 |
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| CN201711192688.8A Withdrawn CN107761188A (en) | 2017-11-24 | 2017-11-24 | The preparation method of copper zinc composite antibacterial polyester fiber |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108660538A (en) * | 2018-06-08 | 2018-10-16 | 佛山市南海区佳妍内衣有限公司 | A kind of antimicrobial form Multifunctional polyester fiber |
| CN108756703A (en) * | 2018-07-02 | 2018-11-06 | 佛山市南海区佳妍内衣有限公司 | Screen door structure with anti-haze bactericidal effect |
| CN110952166A (en) * | 2019-11-11 | 2020-04-03 | 江苏康溢臣生命科技有限公司 | Preparation process of cotton-like efficient moisture-absorbing moisture-conducting antibacterial fiber |
| CN111253719A (en) * | 2019-11-18 | 2020-06-09 | 厦门翔鹭化纤股份有限公司 | Organic zinc antibacterial PET granules and preparation method thereof |
| CN111394824A (en) * | 2020-04-01 | 2020-07-10 | 太仓市嘉伟纺织有限公司 | Preparation process of antibacterial high-shrinkage polyester fiber |
| CN111748084A (en) * | 2020-06-30 | 2020-10-09 | 四川东材科技集团股份有限公司 | Antibacterial flame-retardant polyester resin and preparation method thereof |
| CN115058787A (en) * | 2022-06-02 | 2022-09-16 | 浙江理工大学 | Preparation method of antibacterial and antiviral cool fiber |
-
2017
- 2017-11-24 CN CN201711192688.8A patent/CN107761188A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108660538A (en) * | 2018-06-08 | 2018-10-16 | 佛山市南海区佳妍内衣有限公司 | A kind of antimicrobial form Multifunctional polyester fiber |
| CN108756703A (en) * | 2018-07-02 | 2018-11-06 | 佛山市南海区佳妍内衣有限公司 | Screen door structure with anti-haze bactericidal effect |
| CN110952166A (en) * | 2019-11-11 | 2020-04-03 | 江苏康溢臣生命科技有限公司 | Preparation process of cotton-like efficient moisture-absorbing moisture-conducting antibacterial fiber |
| CN111253719A (en) * | 2019-11-18 | 2020-06-09 | 厦门翔鹭化纤股份有限公司 | Organic zinc antibacterial PET granules and preparation method thereof |
| CN111394824A (en) * | 2020-04-01 | 2020-07-10 | 太仓市嘉伟纺织有限公司 | Preparation process of antibacterial high-shrinkage polyester fiber |
| CN111748084A (en) * | 2020-06-30 | 2020-10-09 | 四川东材科技集团股份有限公司 | Antibacterial flame-retardant polyester resin and preparation method thereof |
| CN115058787A (en) * | 2022-06-02 | 2022-09-16 | 浙江理工大学 | Preparation method of antibacterial and antiviral cool fiber |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication | ||
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Application publication date: 20180306 |