CN106917157B - Degradable antibacterial polylactic acid elastomer and preparation method thereof - Google Patents
Degradable antibacterial polylactic acid elastomer and preparation method thereof Download PDFInfo
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- CN106917157B CN106917157B CN201710160492.4A CN201710160492A CN106917157B CN 106917157 B CN106917157 B CN 106917157B CN 201710160492 A CN201710160492 A CN 201710160492A CN 106917157 B CN106917157 B CN 106917157B
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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
- 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
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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
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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
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- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
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- Biological Depolymerization Polymers (AREA)
- Artificial Filaments (AREA)
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Abstract
The invention discloses a kind of degradable antibacterial polylactic acid elastomers, include 100 parts of polylactic acid, 5-10 parts of maleic anhydride graft compatilizer, 1-2 parts of peroxidized t-butyl perbenzoate, 8-12 parts of antibacterial agent, 5-8 parts of citric acid, 10-16 parts of the tert-butyl alcohol, 2-5 parts of vinylpolydimethyl silane, 0.2-0.5 parts of phosphite by mass fraction；The antibacterial agent includes 20 parts of nano-cerium oxide, 75 parts of nano zine oxide, 5 parts of modified activated carbon by mass fraction, wherein the modified activated carbon includes 80 parts of active carbon, 5 parts of cerous nitrate, 5 parts of starch, 10 parts of citric acid solution that concentration is 3mol/L by mass fraction.The raw materials used in the present invention is nontoxic or intimate nontoxic, composite green chemistry principle, and obtained fiber is a kind of degradable antibacterial polylactic acid elastomer degradable, elastic big and with anti-microbial property, and whole preparation method is simple, feasible.
Description
Technical field
The present invention relates to a kind of fiber, especially degradable antibacterial polylactic acid elastomer.
Background technique
Polylactic acid is bound up as unit of microbial fermentation product lactic acid.It can be thorough after polylactic acid article is discarded
Carbon dioxide and who are resolved into, is not polluted the environment, thus is a kind of degradation material of complete natural circulation type all.But polylactic acid
Brittleness is big, defect with high hardness limits its further application, especially also needs to be mentioned in fiber art, elastic property
It is high.As people are to the pay attention to day by day of environment and own health, the functional form of acid fiber by polylactic is required also to be gradually increased.
Summary of the invention
It provides a kind of degradable, elastic big and has the purpose of the present invention is to solve above-mentioned the deficiencies in the prior art
There is the degradable antibacterial polylactic acid elastomer of anti-microbial property.
To achieve the goals above, the degradable antibacterial polylactic acid elastomer designed by the present invention, by mass fraction packet
Include 100 parts of polylactic acid, 5-10 parts of maleic anhydride graft compatilizer, 1-2 parts of peroxidized t-butyl perbenzoate, 8-12 parts of antibacterial agent,
5-8 parts of citric acid, 10-16 parts of the tert-butyl alcohol, 2-5 parts of vinylpolydimethyl silane, 0.2-0.5 parts of phosphite；The antibacterial
Agent includes 20 parts of nano-cerium oxide, 75 parts of nano zine oxide, 5 parts of modified activated carbon by mass fraction, wherein the modified active
Charcoal includes 80 parts of active carbon, 5 parts of cerous nitrate, 5 parts of starch, 10 parts of citric acid solution that concentration is 3mol/L by mass fraction.
Degradable antibacterial polylactic acid elastomer the preparation method is as follows:
Step 1: prepare modified activated carbon, active carbon is first passed through into ethyl alcohol and impregnates and filters after stirring 10min, takes 80 parts
It is put into reactor, the citric acid solution, 5 parts of cerous nitrates and 5 parts of starch that 10 parts of concentration are 3mol/L is added, is in bath temperature
It is stirred to react 3h at 75 DEG C, is put into Muffle furnace after cooling, takes out and is cooled to room temperature after calcining 2h at being 600 DEG C in temperature, grind
Being milled to partial size is 80-100nm, for use；
Step 2: antibacterial agent is prepared, 20 parts of nano-cerium oxides, 75 parts of nano zine oxides and 5 parts of modified activated carbons are abundant
Mixing, for use；
Step 3: degradable antibacterial polylactic acid elastomer is prepared, by 100 parts of polylactic acid, 5-10 parts of maleic anhydride grafting
Compatilizer and 1-2 parts of peroxidized t-butyl perbenzoates are put into reactor, are uniformly mixed, and continue to stir, at 200-220 DEG C
2h is reacted, under slow stirring, then 8-12 parts of antibacterial agents, 5-8 parts of citric acids, 10-16 parts of tert-butyl alcohols, 2- are added into reactor
5 parts of vinylpolydimethyl silane and 0.2-0.5 parts of phosphites, frit reaction 2h, leads to after reaction at 220-240 DEG C
Enter and squeeze out and be granulated in screw extruder, obtains polylactic acid master batch；Polylactic acid master batch is sent into melt spinning machine hopper, by spraying
Silk head sprays, and is wound in tube filler after crosswind is cooling by winding device, and it is fine to finally obtain degradable antibacterial polylactic acid elasticity
Dimension.
Wherein, each regional temperature control of the screw extruder is at 200-240 DEG C；The temperature used of spinning machine is in 240-
290 DEG C, spinning head aperture is 0.15mm, and the temperature of the crosswind is 23 DEG C, wind speed 0.4m/s, humidity 75%.
Polylactic acid is the polymer obtained with lactic acid for main polymerizable raw material, and raw material sources are abundant and can regenerate.It is poly-
The production process of lactic acid is pollution-free, and product can be biodegradable, realizes circulation in nature, therefore is ideal green
Color high molecular material.Applied in production fiber, the presence of polylactic acid makes the fiber with more degradable performance.Maleic acid
Acid anhydride is grafted compatilizer by introducing highly polar reactive group, so that material is had high polarity and reactivity, is a kind of macromolecule circle
Face coupling agent, compatilizer, dispersion enhancing agents, also, it can improve to a certain extent there are also certain toughening, enhancing performance
The more fragile disadvantage of pure acid fiber by polylactic promotes toughness.Wherein, peroxidized t-butyl perbenzoate is as a kind of initiator, energy
Enough progress for promoting reaction, so that reaction is more abundant.In order to enable the acid fiber by polylactic of preparation has certain anti-microbial property,
We joined antibacterial agent in system, which is the mixture of nano-cerium oxide, nano zine oxide and modified activated carbon.
On the antibacterial functions that nano zine oxide originally has, add modified activated carbon, can promote to a certain extent to germ,
The harmful microbes suction-operated such as bacterium, and the addition of nano-cerium oxide can reinforce the suction-operated of modified activated carbon,
It is interspersed in the structural system of active carbon, nano-cerium oxide has absorption to ultraviolet, can enhance the antibacterial of nano zine oxide
Performance.In addition, the cerium ion in the cerous nitrate for including in modified activated carbon grafts under the solutions of weak acidity of citric acid solution
On activated carbon structure, increase the adsorption capacity of active carbon, the starch of addition provides degradable environment for modified activated carbon.Except this it
Outside, citric acid can carry out the adjusting of pH value to reaction system, promote the good progress of reaction；Vinylpolydimethyl silane is
The elasticity of fiber can be improved in addition system for a kind of organic silicon rubber, and the addition of phosphite has facilitation to it, can
The elasticity that fiber is made is promoted to a certain extent.The tert-butyl alcohol can do solvent use, promote being uniformly distributed for each component.
The degradable antibacterial polylactic acid elastomer that the present invention obtains, its technical effect is that raw materials used is nontoxic or intimate
It is nontoxic, composite green chemistry principle, and obtained fiber is a kind of degradable, elastic big and dropping with anti-microbial property
Antibacterial polylactic acid elastomer is solved, whole preparation method is simple, feasible.
Specific embodiment
Below with reference to embodiment, the present invention is further described.
Embodiment 1:
Degradable antibacterial polylactic acid elastomer provided by the present embodiment includes 100 parts of polylactic acid, horse by mass fraction
8 parts of maleic anhydride grafted compatilizer, 2 parts of peroxidized t-butyl perbenzoate, 8 parts of antibacterial agent, 6 parts of citric acid, 12 parts of the tert-butyl alcohol, ethylene
3 parts of base polydimethylsiloxane, 0.3 part of phosphite；The antibacterial agent includes 20 parts of nano-cerium oxide, nano oxygen by mass fraction
Change 75 parts of zinc, 5 parts of modified activated carbon, wherein the modified activated carbon by mass fraction include 80 parts of active carbon, 5 parts of cerous nitrate,
5 parts of starch, 10 parts of citric acid solution that concentration is 3mol/L.
Degradable antibacterial polylactic acid elastomer the preparation method is as follows:
Step 1: prepare modified activated carbon, active carbon is first passed through into ethyl alcohol and impregnates and filters after stirring 10min, takes 80 parts
It is put into reactor, the citric acid solution, 5 parts of cerous nitrates and 5 parts of starch that 10 parts of concentration are 3mol/L is added, is in bath temperature
It is stirred to react 3h at 75 DEG C, is put into Muffle furnace after cooling, takes out and is cooled to room temperature after calcining 2h at being 600 DEG C in temperature, grind
Being milled to partial size is 90nm, for use；
Step 2: antibacterial agent is prepared, 20 parts of nano-cerium oxides, 75 parts of nano zine oxides and 5 parts of modified activated carbons are abundant
Mixing, for use；
Step 3: degradable antibacterial polylactic acid elastomer is prepared, 100 parts of polylactic acid, 8 parts of maleic anhydride grafting are compatible
Agent and 2 parts of peroxidized t-butyl perbenzoates are put into reactor, are uniformly mixed, and continue to stir, are reacted 2h at 200 DEG C,
It is slowly stirred down, then 8 parts of antibacterial agents, 6 parts of citric acids, 12 parts of tert-butyl alcohols, 3 parts of vinylpolydimethyl silicon is added into reactor
Alkane and 0.3 part of phosphite, the frit reaction 2h at 240 DEG C are passed through in screw extruder after reaction and squeeze out and be granulated, obtain
To polylactic acid master batch；Polylactic acid master batch is sent into melt spinning machine hopper, is sprayed by spinning head, by rolling up after crosswind is cooling
Winding apparatus is wound in tube filler, finally obtains degradable antibacterial polylactic acid elastomer.
Wherein, each regional temperature control of the screw extruder is at 210 DEG C；The temperature used of spinning machine is at 270 DEG C, spinneret
Head bore diameter is 0.15mm, and the temperature of the crosswind is 23 DEG C, wind speed 0.4m/s, humidity 75%.
Obtained degradable antibacterial polylactic acid elastomer is subjected to performance detection, 100%, which extends lower recovery rate, is
94.8%；Inhibition zone test the result shows that, degradable antibacterial polylactic acid elastomer is to escherichia coli provided by the present embodiment
The inhibiting rate of bacterium and staphylococcus aureus is up to 99.97%.
Embodiment 2:
Degradable antibacterial polylactic acid elastomer provided by the present embodiment, raw material and preparation method substantially with embodiment 1
Identical, the main distinction is, in the present embodiment, mass fraction used in antibacterial agent is 10 parts, and vinylpolydimethyl silane is 4
Part.
Obtained degradable antibacterial polylactic acid elastomer is subjected to performance detection, 100%, which extends lower recovery rate, is
95.6%；Inhibition zone test the result shows that, degradable antibacterial polylactic acid elastomer provided in this embodiment is to escherichia coli
With the inhibiting rate of staphylococcus aureus up to 99.98%.
Embodiment 3:
Degradable antibacterial polylactic acid elastomer provided by the present embodiment, raw material and preparation method substantially with embodiment 1
Identical, the main distinction is, in the present embodiment, mass fraction used in antibacterial agent is 12 parts, and vinylpolydimethyl silane is 5
Part.
Obtained degradable antibacterial polylactic acid elastomer is subjected to performance detection, 100%, which extends lower recovery rate, is
96.9%；Inhibition zone test the result shows that, degradable antibacterial polylactic acid elastomer provided in this embodiment is to escherichia coli
With the inhibiting rate of staphylococcus aureus up to 99.99%.
Claims (3)
1. a kind of degradable antibacterial polylactic acid elastomer, it is characterised in that: by mass fraction include 100 parts of polylactic acid, Malaysia
Acid anhydrides is grafted compatilizer 5-10 parts, 1-2 parts of peroxidized t-butyl perbenzoate, 8-12 parts of antibacterial agent, 5-8 parts of citric acid, the tert-butyl alcohol
10-16 parts, 2-5 parts of vinylpolydimethyl silane, 0.2-0.5 parts of phosphite；The antibacterial agent includes receiving by mass fraction
Rice 20 parts of cerium oxide, 75 parts of nano zine oxide, 5 parts of modified activated carbon, wherein the modified activated carbon includes living by mass fraction
Property 80 parts of charcoal, 5 parts of cerous nitrate, 5 parts of starch, concentration be 10 parts of citric acid solution of 3mol/L.
2. a kind of preparation method of degradable antibacterial polylactic acid elastomer as described in claim 1, it is characterised in that:
Step 1: prepare modified activated carbon, active carbon is first passed through into ethyl alcohol and impregnates and filters after stirring 10min, takes 80 parts to be put into
In reactor, the citric acid solution, 5 parts of cerous nitrates and 5 parts of starch that 10 parts of concentration are 3mol/L is added, is 75 DEG C in bath temperature
Under be stirred to react 3h, be put into Muffle furnace after cooling, calcine to take out after 2h at being 600 DEG C in temperature and be cooled to room temperature, be ground to
Partial size is 80-100nm, for use；
Step 2: preparing antibacterial agent, 20 parts of nano-cerium oxides, 75 parts of nano zine oxides and 5 parts of modified activated carbons are sufficiently mixed,
For use；
Step 3: degradable antibacterial polylactic acid elastomer is prepared, 100 parts of polylactic acid, 5-10 parts of maleic anhydride grafting are compatible
Agent and 1-2 parts of peroxidized t-butyl perbenzoates are put into reactor, are uniformly mixed, and continue to stir, are reacted at 200-220 DEG C
2h under slow stirring, then 8-12 parts of antibacterial agents, 5-8 parts of citric acids, the 10-16 parts of tert-butyl alcohols, 2-5 parts is added into reactor
Vinylpolydimethyl silane and 0.2-0.5 parts of phosphites, frit reaction 2h, is passed through after reaction at 220-240 DEG C
It squeezes out and is granulated in screw extruder, obtain polylactic acid master batch；Polylactic acid master batch is sent into melt spinning machine hopper, by spinneret
Head sprays, and is wound in tube filler after crosswind is cooling by winding device, finally obtains degradable antibacterial polylactic acid elastomer.
3. the preparation method of degradable antibacterial polylactic acid elastomer according to claim 2, it is characterised in that: the spiral shell
Each regional temperature control of bar extruder is at 200-240 DEG C；At 240-290 DEG C, spinning head aperture is the temperature used of spinning machine
0.15mm, the temperature of the crosswind are 23 DEG C, wind speed 0.4m/s, humidity 75%.
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| CN201710160492.4A CN106917157B (en) | 2017-03-17 | 2017-03-17 | Degradable antibacterial polylactic acid elastomer and preparation method thereof |
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| CN106917157B true CN106917157B (en) | 2019-06-21 |
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Families Citing this family (5)
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| CN107699981A (en) * | 2017-09-20 | 2018-02-16 | 安徽锦翔纺织服饰有限公司 | A kind of environment-friendly degradable fiber and preparation method thereof |
| CN113529206A (en) * | 2020-04-22 | 2021-10-22 | 中国石油化工股份有限公司 | Antibacterial and deodorant ES fiber and preparation method thereof |
| CN111549392B (en) * | 2020-04-24 | 2021-04-23 | 北京化工大学 | Preparation method of antibacterial polyphenylene sulfide fiber |
| CN111728293A (en) * | 2020-05-28 | 2020-10-02 | 南京微米电子产业研究院有限公司 | Novel degradable nanofiber mask |
| CN113754916A (en) * | 2021-10-19 | 2021-12-07 | 江苏金世缘乳胶制品股份有限公司 | Preparation process of rare earth antibacterial natural latex product |
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| CN102086565A (en) * | 2010-12-08 | 2011-06-08 | 江南大学 | Polylactic acid antibacterial nanofiber membrane and preparation method thereof |
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| CN105239194A (en) * | 2015-11-20 | 2016-01-13 | 王庆 | Method of preparing flame-retarding anti-microbial polylactic acid fibers, spinning fibers into yarn and making fabric |
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Patent Citations (4)
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|---|---|---|---|---|
| CN101358382A (en) * | 2008-08-26 | 2009-02-04 | 东华大学 | Antibacterial nano fiber material and preparation method thereof |
| CN102086565A (en) * | 2010-12-08 | 2011-06-08 | 江南大学 | Polylactic acid antibacterial nanofiber membrane and preparation method thereof |
| CN102212896A (en) * | 2011-05-27 | 2011-10-12 | 东华大学 | High-efficiency antibacterial mildew-proof PLA (poly lactic acid) fiber with skin-core structure and preparation method thereof |
| CN105239194A (en) * | 2015-11-20 | 2016-01-13 | 王庆 | Method of preparing flame-retarding anti-microbial polylactic acid fibers, spinning fibers into yarn and making fabric |
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