CN110760167A - Long-acting antibacterial transparent PET master batch, window film and preparation method thereof - Google Patents
Long-acting antibacterial transparent PET master batch, window film and preparation method thereof Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/18—Homopolymers or copolymers of nitriles
- C08J2433/20—Homopolymers or copolymers of acrylonitrile
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
- C08K5/3432—Six-membered rings
- C08K5/3435—Piperidines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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Abstract
The invention relates to the technical field of PET (polyethylene terephthalate) master batches, and particularly relates to a long-acting antibacterial transparent PET master batch, a window film and a preparation method thereof. The composite material comprises the following raw materials in parts by weight: 50 parts of PET resin, 40-50 parts of special antibacterial agent, 2-6 parts of antioxidant, 1-4 parts of light stabilizer and 1-3 parts of ultraviolet absorbent. The mechanism of the special antibacterial agent of the invention is that: although the softening point of polyacrylonitrile is lower, the melting point is higher, the polyacrylonitrile microspheres can keep better structural integrity in the process of PET melt extrusion, after PET stretching film forming, because the thickness of the polyacrylonitrile microspheres is equivalent to the film thickness, the polyacrylonitrile microspheres are inserted into the BOPET film and exposed in the air, the distribution condition of nano titanium dioxide on the film surface is improved, and the finally prepared film material has the characteristic of long-acting antibiosis without spraying treatment.
Description
Technical Field
The invention relates to the technical field of PET (polyethylene terephthalate) master batches, and particularly relates to a long-acting antibacterial transparent PET master batch, a window film and a preparation method thereof.
Background
The polyester polymer is widely applied to products such as toys, window films, packaging materials and the like. With the progress of society, the use frequency is higher and higher, and the variety is more and more. However, these products do not have the function of bacteriostasis, are easy to breed or propagate various harmful bacteria, molds, viruses and other microorganisms, become a public transmission source and bring great trouble to the health of people.
The nano titanium dioxide is a new antibacterial agent. The nano titanium dioxide decomposes bacteria under the photocatalysis to achieve the antibacterial effect. The electronic structure of the nano titanium dioxide is characterized by being full of TiO2In a system of water and air, when the energy of electrons reaches or exceeds the band gap energy of the nano titanium dioxide under the irradiation of sunlight, especially ultraviolet rays, electrons can be excited from the valence band to the conduction band, corresponding holes are generated in the valence band, namely electron and hole pairs are generated, under the action of an electric field, the electrons and the holes are separated and migrate to different positions on the surface of particles to generate a series of reactions, and the electrons are adsorbed and dissolved in TiO2Oxygen-trapped electron formation of O at the surface2The superoxide anion radical formed reacts with (oxidizes) most organic species. Simultaneously can react with organic matters in bacteria to generate CO2And H2O; while holes will adsorb on the TiO2OH and H of the surface2O is oxidized into OH, which has strong oxidizing ability to attack the unsaturated bond of organic matter or extract H atom to generate new free radical to excite chain reaction and finally decompose bacteria.
And due to the characteristics of absorbing ultraviolet rays and absorbing moisture and air, the nano titanium dioxide can generally exert better performance by coating the coating liquid on the surface of a product. However, in view of economic efficiency, the window film manufacturers need additional coating materials, coating devices and curing equipment, which is costly, and the coating and curing of the film materials occupy a large area and have low efficiency.
Therefore, the development of the long-acting antibacterial master batch is a technical problem to be solved urgently.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a long-acting antibacterial transparent PET master batch, a window film and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the long-acting antibacterial transparent PET master batch comprises the following raw materials in parts by weight:
wherein, the special antibacterial agent is prepared by the following steps:
(1) dissolving 20-30 parts by weight of acrylonitrile in 100 parts by weight of organic solvent, then adding 0.1-0.3 part by weight of first initiator, stirring and mixing, heating to 40-50 ℃, and reacting for 2-4h to obtain precursor solution;
(2) adding 6-12 parts by weight of nano titanium dioxide and 0.1-0.2 part by weight of second initiator into the precursor solution, stirring and dispersing, heating to 50-60 ℃, and reacting for 3-5 hours to obtain a suspension;
(3) and carrying out electrostatic spraying on the suspension to obtain the special antibacterial agent.
In the preparation method of the special antibacterial agent, acrylonitrile is used for initiating polymerization to form a core for the first time, and acrylonitrile is used for initiating polymerization for the second time to coat the acrylonitrile core with nano titanium dioxide, so that the polyacrylonitrile microsphere with the nano titanium dioxide distributed on the surface is prepared, the particle size of the polyacrylonitrile microsphere is 10-30 mu m, and the thickness of the polyacrylonitrile microsphere is equivalent to that of a membrane material. The mechanism of the special antibacterial agent of the invention is that: although the softening point of polyacrylonitrile is lower, the melting point is higher, the polyacrylonitrile microspheres can keep better structural integrity in the process of PET melt extrusion, after PET stretching film forming, because the thickness of the polyacrylonitrile microspheres is equivalent to the film thickness, the polyacrylonitrile microspheres are inserted into the BOPET film and exposed in the air, the distribution condition of nano titanium dioxide on the film surface is improved, and the finally prepared film material has the characteristic of long-acting antibiosis without spraying treatment.
Wherein the organic solvent is dimethyl sulfoxide.
Wherein the first initiator and the second initiator are both azobisisobutyronitrile.
Wherein the particle size of the nano titanium dioxide is 15-25 nm.
Wherein the spraying voltage of the electrostatic spraying is 20-30kV, and the spraying temperature is 20-30 ℃.
Wherein the antioxidant is antioxidant 168 and/or antioxidant 1076.
Wherein the light stabilizer is bis (1, 2,2,6, 6-pentamethyl-4-piperidyl) sebacate and/or poly (1-hydroxyethyl-2, 2,6, 6-tetramethyl-4-hydroxypiperidine) succinate.
Wherein the ultraviolet absorbent is 2-cyano-3, 3' -diphenylacrylic acid-2-ethylhexyl ester and/or 2- (2-hydroxy-3-tert-butyl-5-methylphenyl) -5-chlorobenzotriazole.
The long-acting antibacterial transparent PET master batch is prepared by the following method: all the raw materials are put into a double-screw extruder for melt extrusion, and the extrusion temperature is 230-260 ℃.
A BOPET window film comprises the following raw materials in parts by weight:
100 parts of PET resin
50-70 parts of long-acting antibacterial transparent PET master batch
0.1-10 parts of functional assistant.
The preparation method of the BOPET window film comprises the following steps: and melting and mixing the PET resin, the heat-insulating master batch and the rest of auxiliary agents, and performing biaxial tension film forming to obtain the BOPET window film.
The invention has the beneficial effects that: in the preparation method of the special antibacterial agent, acrylonitrile is used for initiating polymerization to form a core for the first time, and acrylonitrile is used for initiating polymerization for the second time to coat the acrylonitrile core with nano titanium dioxide, so that the polyacrylonitrile microsphere with the nano titanium dioxide distributed on the surface is prepared, the particle size of the polyacrylonitrile microsphere is 10-30 mu m, and the thickness of the polyacrylonitrile microsphere is equivalent to that of a membrane material. The mechanism of the special antibacterial agent of the invention is that: although the softening point of polyacrylonitrile is lower, the melting point is higher, the polyacrylonitrile microspheres can keep better structural integrity in the process of PET melt extrusion, after PET stretching film forming, because the thickness of the polyacrylonitrile microspheres is equivalent to the film thickness, the polyacrylonitrile microspheres are inserted into the BOPET film and exposed in the air, the distribution condition of nano titanium dioxide on the film surface is improved, and the finally prepared film material has the characteristic of long-acting antibiosis without spraying treatment.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
The long-acting antibacterial transparent PET master batch comprises the following raw materials in parts by weight:
wherein, the special antibacterial agent is prepared by the following steps:
(1) dissolving 20 parts by weight of acrylonitrile in 100 parts by weight of organic solvent, adding 0.1 part by weight of first initiator, stirring and mixing, heating to 40 ℃, and reacting for 2 hours to obtain a precursor solution;
(2) adding 6 parts by weight of nano titanium dioxide and 0.1 part by weight of second initiator into the precursor solution, stirring and dispersing, heating to 50 ℃, and reacting for 3 hours to obtain a suspension;
(3) and carrying out electrostatic spraying on the suspension to obtain the special antibacterial agent.
Wherein the organic solvent is dimethyl sulfoxide.
Wherein the first initiator and the second initiator are both azobisisobutyronitrile.
Wherein the particle size of the nano titanium dioxide is 15 nm.
Wherein the spraying voltage of the electrostatic spraying is 20kV, and the spraying temperature is 20 ℃.
Wherein the antioxidant is antioxidant 168.
Wherein the light stabilizer is bis (1, 2,2,6, 6-pentamethyl-4-piperidyl) sebacate.
Wherein the ultraviolet absorbent is 2-cyano-3, 3' -diphenylacrylic acid-2-ethylhexyl ester.
A BOPET window film comprises the following raw materials in parts by weight:
100 parts of PET resin
50 parts of long-acting antibacterial transparent PET master batch
0.1 part of functional auxiliary agent;
the functional auxiliary agent is an antioxidant 1010.
The preparation method of the BOPET window film comprises the following steps: and melting and mixing the PET resin, the heat-insulating master batch and the rest of auxiliary agents, and performing biaxial tension film forming to obtain the BOPET window film.
Example 2
The long-acting antibacterial transparent PET master batch comprises the following raw materials in parts by weight:
wherein, the special antibacterial agent is prepared by the following steps:
(1) dissolving 20-30 parts by weight of acrylonitrile in 100 parts by weight of organic solvent, adding 0.3 part by weight of first initiator, stirring and mixing, heating to 50 ℃, and reacting for 4 hours to obtain a precursor solution;
(2) adding 12 parts by weight of nano titanium dioxide and 0.2 part by weight of second initiator into the precursor solution, stirring and dispersing, heating to 60 ℃, and reacting for 5 hours to obtain a suspension;
(3) and carrying out electrostatic spraying on the suspension to obtain the special antibacterial agent.
Wherein the organic solvent is dimethyl sulfoxide.
Wherein the first initiator and the second initiator are both azobisisobutyronitrile.
Wherein the particle size of the nano titanium dioxide is 25 nm.
Wherein the spraying voltage of the electrostatic spraying is 30kV, and the spraying temperature is 30 ℃.
Wherein the antioxidant is an antioxidant 1076.
Wherein the light stabilizer is poly (1-hydroxyethyl-2, 2,6, 6-tetramethyl-4-hydroxypiperidine) succinate.
Wherein the ultraviolet absorbent is 2- (2-hydroxy-3 tert-butyl-5-methylphenyl) -5-chlorobenzotriazole.
A BOPET window film comprises the following raw materials in parts by weight:
100 parts of PET resin
Long-acting antibacterial transparent PET master batch 70 parts
10 parts of functional auxiliary agent;
the functional auxiliary agents are antistatic agents, lubricants and antioxidants
The preparation method of the BOPET window film comprises the following steps: and melting and mixing the PET resin, the heat-insulating master batch and the rest of auxiliary agents, and performing biaxial tension film forming to obtain the BOPET window film.
Example 3
The long-acting antibacterial transparent PET master batch comprises the following raw materials in parts by weight:
wherein, the special antibacterial agent is prepared by the following steps:
(1) dissolving 25 parts by weight of acrylonitrile in 100 parts by weight of organic solvent, adding 0.2 part by weight of first initiator, stirring and mixing, heating to 45 ℃, and reacting for 3 hours to obtain a precursor solution;
(2) adding 9 parts by weight of nano titanium dioxide and 0.15 part by weight of second initiator into the precursor solution, stirring and dispersing, heating to 55 ℃, and reacting for 4 hours to obtain a suspension;
(3) and carrying out electrostatic spraying on the suspension to obtain the special antibacterial agent.
Wherein the organic solvent is dimethyl sulfoxide.
Wherein the first initiator and the second initiator are both azobisisobutyronitrile.
Wherein the particle size of the nano titanium dioxide is 20 nm.
Wherein the spraying voltage of the electrostatic spraying is 25kV, and the spraying temperature is 25 ℃.
Wherein the antioxidant is prepared from antioxidant 168 and antioxidant 1076 according to a weight ratio of 1: 1 in a certain proportion.
Wherein the light stabilizer is prepared from bis (1, 2,2,6, 6-pentamethyl-4-piperidyl) sebacate and poly (1-hydroxyethyl-2, 2,6, 6-tetramethyl-4-hydroxypiperidine) succinate according to the weight ratio of 1: 1 in a certain proportion.
Wherein the ultraviolet absorbent is prepared from 2-cyano-3, 3' -diphenylacrylic acid-2-ethylhexyl ester and 2- (2-hydroxy-3-tert-butyl-5-methylphenyl) -5-chlorobenzotriazole according to the weight ratio of 1: 1 in a certain proportion.
A BOPET window film comprises the following raw materials in parts by weight:
100 parts of PET resin
60 parts of long-acting antibacterial transparent PET master batch
0.1 part of functional auxiliary agent
The functional auxiliary agent is an antioxidant 1010.
The preparation method of the BOPET window film comprises the following steps: and melting and mixing the PET resin, the heat-insulating master batch and the rest of auxiliary agents, and performing biaxial tension film forming to obtain the BOPET window film.
Comparative example 1
This comparative example is a commercially available conventional BOPET film and a commercially available conventional nano-titania coating is applied to the film.
Comparative example 2
This comparative example differs from example 3 in that:
the antibacterial PET master batch comprises the following raw materials in parts by weight:
the films of example 3, comparative example 1 and comparative example 2 were tested for tensile strength, elongation at break and antimicrobial properties according to GB/T13022, GB/T21866, wherein the tensile strength and elongation at break of comparative example 2 was tested for BOPET films made directly from the antimicrobial PET masterbatch, and the test results are given in the following Table:
| tensile Strength (MPa) | Elongation at Break (%) | Antibacterial ratio (%) | |
| Example 3 | 113 | 470 | 90 |
| Comparative example 1 | 127 | 420 | 93 |
| Comparative example 2 | 132 | 560 | 84 |
From the aspect of antibacterial performance, the direct coating of the nano-silica coating is still the best choice, but the BOPET film of the invention can also realize the antibacterial rate of 90 percent, and the antibacterial performance is also relatively excellent; in the aspect of tensile strength, the commercial BOPET film is not modified by an antibacterial agent, so that the mechanical property is kept better, and the tensile strength and the elongation at break are better represented; from the aspect of the performance of elongation at break, comparative example 1 is inferior to the BOPET film of the present invention in that the toughness of the finished film is lowered due to the incorporation of a large amount of nano-titania, and thus the elongation at break is the worst.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A long-acting antibacterial transparent PET master batch is characterized in that: the composite material comprises the following raw materials in parts by weight:
wherein, the special antibacterial agent is prepared by the following steps:
(1) dissolving 20-30 parts by weight of acrylonitrile in 100 parts by weight of organic solvent, then adding 0.1-0.3 part by weight of first initiator, stirring and mixing, heating to 40-50 ℃, and reacting for 2-4h to obtain precursor solution;
(2) adding 6-12 parts by weight of nano titanium dioxide and 0.1-0.2 part by weight of second initiator into the precursor solution, stirring and dispersing, heating to 50-60 ℃, and reacting for 3-5 hours to obtain a suspension;
(3) and carrying out electrostatic spraying on the suspension to obtain the special antibacterial agent.
2. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the organic solvent is dimethyl sulfoxide.
3. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the first initiator and the second initiator are both azobisisobutyronitrile.
4. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the particle size of the nano titanium dioxide is 15-25 nm.
5. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the spraying voltage of the electrostatic spraying is 20-30kV, and the spraying temperature is 20-30 ℃.
6. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the antioxidant is antioxidant 168 and/or antioxidant 1076.
7. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the light stabilizer is bis (1, 2,2,6, 6-pentamethyl-4-piperidyl) sebacate and/or poly (1-hydroxyethyl-2, 2,6, 6-tetramethyl-4-hydroxypiperidine) succinate.
8. The long-acting antibacterial transparent PET master batch according to claim 1, characterized in that: the ultraviolet absorbent is 2-cyano-3, 3' -diphenylacrylic acid-2-ethylhexyl ester and/or 2- (2-hydroxy-3-tert-butyl-5-methylphenyl) -5-chlorobenzotriazole.
9. A BOPET window film is characterized in that: the composite material comprises the following raw materials in parts by weight:
100 parts of PET resin
50-70 parts of long-acting antibacterial transparent PET master batch
0.1-10 parts of functional auxiliary agent;
the long-acting antibacterial transparent PET master batch is the long-acting antibacterial transparent PET master batch according to any one of claims 1 to 8.
10. The method of making a BOPET window film of claim 9, wherein: and melting and mixing the PET resin, the heat-insulating master batch and the rest of auxiliary agents, and performing biaxial tension film forming to obtain the BOPET window film.
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| CN111363319A (en) * | 2020-03-22 | 2020-07-03 | 李丹丹 | Antibacterial and antistatic polyester film |
| CN112175362A (en) * | 2020-10-13 | 2021-01-05 | 广州九圆塑业有限公司 | PET composite material and preparation method thereof |
| CN113455518A (en) * | 2021-07-12 | 2021-10-01 | 新盈环保科技有限公司 | Nano titanium dioxide doped sterilization material and preparation method thereof |
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| CN112175362A (en) * | 2020-10-13 | 2021-01-05 | 广州九圆塑业有限公司 | PET composite material and preparation method thereof |
| CN113455518A (en) * | 2021-07-12 | 2021-10-01 | 新盈环保科技有限公司 | Nano titanium dioxide doped sterilization material and preparation method thereof |
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