CN114750495A - Antibacterial and anti-aging PET (polyethylene terephthalate) sheet and preparation method thereof - Google Patents
Antibacterial and anti-aging PET (polyethylene terephthalate) sheet and preparation method thereof Download PDFInfo
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- CN114750495A CN114750495A CN202210305906.9A CN202210305906A CN114750495A CN 114750495 A CN114750495 A CN 114750495A CN 202210305906 A CN202210305906 A CN 202210305906A CN 114750495 A CN114750495 A CN 114750495A
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- pet
- ultraviolet
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- antibacterial
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- 229920000139 polyethylene terephthalate Polymers 0.000 title claims abstract description 178
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 15
- 239000005020 polyethylene terephthalate Substances 0.000 title claims description 163
- -1 polyethylene terephthalate Polymers 0.000 title claims description 8
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- 238000000576 coating method Methods 0.000 claims abstract description 55
- 239000000463 material Substances 0.000 claims abstract description 36
- 229920002799 BoPET Polymers 0.000 claims abstract description 31
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 claims abstract description 17
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Images
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- B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
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- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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Abstract
The invention provides an antibacterial and anti-aging PET sheet and a preparation method thereof, belonging to the technical field of PET materials. The invention includes: a base layer of PET. The PET base layer is a microporous PET base layer, and the top of the PET base layer is provided with an antibacterial hydrophilic coating; one side of the PET basic layer, which is far away from the antibacterial hydrophilic coating, is fixedly provided with an anti-ultraviolet layer and a PET film through a transparent PET composite adhesive layer; the material of the ultraviolet resistant layer is ultraviolet resistant transparent PET. The antibacterial anti-aging PET sheet takes microcellular foaming PET as a PET base layer, and has the effects of light weight and high strength under the same conditions; the PET material of the ultraviolet-resistant layer not only further enhances the integral strength of the sheet, but also has good ultraviolet-resistant transmission performance, and widens the use effect of the PET sheet; the antibacterial hydrophilic coating uses quaternized N, N-dimethylethylenediamine as an antibacterial agent, and has a good antibacterial effect; the ultraviolet radiation grafting treatment of the PET film does not influence the performance of PET, and has good ultraviolet resistance, wear resistance and other properties.
Description
Technical Field
The invention relates to the technical field of PET materials, in particular to an antibacterial and anti-aging PET sheet and a preparation method thereof.
Background
Polyethylene terephthalate (PET) is prepared by exchange of dimethyl terephthalate and ethylene glycol or esterification of terephthalic acid and ethylene glycol to synthesize dihydroxy ethyl terephthalate, and then polycondensation reaction. The polyester belongs to crystalline saturated polyester, is a milky white or light yellow highly crystalline polymer, has smooth and glossy surface, is a common resin in life, and can be divided into APET, RPET and PETG. The material has excellent physical and mechanical properties in a wide temperature range, the long-term use temperature can reach 120 ℃, the electrical insulation property is excellent, and even under high temperature and high frequency, the electrical property is still good, but the corona resistance, the creep resistance, the fatigue resistance, the friction resistance and the dimensional stability are good.
The polyester material has the advantages of high strength, large modulus, small elongation, good heat resistance, impact resistance, good fatigue resistance and the like, can be widely applied to high-pressure hose, industrial cloth, geogrids, waterproof materials, cord fabric, advertising lamp box cloth, membrane structure materials for buildings, hoisting belts, airbags, covering cloth, conveying belts, other reinforcing materials and the like, and is a good material for a plurality of industrial textiles.
However, the industrial textile made of polyester material is easy to age by light in the outdoor application process, and the application range of the industrial textile is limited to a certain extent. In the application process of the polyester material in the industrial fields of outdoor advertising lamp box cloth, covering cloth and the like, the polyester material needs to be tested under the environmental conditions of sunlight, heat, oxygen, water and the like, wherein the ultraviolet aging resistance is an important index for measuring the durability of the outdoor polyester material. At present, the research on the ultraviolet aging resistance modification of polyester materials is extremely important.
In summary, it is important in the art to improve the antibacterial property and the light aging resistance of the polyester sheet. Therefore, the invention researches an antibacterial and anti-aging PET sheet and a preparation method thereof.
Disclosure of Invention
Aiming at the technical problems, the invention aims to overcome the defects of the prior art and provide an antibacterial and anti-aging PET sheet and a preparation method thereof,
the technical scheme adopted by the invention is as follows:
an antibacterial and aging-resistant PET sheet comprises a PET base layer.
The PET base layer is a microporous PET base layer, and the top of the PET base layer is provided with an antibacterial hydrophilic coating;
an anti-ultraviolet layer is fixedly arranged on one side, away from the antibacterial hydrophilic coating, of the PET base layer through a transparent PET composite adhesive layer, and a PET film is arranged at the bottom of the anti-ultraviolet layer;
the material of the anti-ultraviolet layer is anti-ultraviolet transparent PET.
A preparation method of an antibacterial and aging-resistant PET sheet comprises the following steps:
s1 preparation of PET base layer
1) Preparing raw materials: pretreating a PET sheet and preparing a foaming agent base material;
2) pretreatment: placing the PET sheet in an electrothermal blowing drying oven, carrying out annealing heat treatment on the sheet at a certain temperature and for a certain time, then reducing the temperature in the electrothermal blowing drying oven to room temperature, and taking out the sheet to obtain an annealed PET sheet;
3) Die pressing: putting the heat-treated PET sheet and the foaming agent base material into a mold cavity, placing on a mold press with constant temperature, applying certain pressure, quickly releasing pressure after a period of time, quickly taking out the foamed sample from the mold, and cooling to obtain the microporous foamed PET sheet and obtain the PET base layer.
S2 preparation of ultraviolet-resistant layer
1) The ultraviolet-resistant layer is composed of the following raw materials in parts by mass: 100 parts by mass of PET, 1 part by mass of dimethyl 4-methoxyphenylmethylenemalonate; uniformly mixing and drying the raw materials of the ultraviolet-resistant layer until the water content of the raw materials is lower than 50 ppm;
2) and (3) placing the raw material mixture in the previous step into a PET (polyethylene terephthalate) extrusion sheet machine for extrusion molding to obtain the anti-ultraviolet layer.
S3, bonding and fixing the PET base layer and the ultraviolet resistant layer
And uniformly coating transparent PET composite glue on the surface of the PET base layer, which is contacted with the anti-ultraviolet layer, to obtain a transparent PET composite glue layer, and stably fixing the anti-ultraviolet layer on the PET base layer by using a molding press.
S4 application of antibacterial hydrophilic coating
And uniformly coating the antibacterial hydrophilic coating on one side of the PET basic layer, which is far away from the ultraviolet-resistant layer, and air-drying at normal temperature to obtain the antibacterial PET sheet.
S5 preparation of PET film
The method comprises the following steps of cleaning the PET film by a Soxhlet extraction method, and then carrying out acrylamide ultraviolet radiation grafting treatment on the PET film, wherein the method comprises the following specific steps:
cleaning a PET film → drying the film → swelling m-cresol → cleaning → ultraviolet radiation → cleaning → drying → packaging.
S6, hot-pressing pad pasting
And finally, attaching the PET film to the surface of the anti-ultraviolet layer on the side, away from the antibacterial hydrophilic coating, of the antibacterial PET sheet obtained in the step S4, and fixing the antibacterial PET sheet by utilizing a hot pressing process to obtain the antibacterial anti-aging PET sheet.
On the basis of and as a preferred embodiment of the above embodiment, in step S1, the foaming agent substrate is prepared from low-density polyethylene, foaming agent Azodicarbonamide (AC) and crosslinking agent dicumyl peroxide (DCP) in a ratio of 1-5: 2-15: 2-6, uniformly mixing on a constant-temperature double-roller open mill, discharging and cutting into sheets to obtain the foaming agent base material.
On the basis of the scheme and as a preferable scheme of the scheme, the length-diameter ratio of a screw of the extrusion sheet machine in the step S2 is 28-36, the melt extrusion temperature of the extrusion sheet machine is 265-275 ℃, and at the same time of ensuring that the performance of raw materials is not influenced,
on the basis of the scheme, as a preferable scheme of the scheme, the antibacterial hydrophilic coating is a coating which is formed by combining catechol and APTES and has an adhesive property and a cross-linked network structure, and 20-100 parts of quaternized N, N-dimethylethylenediamine is added into the coating to serve as an antibacterial agent, so that the antibacterial hydrophilic coating is ensured to be stably bonded and fixed on the sheet, and has a good antibacterial hydrophilic effect.
The beneficial effects of the invention are:
compared with the prior art, the antibacterial anti-aging PET sheet disclosed by the invention has the advantages that the microporous foamed PET is used as a PET base layer, and the effects of light weight and high strength are achieved under the same conditions; the PET material of the anti-ultraviolet layer not only further enhances the overall strength of the sheet, but also has good anti-ultraviolet transmission performance, and widens the use effect of the PET sheet; the antibacterial hydrophilic coating uses quaternized N, N-dimethylethylenediamine as an antibacterial agent, and has a good antibacterial effect; the ultraviolet radiation grafting treatment of the PET film does not influence the performance of PET, and has good ultraviolet resistance, wear resistance and other properties. The antibacterial and ageing-resistant PET sheet produced by the invention has good ultraviolet resistance and ageing resistance, and the added auxiliary agent is tasteless and nontoxic and is green and environment-friendly.
Drawings
FIG. 1 is a schematic structural view of a PET sheet according to the invention;
FIG. 2 is an ultraviolet radiation device;
FIG. 3 is a reaction equation for the synthesis of quaternized N, N-dimethylethylenediamine as an antimicrobial agent.
In the figure, 1-PET base layer; 2-antibacterial hydrophilic coating; 3-transparent PET composite glue layer; 4-an anti-ultraviolet layer; 5-PET film; 6-an ultraviolet lamp; 7-a reaction vessel; 8-sample base station.
Detailed Description
The present invention will be further described with reference to specific examples, which are intended to clearly and completely describe the technical solutions in the examples of the present invention, and it should be understood that the described examples are only a part of the examples of the present invention, and not all of the examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following describes the method for testing and evaluating each index of the present invention:
(1) antibacterial property test of PET sheet
Refer to the antibacterial test of the high polymer material sticking film method. The antibacterial test by the film pasting method specifically comprises the steps of cutting a sample into sample pieces with the size of 2 multiplied by 2cm, soaking the sample pieces in phosphate buffer solution for 0, 1, 3, 5 and 7 days respectively, taking out the sample pieces, and cleaning the sample pieces with medical alcohol. The specific operation steps of the detection operation of the film pasting method are as follows:
and (4) sterilizing the cleaned sheet under an ultraviolet lamp, and using the sterilized sheet after sterilization. The operation of the sticking film method is that the original bacterial liquid cultured before is diluted to 5 xI 0 by Luria-Bertani bacterial culture medium5CFU/mL is to be used (CFU, colony forming unit). And then putting the cut sheet into six-hole plates, wherein the first hole of each six-hole plate is a pure bacteria liquid control sample, the other holes are sheet samples, the PET sheet samples with the same size and thickness are taken as a PET sheet control group, and the sheet samples in the embodiment are experimental groups. Each set of samples was tested in 3 replicates. And dripping 32L of diluted bacteria liquid in the middle of the PET sheet sample in each hole by using a pipette gun, and then covering the diluted bacteria liquid by using a cover glass to ensure that the sample is uniformly covered on the surface of the material. Breeding for 24 hours at 37 ℃, adding 5mL of phosphate buffer solution into each well, repeatedly washing the cover slips and the bacteria on the surfaces of the cover slips, then shaking for half an hour in a shaking table to enable the bacteria to be washed into the phosphate buffer solution from the sheets and the cover slips, and enabling the bacteria in the phosphate buffer solution to be distributed more uniformly; diluting the diluted bacterial liquid in the six-hole plate by 400 times by using a phosphate buffer solution, and then uniformly coating 50uL of the diluted bacterial liquid on the surface of a solid culture medium with the diameter of 9cm by using a spiral plate paving instrument. And after 24h, photographing, counting and calculating. The calculation formula is as follows:
Wherein, CFUcRefers to the number of colonies on the surface of the control group, CFUqMeans thatAnd the number of surviving colonies on the surface of the sample.
(2) Light aging resistance of PET sheet
Firstly, the ultraviolet transmittance is calculated and calibrated by using a digital ultraviolet tester-UV-340 for measurement.
(3) Yellowness index
The yellowness index YI of the PET sheet was measured with a colorimeter.
(4) Aging resistance
The aging resistance test is reflected by the retention of the elongation at break of the sample.
Elongation at break was determined according to ASTM-D882-97 as follows: the initial elongation at break (A) of the film sample was determined by first measuring the elongation at break of the film sample that had not been subjected to accelerated aging treatment0) (ii) a Placing a modified polyester film sample cut according to a standard in a sealed HAST high-pressure accelerated aging test box, and after 48 hours and 72 hours under the conditions of 121 ℃ and 100% RH of humidity, obtaining the elongation at break (taking the arithmetic mean value of at least three groups of data tested by the same sample), wherein the elongation at break of the sample after accelerated aging treatment is (A)1) The calculation formula is as follows:
retention of elongation at break ═ elongation at break after aging (A)1) Initial elongation at Break (A)0)×100％。
The present invention will be described more fully below with reference to examples and comparative examples.
Example one
As shown in fig. 1, an antibacterial aging-resistant PET sheet includes a PET base layer 1; the PET base layer 1 is a microporous PET base layer, and the top of the PET base layer 1 is provided with an antibacterial hydrophilic coating 2; an anti-ultraviolet layer 4 is fixedly arranged on one side, away from the antibacterial hydrophilic coating 2, of the PET base layer 1 through a transparent PET composite adhesive layer 3, and a PET film 5 is arranged at the bottom of the anti-ultraviolet layer 4; the material of the anti-ultraviolet layer 4 is anti-ultraviolet transparent PET.
A preparation method of an antibacterial and aging-resistant PET sheet comprises the following steps:
s1 preparation of PET base layer 1
1) Preparing raw materials: pretreating a PET sheet and preparing a foaming agent base material;
2) pretreatment: placing the PET sheet in an electrothermal blowing drying oven, carrying out annealing heat treatment on the sheet at a certain temperature and for a certain time, then reducing the temperature in the electrothermal blowing drying oven to room temperature, and taking out the sheet to obtain an annealed PET sheet;
3) die pressing: and putting the heat-treated PET sheet and the foaming agent base material into a die cavity, putting the die cavity on a die press with constant temperature, applying certain pressure, quickly releasing pressure after a period of time, quickly taking out the foaming sample from the die, and cooling to obtain the microporous foaming PET sheet to obtain the PET base layer 1.
S2 preparation of ultraviolet-resistant layer 4
1) The ultraviolet-resistant layer 4 is composed of the following raw materials in parts by mass: 100 parts by mass of PET, 1 part by mass of dimethyl 4-methoxyphenylmethylenemalonate; uniformly mixing and drying the raw materials of the ultraviolet-resistant layer 4 until the water content of the raw materials is lower than 50 ppm;
2) and (3) placing the raw material mixture in the previous step into a PET (polyethylene terephthalate) extrusion sheet machine for extrusion molding to obtain the anti-ultraviolet layer 4.
S3, bonding and fixing the PET base layer 1 and the ultraviolet-resistant layer 4
And uniformly coating transparent PET composite adhesive on one surface of the PET basic layer 1 contacted with the anti-ultraviolet layer 4 to obtain a transparent PET composite adhesive layer 3, and stably fixing the anti-ultraviolet layer 4 on the PET basic layer 1 by using a molding press.
S4 coating of antibacterial hydrophilic coating 2
And (3) uniformly coating the antibacterial hydrophilic coating 2 on one side of the PET basic layer 1, which is far away from the ultraviolet-resistant layer 4, and air-drying at normal temperature to obtain the antibacterial PET sheet.
S5 preparation of PET film 5
The method comprises the following steps of cleaning the PET film by a Soxhlet extraction method, and then carrying out acrylamide ultraviolet radiation grafting treatment on the PET film, wherein the method comprises the following specific steps:
washing a PET film → drying the film → swelling m-cresol → washing → ultraviolet radiation → washing → drying → packaging.
S6, hot-pressing pad pasting
And finally, attaching the PET film 5 to the surface of the anti-ultraviolet layer 4 on the side, away from the anti-bacterial hydrophilic coating 2, of the anti-bacterial PET sheet obtained in the step S4, and fixing the anti-bacterial PET sheet by utilizing a hot pressing process to obtain the anti-bacterial anti-aging PET sheet.
Specifically, S5 the PET film 5 is prepared by cleaning the PET film (cutting according to requirements) by a Soxhlet extraction method for 6 hours, and then drying the film in a forced air oven at 70 ℃ for 8 hours; swelling the dried film with m-cresol, cleaning with ethanol to remove excessive m-cresol on the surface of the film, placing the swollen film in a liquid-phase ultraviolet irradiation device (shown in figure 2) for ultraviolet irradiation grafting reaction, placing the film in a sample base station 8, and performing overall irradiation by an ultraviolet lamp 6 at the top; and (3) cleaning the PET film subjected to ultraviolet irradiation grafting by using an ultrasonic cleaning instrument for 3h, changing water every 15min, and then drying the cleaned film in a vacuum oven at 70 ℃ for 6 h. Wherein, the ultraviolet irradiation time of the embodiment is 60 min; the swelling temperature is 70 ℃; the concentration of the benzophenone is 0.5 mol/L; the concentration of acrylamide is 1 mol/L; the swelling time was 1 h.
Further, in step S1, the foaming agent base material is prepared from low-density polyethylene, foaming agent Azodicarbonamide (AC), and crosslinking agent dicumyl peroxide (DCP) in a ratio of 1-5: 2-15: 2-6, uniformly mixing on a constant-temperature double-roller open mill, discharging and cutting into sheets to obtain the foaming agent base material.
Further, the length-diameter ratio of the screw of the extrusion sheet machine in the step S2 is 28-36, and the melt extrusion temperature of the extrusion sheet machine is 265-275 ℃. Still further, the antibacterial hydrophilic coating 2 is a coating which is formed by combining catechol and APTES and has an adhesive property and a cross-linked network structure, and 20 parts of quaternized N, N-dimethylethylenediamine is added into the coating to serve as an antibacterial agent. Specifically, the preparation of the antibacterial hydrophilic coating 2 comprises two parts of quaternization N, N-dimethylethylenediamine preparation and coating preparation, wherein the quaternization N, N-dimethylethylenediamine preparation process comprises the following steps:
12.5g of octyl bromide and 4.4g N, N-dimethylethylenediamine were taken in a 200mL round-bottomed flask, followed by 17.0g of isopropanol. The reaction was carried out in an oil bath at 50 ℃ with a magnetic stirring speed of 450 rpm. After the reaction time is 48 hours, ethyl acetate is used as a precipitator, white precipitate is obtained through precipitation and centrifugation, the white precipitate is washed, and after the white precipitate is washed for at least three times, the white precipitate is placed in a vacuum drying oven for drying treatment for 72 hours, and the final product is obtained.
The coating of the antibacterial hydrophilic coating 2 is prepared as follows:
firstly, preparing Tris-HCl buffer solution with the pH value of 8.5, and adding catechol to prepare 2mg/mL Catechol (CA) solution. Then ethanol solution with APTES concentration of 60mg/mL is prepared. Then, APTES ethanol solution with the concentration of 60mg/mL is added into the prepared catechol-containing buffer solution, and the volume ratio of the mixture of the CA solution and the APTES solution is 10: 1. Then, Tris-HCl buffer solution containing quaternized N, N-dimethylethylenediamine with the same volume as the APTES solution was added. Wherein the concentration of the quaternized N, N-dimethylethylenediamine is 20-100 mg/mL. After the mixed solution was prepared, the sheet was immersed in the solution and reacted for 6 hours in a shaker. And (3) alternately washing the reacted sheet by using ethanol and deionized water, repeating the washing for at least five times, soaking the sheet in a deionized water environment for 12 hours, and finally naturally drying the PVC material for testing, wherein the reaction principle is shown in figure 3.
Still further, the temperature and roller speed parameters of each zone of the PET extrusion sheet machine of the ultraviolet-resistant layer 4 are shown in the following table:
TABLE 1
Example two
An antibacterial and aging-resistant PET sheet comprises a PET base layer 1; the PET base layer 1 is a microporous PET base layer, and the top of the PET base layer 1 is provided with an antibacterial hydrophilic coating 2; an anti-ultraviolet layer 4 is fixedly arranged on one side, away from the antibacterial hydrophilic coating 2, of the PET base layer 1 through a transparent PET composite adhesive layer 3, and a PET film 5 is arranged at the bottom of the anti-ultraviolet layer 4; the material of the anti-ultraviolet layer 4 is anti-ultraviolet transparent PET.
A preparation method of an antibacterial and aging-resistant PET sheet comprises the following steps:
s1 preparation of PET base layer 1
1) Preparing raw materials: pretreating a PET sheet and preparing a foaming agent base material;
2) pretreatment: placing the PET sheet in an electrothermal blowing drying oven, carrying out annealing heat treatment on the sheet at a certain temperature and for a certain time, then reducing the temperature in the electrothermal blowing drying oven to room temperature, and taking out the sheet to obtain an annealed PET sheet;
3) die pressing: and putting the heat-treated PET sheet and the foaming agent base material into a die cavity, putting the die cavity on a die press with constant temperature, applying certain pressure, quickly releasing pressure after a period of time, quickly taking out the foaming sample from the die, and cooling to obtain the microporous foaming PET sheet to obtain the PET base layer 1.
S2 preparation of ultraviolet-resistant layer 4
1) The ultraviolet-resistant layer 4 is composed of the following raw materials in parts by mass: 100 parts by mass of PET, 1 part by mass of dimethyl 4-methoxyphenylmethylenemalonate; uniformly mixing and drying the raw materials of the ultraviolet-resistant layer 4 until the water content of the raw materials is lower than 50 ppm;
2) and (3) placing the raw material mixture in the previous step into a PET (polyethylene terephthalate) extrusion sheet machine for extrusion molding to obtain the anti-ultraviolet layer 4.
S3, bonding and fixing the PET base layer 1 and the ultraviolet-resistant layer 4
And uniformly coating transparent PET composite adhesive on the surface of the PET base layer 1, which is in contact with the anti-ultraviolet layer 4, to obtain a transparent PET composite adhesive layer 3, and then stably fixing the anti-ultraviolet layer 4 on the PET base layer 1 by using a mould press.
S4 coating of antibacterial hydrophilic coating 2
And (3) uniformly coating the antibacterial hydrophilic coating 2 on one side of the PET basic layer 1, which is far away from the ultraviolet-resistant layer 4, and air-drying at normal temperature to obtain the antibacterial PET sheet.
S5 preparation of PET film 5
The method comprises the following steps of cleaning the PET film by a Soxhlet extraction method, and then carrying out acrylamide ultraviolet radiation grafting treatment on the PET film, wherein the method comprises the following specific steps:
washing a PET film → drying the film → swelling m-cresol → washing → ultraviolet radiation → washing → drying → packaging.
S6, hot-pressing pad pasting
And finally, attaching the PET film 5 to the surface of the anti-ultraviolet layer 4 on the side, away from the anti-bacterial hydrophilic coating 2, of the anti-bacterial PET sheet obtained in the step S4, and fixing the anti-bacterial PET sheet by utilizing a hot pressing process to obtain the anti-bacterial anti-aging PET sheet.
The preparation parameters of the PET film 5 of S5 in this example are: the ultraviolet irradiation time is 60 min; the swelling temperature is 70 ℃; the concentration of the benzophenone is 0.5 mol/L; the concentration of acrylamide is 1 mol/L; the swelling time was 1 h.
Further, in step S1, the foaming agent base material is prepared from low-density polyethylene, foaming agent Azodicarbonamide (AC), and crosslinking agent dicumyl peroxide (DCP) in a ratio of 1-5: 2-15: 2-6, uniformly mixing on a constant-temperature double-roller open mill, discharging and cutting into sheets to obtain the foaming agent base material.
Further, the antibacterial hydrophilic coating 2 is a coating which is formed by combining catechol and APTES and has an adhesive property and a cross-linked network structure, and 60 parts of quaternized N, N-dimethylethylenediamine is added in the coating to serve as an antibacterial agent.
EXAMPLE III
In this embodiment, ordinary PET master batches are melt-blended to serve as a blank control group, sheet preparation is performed according to the same sheet preparation process as in the first embodiment, and transparent PET composite glue is used for sheet bonding, so that the final sheet has the same size as that in the first embodiment.
The antibacterial property test of the PET sheet, and the performance tests of the PET sheet in terms of light aging resistance, yellowness index, aging resistance, and the like will be further analyzed below. Table 2 shows the antibacterial property test data of the PET sheet:
table 2 antimicrobial property test of PET sheet
As can be seen from table 2, the greater the amount of N, N-dimethylethylenediamine added as an antimicrobial agent, the less bacterial coverage of the sheet surface and no biofilm were formed, indicating that the higher the antimicrobial rate was, and the less bacterial adhesion was. As the quaternary ammonium salt has excellent and efficient antibacterial performance, the quaternized N, N-dimethylethylenediamine can be used as an antibacterial agent to realize antibacterial modification of polyester, and endow PET with good antibacterial hydrophilic performance, so that the PET has the characteristics of good antibacterial performance and biocompatibility. In an antibacterial test, the modified antibacterial and anti-aging PET sheet still has antibacterial performance on staphylococcus aureus after being soaked in phosphate buffer solution for 7 days, and can effectively reduce bacterial adhesion and inhibit the formation of a biological film.
The following are the light transmission performance test data of the sheet of the present invention, and the specific data are shown in table 3:
TABLE 3 sheet light transmission Performance test
As can be seen from table 3, in the third comparative example, the ultraviolet-resistant layer 4 made of the ultraviolet-resistant transparent PET material endows the sheet with good ultraviolet resistance, and the ultraviolet shielding rate exceeds 93%; the high level of quaternized N, N-dimethylethylenediamine antimicrobial agent of example two imparts a coating thickness to the sheet that further enhances the uv resistance to some extent as compared to example one.
Table 4 shows the yellowness index and elongation at break retention test data of the PET sheet of the present invention, as shown in table 4:
TABLE 4 yellowness index and elongation at break retention test of PET sheets
As can be seen from table 4, the antibacterial hydrophilic coating 2 having quaternized N, N-dimethylethylenediamine as an antibacterial agent can stably exist during processing without problems such as discoloration; but also can ensure better elongation at break.
In conclusion, tables 2 to 4 show that the uvioresistant performance of the uvioresistant PET is far better than that of the common PET, and the added quaternized N, N-dimethylethylenediamine as an antibacterial agent has higher melting point, can stably exist at the PET processing temperature, does not generate color change or other chemical reactions, and therefore does not influence the transparency of sheets in the processing process. As can be seen from Table 6, the product of the invention has better light transmittance, and the auxiliary agent is nontoxic, so that the finally produced uvioresistant PET transparent sheet is nontoxic and environment-friendly.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations can be devised by those skilled in the art in light of the above teachings. Therefore, the technical solutions that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the prior art according to the concepts of the present invention should be within the scope of protection determined by the claims.
Claims (5)
1. An antibacterial and ageing-resistant PET sheet comprising a PET base layer (1), characterized in that:
the PET base layer (1) is a microporous PET base layer, and the top of the PET base layer (1) is provided with an antibacterial hydrophilic coating (2);
an anti-ultraviolet layer (4) is fixedly arranged on one side, away from the antibacterial hydrophilic coating (2), of the PET basic layer (1) through a transparent PET composite adhesive layer (3), and a PET thin film (5) is arranged at the bottom of the anti-ultraviolet layer (4);
the material of the anti-ultraviolet layer (4) is anti-ultraviolet transparent PET.
2. The method for preparing the antibacterial and aging-resistant PET sheet according to claim 1, comprising the following steps:
s1 preparation of PET base layer (1)
1) Preparing raw materials: pretreating a PET sheet and preparing a foaming agent base material;
2) pretreatment: placing the PET sheet in an electrothermal blowing drying oven, carrying out annealing heat treatment on the sheet at a certain temperature and for a certain time, then reducing the temperature in the electrothermal blowing drying oven to room temperature, and taking out the sheet to obtain an annealed PET sheet;
3) die pressing: and putting the heat-treated PET sheet and the foaming agent base material into a die cavity, putting the die cavity on a die press with constant temperature, applying certain pressure, quickly releasing pressure after a period of time, quickly taking out the foaming sample from the die, and cooling to obtain the microporous foaming PET sheet to obtain the PET base layer (1).
S2 preparation of ultraviolet-resistant layer (4)
1) The ultraviolet-resistant layer (4) is composed of the following raw materials in parts by mass: 100 parts by mass of PET, 1 part by mass of dimethyl 4-methoxyphenylmethylenemalonate; uniformly mixing and drying the raw materials of the ultraviolet-resistant layer (4) until the water content of the raw materials is lower than 50 ppm;
2) and (3) placing the raw material mixture in the previous step into a PET (polyethylene terephthalate) extrusion sheet machine for extrusion molding to obtain the anti-ultraviolet layer (4).
S3, and the PET basic layer (1) and the ultraviolet resistant layer (4) are bonded and fixed
And uniformly coating transparent PET composite glue on the surface of the PET base layer (1) contacted with the anti-ultraviolet layer (4) to obtain a transparent PET composite glue layer (3), and stably fixing the anti-ultraviolet layer (4) on the PET base layer (1) by using a mould press.
S4 application of antibacterial hydrophilic coating (2)
And (3) uniformly coating the antibacterial hydrophilic coating (2) on one side of the PET basic layer (1) far away from the anti-ultraviolet layer (4), and air-drying at normal temperature to obtain the antibacterial PET sheet.
S5 production of PET film (5)
The method comprises the following steps of cleaning the PET film by a Soxhlet extraction method, and then carrying out acrylamide ultraviolet radiation grafting treatment on the PET film, wherein the method comprises the following specific steps:
washing a PET film → drying the film → swelling m-cresol → washing → ultraviolet radiation → washing → drying → packaging.
S6, hot-pressing pad pasting
And finally, the PET film (5) is attached to the surface of the anti-ultraviolet layer (4) on the side, away from the anti-bacterial hydrophilic coating (2), of the anti-bacterial PET sheet obtained in the step S4, and the anti-bacterial anti-aging PET sheet is fixed by utilizing a hot pressing process to obtain the anti-bacterial anti-aging PET sheet.
3. The antibacterial and aging-resistant PET sheet and the preparation method thereof according to claim 2, wherein the foaming agent substrate of step S1 is prepared from low density polyethylene, foaming agent Azodicarbonamide (AC) and crosslinking agent dicumyl peroxide (DCP) according to the mixture ratio of 1-5: 2-15: 2-6, uniformly mixing on a constant-temperature double-roller open mill, discharging and cutting into sheets to obtain the foaming agent base material.
4. The antibacterial and anti-aging PET sheet as claimed in claim 2, wherein the length/diameter ratio of the screw of the extrusion sheet machine in the step S2 is 28-36, and the melt extrusion temperature of the extrusion sheet machine is 265-275 ℃.
5. The antibacterial and aging-resistant PET sheet and the preparation method thereof according to claim 1, wherein the antibacterial hydrophilic coating (2) is a coating which is a combination of catechol and APTES and has a cross-linked network structure and has an adhesive property, and 20-100 parts of quaternized N, N-dimethylethylenediamine is added in the coating as an antibacterial agent.
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