CN117681522A - Antibacterial film of compound paper and preparation method thereof - Google Patents
Antibacterial film of compound paper and preparation method thereof Download PDFInfo
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- CN117681522A CN117681522A CN202311854456.XA CN202311854456A CN117681522A CN 117681522 A CN117681522 A CN 117681522A CN 202311854456 A CN202311854456 A CN 202311854456A CN 117681522 A CN117681522 A CN 117681522A
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- antibacterial
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 66
- 150000001875 compounds Chemical class 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001125 extrusion Methods 0.000 claims abstract description 60
- 239000002994 raw material Substances 0.000 claims abstract description 54
- 229920005629 polypropylene homopolymer Polymers 0.000 claims abstract description 24
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 15
- 238000004806 packaging method and process Methods 0.000 claims abstract description 12
- 239000002216 antistatic agent Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 91
- 238000002156 mixing Methods 0.000 claims description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000002981 blocking agent Substances 0.000 claims description 24
- 238000005520 cutting process Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000000155 melt Substances 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 10
- 238000007493 shaping process Methods 0.000 claims description 10
- 239000004743 Polypropylene Substances 0.000 claims description 9
- -1 polypropylene Polymers 0.000 claims description 9
- 229920001155 polypropylene Polymers 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000009966 trimming Methods 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 238000001746 injection moulding Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- 230000036541 health Effects 0.000 abstract description 6
- 244000000010 microbial pathogen Species 0.000 abstract description 6
- 239000012620 biological material Substances 0.000 abstract description 2
- 230000001580 bacterial effect Effects 0.000 description 12
- 238000012258 culturing Methods 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 238000009499 grossing Methods 0.000 description 9
- 241000588724 Escherichia coli Species 0.000 description 8
- 241000191967 Staphylococcus aureus Species 0.000 description 8
- 238000006073 displacement reaction Methods 0.000 description 8
- 238000001514 detection method Methods 0.000 description 6
- 238000011534 incubation Methods 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- 238000009864 tensile test Methods 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 4
- 230000000845 anti-microbial effect Effects 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 230000003044 adaptive effect Effects 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000007655 standard test method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 208000035473 Communicable disease Diseases 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
- B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a compound paper antibacterial film and a preparation method thereof, and relates to the technical field of synthetic biological materials, wherein the compound paper antibacterial film comprises an auxiliary layer, a main extrusion layer and an auxiliary layer; the auxiliary raw material is prepared from the following components in parts by weight: homo-polypropylene: 90-98 wt%; antiblocking agent: 2-10wt%; the main extrusion layer raw material is prepared from the following components in parts by weight: homo-polypropylene: 90-93 wt%; antibacterial agent: 6 to 9 weight percent; antistatic agent: 1 to 3 weight percent; the auxiliary two-layer raw material is prepared from the following components in parts by weight: homo-polypropylene: 88-96 wt%; antiblocking agent: 4-12 wt%. The double-paper antibacterial film provided by the invention can effectively reduce the threat of pathogenic microorganisms to human health and safety, and provides safer and more sanitary food packaging and book use experience.
Description
Technical Field
The invention relates to the technical field of synthetic biological materials, in particular to a compound paper antibacterial film and a preparation method thereof.
Background
Due to the continuous improvement of the technological level and the continuous increase of economy, people consciously have the ability to catch up for higher life quality, and along with the threat of pathogenic microorganisms to human health safety, the requirements of people on the antibacterial functionality of food and book packaging are also growing;
the antibacterial film is used for protecting books and preventing fungus from breeding and spreading, and is helpful for keeping the surfaces of the books clean and sanitary, especially in the dense environments of public places, libraries, schools and the like, books are easy to be polluted by various bacteria and viruses, and the risk of infectious diseases can be reduced and safer and more sanitary book use experience is provided by applying the antibacterial film;
the paper-coated film for food outer cartons is a film material applied to food outer packaging, and is generally used for wrapping the surface of the food outer cartons so as to provide protection and sanitary barrier for food.
At present, the technical field of the compound paper antibacterial film generally has the advantages of shorter persistence of antibacterial performance, excessively obvious reduction of the antibacterial performance of the compound paper antibacterial film after long-time use, lower glossiness, dimness and insufficient load intensity, and easy tensile deformation. Therefore, we propose a double paper antibacterial film and a preparation method thereof to solve the problems in the prior art.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide a compound paper antibacterial film and its preparation method, which aims to solve the above problems.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the compound paper antibacterial film comprises an auxiliary layer, a main extrusion layer and an auxiliary layer;
the auxiliary raw material is prepared from the following components in parts by weight:
homo-polypropylene: 90-98 wt%;
antiblocking agent: 2-10wt%;
the main extrusion layer raw material is prepared from the following components in parts by weight:
homo-polypropylene: 90-93 wt%;
antibacterial agent: 6 to 9 weight percent;
antistatic agent: 1 to 3 weight percent;
the auxiliary two-layer raw material is prepared from the following components in parts by weight:
homo-polypropylene: 88-96 wt%;
antiblocking agent: 4-12 wt%;
the anti-blocking agent is a silicon dioxide anti-blocking agent, and the antibacterial agent is at least one of a silver ion antibacterial agent and a titanium dioxide antibacterial agent.
The preparation method of the compound paper antibacterial film comprises the following steps:
step one: mixing the raw materials of all layers of products;
step two: heating, melting and filtering the raw materials of each layer through an extruder;
step three: carrying out injection molding extrusion molding on the melt after melting and filtering through a die head;
step four: carrying out water cooling solidification crystallization on the extrusion molding product, and carrying out water removal treatment on the molding product;
step five: longitudinally stretching and shaping the formed thick sheet through the speed difference of each roller after the formed thick sheet is heated by the roller;
step six: transversely stretching and shaping the longitudinally stretched thick sheet by heating through an oven;
step seven: trimming, surface high-pressure impact treatment and rolling are carried out on the film which is transversely stretched;
step eight: and cutting, packaging and warehousing the rolled product.
As a preferred embodiment, in step one, a secondary layer is prepared: sequentially adding the homopolymerized polypropylene and the anti-blocking agent into a first mixing container according to the weight fraction ratio of an auxiliary layer;
preparing a main extrusion layer: sequentially adding the homopolymerized polypropylene, the antibacterial agent and the antistatic agent into a second mixing container according to the weight fraction ratio of the main extrusion layer;
preparing an auxiliary two-layer: sequentially adding the homopolymerized polypropylene and the anti-blocking agent into a third mixing container according to the weight fraction ratio of the auxiliary layer to the auxiliary layer;
the first mixing vessel, the second mixing vessel and the third mixing vessel were mixed separately, and after the completion of the mixing, the mixture was introduced into an extruder.
In the second and third steps, the raw materials of the main extrusion layer, the auxiliary first layer and the auxiliary second layer are sequentially heated and melted by an extruder, wherein the heating temperature of the auxiliary first layer is 170-240 ℃ and the heating time is 45-60 min; the heating temperature of the main extrusion layer is 110 ℃ to 150 ℃ and the heating time is 25min to 45min; the heating temperature of the auxiliary two layers is 170 ℃ to 240 ℃ and the heating time is 45min to 60min; the main extrusion layer, the auxiliary first layer and the auxiliary second layer are filtered through the filter to remove impurities and particles in the melt, and the filtered auxiliary first layer, the filtered main extrusion layer and the filtered auxiliary second layer are sequentially pushed into the die and the die head for shaping.
In a preferred scheme, in the fourth step, after the melts of the auxiliary first layer, the main extrusion layer and the auxiliary second layer are sequentially filled in the cavity of the die, the molded product is rapidly solidified and solidified in a water cooling mode.
As a preferred scheme, in the fifth and sixth steps, the formed thick sheet is first longitudinally stretched and shaped by one set of heating rollers, and in the stretching and shaping process, one set of the heating rollers has a heating temperature of 70 ℃ to 100 ℃, then the formed thick sheet is transversely stretched and shaped by the other set of heating rollers, and in the stretching and shaping process, the other set of heating rollers has a heating temperature of 70 ℃ to 100 ℃.
In a seventh step, the formed sheet after the stretching in the longitudinal and transverse directions is cut and trimmed, and the dimensions after cutting are as follows: 80 cm.50cm, then smooth and punch the formed sheet by a punch, and roll the formed sheet after punching.
In a preferred embodiment, in step eight, slitting is performed by a slitter during winding so that the lengths of each roll are uniform, followed by a packaging process.
As a preferable scheme, the double-paper antibacterial film is applied to book paper composite and food packaging composite materials.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and particularly, the technical scheme mainly comprises the following steps;
the antibacterial film of the composite paper provided by the invention has more than 99% of antibacterial property to escherichia coli and staphylococcus aureus, the high glossiness of the antibacterial film of the composite paper can be reflected by the detection according to different detection angles when the glossiness of the prepared antibacterial film of the composite paper is detected, and the displacement distance of the antibacterial film of the composite paper after stretching is within 1 millimeter according to different stretching times in the stretching detection process of the antibacterial film of the composite paper, so that the antibacterial film of the composite paper has high load strength;
due to the continuous improvement of the technological level and the continuous increase of economy, people consciously have the ability to catch up for higher life quality, along with the threat of pathogenic microorganisms to human health safety, the requirements of people on the antibacterial functionality of food and book packaging are also growing, the invention can effectively reduce the threat of pathogenic microorganisms to human health safety, and provide safer and more sanitary food packaging and book use experience.
In order to more clearly illustrate the structural features and efficacy of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a multi-ply antimicrobial film according to an embodiment of the invention;
FIG. 2 is a physical view of a transfer film according to an embodiment of the present invention.
Detailed Description
For the purpose of making the technical solution and advantages of the present invention more apparent, the present invention will be further described in detail below with reference to the accompanying drawings and examples of implementation. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
It will be understood that when an element is referred to as being "fixed to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like are used herein for illustrative purposes only.
The invention is further described below with reference to examples.
Example 1
The weight fraction of the auxiliary layer of raw materials is shown in Table 1, the weight fraction of the main extrusion layer of raw materials is shown in Table 2, and the weight fraction of the auxiliary layer of raw materials is shown in Table 3.
TABLE 1 auxiliary layer raw material composition of example 1
| Component (A) | Mass fraction |
| Homo-polypropylene | 90％ |
| Silicon dioxide anti-blocking agent | 2％ |
TABLE 2 Main extrusion layer raw Material composition of example 1
| Component (A) | Mass fraction |
| Homo-polypropylene | 90％ |
| Silver ion antibacterial agent | 6％ |
| Antistatic agent | 1％ |
TABLE 3 auxiliary two layer raw material composition of example 1
| Component (A) | Mass fraction |
| Homo-polypropylene | 88％ |
| Silicon dioxide anti-blocking agent | 4％ |
The preparation method of the compound paper antibacterial film comprises the following steps:
step one: preparing an auxiliary layer: adding homo-polypropylene and an anti-blocking agent into a first mixing container according to the weight fraction ratio of an auxiliary layer in table 1;
preparing a main extrusion layer: sequentially adding the homopolymerized polypropylene, the antibacterial agent and the antistatic agent into a second mixing container according to the weight fraction ratio of the main extrusion layer in the table 2;
preparing an auxiliary two-layer: sequentially adding the homopolypropylene and the anti-blocking agent into a third mixing container according to the weight fraction ratio of the auxiliary two layers in the table 3;
respectively mixing the first mixing container, the second mixing container and the third mixing container, and introducing the mixture into an extruder after the mixing is finished, wherein the stirring time is 15min;
step two: sequentially heating and melting the raw materials of the main extrusion layer, the auxiliary first layer and the auxiliary second layer through an extruder, wherein the heating temperature of the auxiliary first layer raw material is 190 ℃, and the heating time is 50min; the heating temperature of the main extrusion layer raw material is 130 ℃, and the heating time is 35min; the heating temperature of the auxiliary two-layer raw material is 190 ℃, and the heating time is 50min;
preparing a melt from the heated main extrusion layer, the auxiliary first layer and the auxiliary second layer of raw materials, and introducing the melt and the raw materials into an independent filter for filtering to remove impurities and insufficiently melted particles in the raw materials;
step three: leading the filtered auxiliary layer into a die to be smoothed, wherein the smoothed auxiliary layer is 500cm in length, 80cm in width and 30 mu m in height; introducing the filtered main extrusion layer into a die, covering an auxiliary layer for smoothing, wherein the length of the smoothed main extrusion layer is 500cm, the width of the smoothed main extrusion layer is 80cm, and the height of the smoothed main extrusion layer is 25 mu m; introducing the filtered auxiliary two layers into a die, covering the main extrusion layer for smoothing, wherein the smoothed auxiliary two layers have the length of 500cm, the width of 80cm and the height of 30 mu m;
step four: after the three layers of melt are overlapped, water cooling is carried out on the die outside the die, so that the antibacterial film is convenient to withdraw the film;
step five: after film withdrawal is completed, the formed thick sheet is pressed by a longitudinal stretching heating roller, and is pressed in the heating process, and then the formed thick sheet is stretched by the longitudinal stretching heating roller, wherein the speed difference ratio of front roller to rear roller in the longitudinal heating roller is as follows: 0.2, wherein the heating temperature of the longitudinal heating roller is about 80 ℃;
step six: pressing the formed thick sheet through a transverse stretching heating roller, pressing the formed thick sheet in the heating process, and stretching the formed thick sheet through the transverse stretching heating roller, wherein the speed difference ratio of front roller to rear roller in the transverse heating roller is as follows: 0.3, wherein the heating temperature of the transverse heating roller is kept consistent with the heating temperature of the longitudinal heating roller;
step seven: after the stretching is finished, cutting and trimming the formed sheet, and then smoothing and stamping the formed sheet by a stamping machine to obtain the double-paper antibacterial film.
Antibacterial test: reference is made to ISO 22196:2011 methods for measuring antimicrobial activity of plastics and other non-porous surfaces
S101, sample preparation: cutting three groups of square samples I with 15cm x 15cm of the antibacterial film of the paper, and cleaning the upper surface and the lower surface of the square samples I;
s102, selecting a designated strain: according to the requirements of ISO 22196 standard, staphylococcus aureus and escherichia coli are selected;
s103, preparing bacterial liquid: selecting an adaptive culture dish, and culturing staphylococcus aureus and escherichia coli to a growth stage;
s104, processing a sample: exposing the first sample to the bacterial liquid under aseptic conditions in a soaking mode to ensure that the bacterial liquid is fully contacted with the sample;
s105, incubation: culturing the first group of treated samples under the proper temperature and humidity for 12 hours, culturing the second group of treated samples under the proper temperature and humidity for 24 hours, and culturing the third group of treated samples under the proper temperature and humidity for 21 days;
s106, eluting: after incubation, residual bacterial liquid is washed away with a proper buffer solution, ensuring that adsorbed, adsorbed or sterilized bacteria remain;
s106, counting the eluted colonies by a culture medium plate counting method, and measuring the following table 4:
high gloss test: reference ASTM D523-17 specular gloss Standard test method
S201, cutting a stained or scratched compound paper antibacterial film into a square sample II with the length of 20cm x 20cm, and calibrating a gloss meter;
s202, the glossiness meter emits a beam of light, and the intensity and angle of the reflected light are measured, and the following table 5 is measured:
high load intensity test: reference is made to ISO 527-3:1995 determination of Plastic-tensile Properties-part 3: test conditions for films and sheets
S301, cutting three groups of rectangular samples III with 20cm x 40cm of nondefective and nondefective antibacterial film of the double paper;
s302, accurately clamping a sample III on tensile test equipment to ensure that the sample is in a uniformly stressed state;
s303, starting a tensile test, applying a tensile force at a constant speed according to standard requirements, recording load and displacement data, and carrying out three-tensile data on a first group of samples as shown in the following table 6:
| time (seconds) | Load (Newton) | Displacement (millimeter) | |
| Third group of samples | 0 | 0 | 0 |
| Second group of samples three | 5 | 3 | 0.85 |
| Third group sample three | 10 | 3 | 0.81 |
Example 2
The weight fraction of the auxiliary layer of raw materials is shown in Table 7, the weight fraction of the main extrusion layer of raw materials is shown in Table 8, and the weight fraction of the auxiliary layer of raw materials is shown in Table 9.
TABLE 7 auxiliary layer raw material composition of example 2
| Component (A) | Mass fraction |
| Homo-polypropylene | 94％ |
| Silicon dioxide anti-blocking agent | 6％ |
TABLE 8 Main extrusion layer raw Material composition of example 2
| Component (A) | Mass fraction |
| Homo-polypropylene | 92％ |
| Silicon dioxide anti-blocking agent | 8％ |
| Silicon dioxide anti-blocking agent | 2％ |
TABLE 9 auxiliary two layer raw material composition of example 2
| Component (A) | Mass fraction |
| Homo-polypropylene | 92％ |
| Silicon dioxide anti-blocking agent | 8％ |
The preparation method of the compound paper antibacterial film comprises the following steps:
step one: preparing an auxiliary layer: adding homo-polypropylene and an anti-blocking agent into a first mixing container according to the weight fraction ratio of an auxiliary layer in table 7;
preparing a main extrusion layer: sequentially adding the homopolymerized polypropylene, the antibacterial agent and the antistatic agent into a second mixing container according to the weight fraction ratio of the main extrusion layer in table 8;
preparing an auxiliary two-layer: adding the homopolypropylene and the anti-blocking agent into a third mixing container according to the weight fraction ratio of the auxiliary two layers in the table 9;
respectively mixing the first mixing container, the second mixing container and the third mixing container, and introducing the mixture into an extruder after the mixing is finished, wherein the stirring time is 15min;
step two: sequentially heating and melting the raw materials of the main extrusion layer, the auxiliary first layer and the auxiliary second layer through an extruder, wherein the heating temperature of the auxiliary first layer raw material is 185 ℃, and the heating time is 45min; the heating temperature of the main extrusion layer raw material is 125 ℃, and the heating time is 40min; the heating temperature of the auxiliary two-layer raw material is 185 ℃ and the heating time is 45min;
preparing a melt from the heated main extrusion layer, the auxiliary first layer and the auxiliary second layer of raw materials, and introducing the melt and the raw materials into an independent filter for filtering to remove impurities and insufficiently melted particles in the raw materials;
step three: leading the filtered auxiliary layer into a die to be smoothed, wherein the length of the smoothed auxiliary layer is 50cm, the width of the smoothed auxiliary layer is 80cm, and the height of the smoothed auxiliary layer is 30 mu m; introducing the filtered main extrusion layer into a die, covering an auxiliary layer for smoothing, wherein the length of the smoothed main extrusion layer is 50cm, the width of the smoothed main extrusion layer is 80cm, and the height of the smoothed main extrusion layer is 25 mu m; introducing the filtered auxiliary two layers into a die, covering the main extrusion layer for smoothing, wherein the length of the smoothed auxiliary two layers is 50cm, the width of the smoothed auxiliary two layers is 80cm, and the height of the smoothed auxiliary two layers is 30 mu m;
step four: after the three layers of melt are overlapped, water cooling is carried out on the die outside the die, so that the antibacterial film is convenient to withdraw the film;
step five: after film withdrawal is completed, the formed thick sheet is pressed by a longitudinal stretching heating roller, and is pressed in the heating process, and then the formed thick sheet is stretched by the longitudinal stretching heating roller, wherein the speed difference ratio of front roller to rear roller in the longitudinal heating roller is as follows: 0.2, wherein the heating temperature of the longitudinal heating roller is about 80 ℃;
step six: pressing the formed thick sheet through a transverse stretching heating roller, pressing the formed thick sheet in the heating process, and stretching the formed thick sheet through the transverse stretching heating roller, wherein the speed difference ratio of front roller to rear roller in the transverse heating roller is as follows: 0.3, wherein the heating temperature of the transverse heating roller is kept consistent with the heating temperature of the longitudinal heating roller;
step seven: after the stretching is finished, cutting and trimming the formed sheet, and then smoothing and stamping the formed sheet by a stamping machine to obtain the double-paper antibacterial film.
Antibacterial test: reference is made to ISO 22196:2011 methods for measuring antimicrobial activity of plastics and other non-porous surfaces
S101, sample preparation: cutting three groups of square samples I with 15cm x 15cm of the antibacterial film of the paper, and cleaning the upper surface and the lower surface of the square samples I;
s102, selecting a designated strain: according to the requirements of ISO 22196 standard, staphylococcus aureus and escherichia coli are selected;
s103, preparing bacterial liquid: selecting an adaptive culture dish, and culturing staphylococcus aureus and escherichia coli to a growth stage;
s104, processing a sample: exposing the first sample to the bacterial liquid under aseptic conditions in a soaking mode to ensure that the bacterial liquid is fully contacted with the sample;
s105, incubation: culturing the first group of treated samples under the proper temperature and humidity for 12 hours, culturing the second group of treated samples under the proper temperature and humidity for 24 hours, and culturing the third group of treated samples under the proper temperature and humidity for 21 days;
s106, eluting: after incubation, residual bacterial liquid is washed away with a proper buffer solution, ensuring that adsorbed, adsorbed or sterilized bacteria remain;
s106, counting the eluted colonies by a culture medium plate counting method, and measuring the following table 10:
high gloss test: reference ASTM D523-17 specular gloss Standard test method
S201, cutting a stained or scratched compound paper antibacterial film into a square sample II with the length of 20cm x 20cm, and calibrating a gloss meter;
s202, the glossiness meter emits a beam of light, and the intensity and angle of the reflected light are measured, and the following table 11 is measured:
high load intensity test: reference ISO 527-3:1995 determination of Plastic-tensile Properties-section 3: test conditions for films and sheets
S301, cutting three groups of rectangular samples III with 20cm x 40cm of nondefective and nondefective antibacterial film of the double paper;
s302, accurately clamping a sample III on tensile test equipment to ensure that the sample is in a uniformly stressed state;
s303, starting a tensile test, applying a tensile force at a constant speed according to standard requirements, recording load and displacement data, and carrying out three-tensile data on a first group of samples as shown in the following table 12:
| time (seconds)) | Load (Newton) | Displacement (millimeter) | |
| Third group of samples | 0 | 0 | 0 |
| Second group of samples three | 5 | 3 | 0.92 |
| Third group sample three | 10 | 3 | 0.76 |
Example 3
The weight fractions of the auxiliary layer of raw materials are shown in Table 13, the weight fractions of the main extrusion layer of raw materials are shown in Table 14, and the weight fractions of the auxiliary layer of raw materials are shown in Table 15.
TABLE 13 auxiliary layer raw material composition of example 3
| Component (A) | Mass fraction |
| Homo-polypropylene | 98％ |
| Silicon dioxide anti-blocking agent | 10％ |
TABLE 14 Main extrusion layer raw Material composition of example 3
| Component (A) | Mass fraction |
| Homo-polypropylene | 93％ |
| Silicon dioxide anti-blocking agent | 9％ |
| Silicon dioxide anti-blocking agent | 3％ |
TABLE 15 auxiliary two-layer raw material composition of example 3
| Component (A) | Mass fraction |
| Homo-polypropylene | 96％ |
| Silicon dioxide anti-blocking agent | 12％ |
The preparation method of the compound paper antibacterial film comprises the following steps:
step one: preparing an auxiliary layer: adding homo-polypropylene and an anti-blocking agent into a first mixing container according to the weight fraction ratio of an auxiliary layer in table 13;
preparing a main extrusion layer: sequentially adding the homopolymerized polypropylene, the antibacterial agent and the antistatic agent into a second mixing container according to the weight fraction ratio of the main extrusion layer in table 14;
preparing an auxiliary two-layer: the homo-polypropylene and the anti-blocking agent are added into a third mixing container according to the weight fraction ratio of the auxiliary two layers in the table 15;
respectively mixing the first mixing container, the second mixing container and the third mixing container, and introducing the mixture into an extruder after the mixing is finished, wherein the stirring time is 15min;
step two: sequentially heating and melting the raw materials of the main extrusion layer, the auxiliary first layer and the auxiliary second layer through an extruder, wherein the heating temperature of the auxiliary first layer raw material is 195 ℃ and the heating time is 60min; the heating temperature of the main extrusion layer raw material is 135 ℃ and the heating time is 40min; the heating temperature of the auxiliary two-layer raw material is 195 ℃ and the heating time is 60min;
preparing a melt from the heated main extrusion layer, the auxiliary first layer and the auxiliary second layer of raw materials, and introducing the melt and the raw materials into an independent filter for filtering to remove impurities and insufficiently melted particles in the raw materials;
step three: leading the filtered auxiliary layer into a die to be smoothed, wherein the length of the smoothed auxiliary layer is 50cm, the width of the smoothed auxiliary layer is 80cm, and the height of the smoothed auxiliary layer is 30 mu m; introducing the filtered main extrusion layer into a die, covering an auxiliary layer for smoothing, wherein the length of the smoothed main extrusion layer is 50cm, the width of the smoothed main extrusion layer is 80cm, and the height of the smoothed main extrusion layer is 25 mu m; introducing the filtered auxiliary two layers into a die, covering the main extrusion layer for smoothing, wherein the length of the smoothed auxiliary two layers is 50cm, the width of the smoothed auxiliary two layers is 80cm, and the height of the smoothed auxiliary two layers is 30 mu m;
step four: after the three layers of melt are overlapped, water cooling is carried out on the die outside the die, so that the antibacterial film is convenient to withdraw the film;
step five: after film withdrawal is completed, the formed thick sheet is pressed by a longitudinal stretching heating roller, and is pressed in the heating process, and then the formed thick sheet is stretched by the longitudinal stretching heating roller, wherein the speed difference ratio of front roller to rear roller in the longitudinal heating roller is as follows: 0.2, wherein the heating temperature of the longitudinal heating roller is about 80 ℃;
step six: pressing the formed thick sheet through a transverse stretching heating roller, pressing the formed thick sheet in the heating process, and stretching the formed thick sheet through the transverse stretching heating roller, wherein the speed difference ratio of front roller to rear roller in the transverse heating roller is as follows: 0.3, wherein the heating temperature of the transverse heating roller is kept consistent with the heating temperature of the longitudinal heating roller;
step seven: after the stretching is finished, cutting and trimming the formed sheet, and then smoothing and stamping the formed sheet by a stamping machine to obtain the double-paper antibacterial film.
Antibacterial test: reference is made to ISO 22196:2011 methods for measuring antimicrobial activity of plastics and other non-porous surfaces
S101, sample preparation: cutting three groups of square samples I with 15cm x 15cm of the antibacterial film of the paper, and cleaning the upper surface and the lower surface of the square samples I;
s102, selecting a designated strain: according to the requirements of ISO 22196 standard, staphylococcus aureus and escherichia coli are selected;
s103, preparing bacterial liquid: selecting an adaptive culture dish, and culturing staphylococcus aureus and escherichia coli to a growth stage;
s104, processing a sample: exposing the first sample to the bacterial liquid under aseptic conditions in a soaking mode to ensure that the bacterial liquid is fully contacted with the sample;
s105, incubation: culturing the first group of treated samples under the proper temperature and humidity for 12 hours, culturing the second group of treated samples under the proper temperature and humidity for 24 hours, and culturing the third group of treated samples under the proper temperature and humidity for 21 days;
s106, eluting: after incubation, residual bacterial liquid is washed away with a proper buffer solution, ensuring that adsorbed, adsorbed or sterilized bacteria remain;
s106, counting the eluted colonies by a culture medium plate counting method, and measuring the following table 16:
high gloss test: reference ASTM D523-17 specular gloss Standard test method
S201, cutting a stained or scratched compound paper antibacterial film into a square sample II with the length of 20cm x 20cm, and calibrating a gloss meter;
s202, the glossiness meter emits a beam of light, and the intensity and angle of the reflected light are measured, and the following table 17 is measured:
high load intensity test: reference is made to ISO 527-3:1995 determination of Plastic-tensile Properties-part 3: test conditions for films and sheets
S301, cutting three groups of rectangular samples III with 20cm x 40cm of nondefective and nondefective antibacterial film of the double paper;
s302, accurately clamping a sample III on tensile test equipment to ensure that the sample is in a uniformly stressed state;
s303, starting a tensile test, applying a tensile force at a constant speed according to standard requirements, recording load and displacement data, and carrying out three-tensile data on a first group of samples as shown in the following table 18:
| time (seconds) | Load (Newton) | Displacement (millimeter) | |
| Third group of samples | 0 | 0 | 0 |
| Second group of samples three | 5 | 3 | 0.87 |
| Third group sample three | 10 | 3 | 0.73 |
Analysis of results: the detection result shows that the double-paper antibacterial film provided by the invention has more than 99% of antibacterial property on escherichia coli and staphylococcus aureus; when the glossiness of the prepared compound paper antibacterial film is detected, the high glossiness of the compound paper antibacterial film can be reflected by detecting according to different detection angles; in the process of stretching detection of the compound paper antibacterial film, according to different stretching time, the displacement distance of the stretched compound paper antibacterial film is within 1 millimeter, so that the compound paper antibacterial film has high load strength.
With the continuous improvement of the technological level and the continuous increase of economy, people consciously pursue higher life quality, along with the threat of pathogenic microorganisms to human health safety, the requirements of antibacterial functionality of people on food and book packaging are also growing, the invention can effectively reduce the threat of pathogenic microorganisms to human health safety, and provide safer and more sanitary food packaging and book use experience.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the invention, but any modifications, equivalents, improvements, etc. within the principles of the present invention should be included in the scope of the present invention.
Claims (9)
1. An antibacterial film of a paper-coated type, which is characterized in that: the compound paper antibacterial film comprises an auxiliary layer, a main extrusion layer and an auxiliary layer;
the auxiliary raw material is prepared from the following components in parts by weight:
homo-polypropylene: 90-98 wt%;
antiblocking agent: 2-10wt%;
the main extrusion layer raw material is prepared from the following components in parts by weight:
homo-polypropylene: 90-93 wt%;
antibacterial agent: 6 to 9 weight percent;
antistatic agent: 1 to 3 weight percent;
the auxiliary two-layer raw material is prepared from the following components in parts by weight:
homo-polypropylene: 88-96 wt%;
antiblocking agent: 4-12 wt%;
the anti-blocking agent is a silicon dioxide anti-blocking agent, and the antibacterial agent is at least one of a silver ion antibacterial agent and a titanium dioxide antibacterial agent.
2. A method for preparing the antibacterial film of the compound paper according to claim 1, which is characterized in that: the method comprises the following steps:
step one: mixing the raw materials of all layers of products;
step two: heating, melting and filtering the raw materials of each layer through an extruder;
step three: carrying out injection molding extrusion molding on the melt after melting and filtering through a die head;
step four: carrying out water cooling solidification crystallization on the extrusion molding product, and carrying out water removal treatment on the molding product;
step five: longitudinally stretching and shaping the formed thick sheet through the speed difference of each roller after the formed thick sheet is heated by the roller;
step six: transversely stretching and shaping the longitudinally stretched thick sheet by heating through an oven;
step seven: trimming, surface high-pressure impact treatment and rolling are carried out on the film which is transversely stretched;
step eight: and cutting, packaging and warehousing the rolled product.
3. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: in step one, an auxiliary layer is prepared: sequentially adding the homopolymerized polypropylene and the anti-blocking agent into a first mixing container according to the weight fraction ratio of an auxiliary layer;
preparing a main extrusion layer: sequentially adding the homopolymerized polypropylene, the antibacterial agent and the antistatic agent into a second mixing container according to the weight fraction ratio of the main extrusion layer;
preparing an auxiliary two-layer: sequentially adding the homopolymerized polypropylene and the anti-blocking agent into a third mixing container according to the weight fraction ratio of the auxiliary layer to the auxiliary layer;
the first mixing vessel, the second mixing vessel and the third mixing vessel were mixed separately, and after the completion of the mixing, the mixture was introduced into an extruder.
4. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: in the second step and the third step, sequentially heating and melting the raw materials of the main extrusion layer, the auxiliary first layer and the auxiliary second layer through an extruder, wherein the heating temperature of the auxiliary first layer is 170-240 ℃, and the heating time is 45-60 min; the heating temperature of the main extrusion layer is 110 ℃ to 150 ℃ and the heating time is 25min to 45min; the heating temperature of the auxiliary two layers is 170 ℃ to 240 ℃ and the heating time is 45min to 60min; the main extrusion layer, the auxiliary first layer and the auxiliary second layer are filtered through the filter to remove impurities and particles in the melt, and the filtered auxiliary first layer, the filtered main extrusion layer and the filtered auxiliary second layer are sequentially pushed into the die and the die head for shaping.
5. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: in the fourth step, after the melts of the auxiliary first layer, the main extrusion layer and the auxiliary second layer are sequentially filled in the cavity of the die, the molded product is rapidly solidified and solidified in a water cooling mode.
6. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: in the fifth and sixth steps, the formed thick sheet is first longitudinally stretched and shaped by a longitudinal stretching heating roller, and in the process of stretching and shaping, the heating temperature of the longitudinal stretching is 70 ℃ to 100 ℃, then the formed thick sheet is transversely stretched and shaped by a transverse stretching heating roller, and in the process of stretching and shaping, the heating temperature of the transverse stretching heating roller is 70 ℃ to 100 ℃.
7. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: in the seventh step, the formed sheet after the longitudinal and transverse stretching is cut and trimmed, then the formed sheet is smoothed and punched by a punching machine, and the formed sheet is rolled after the punching is completed.
8. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: in the eighth step, slitting is performed by a slitter during winding so that the length of each roll is uniform, and then packaging treatment is performed.
9. The antibacterial film of the compound paper and the preparation method thereof are characterized in that: the compound paper antibacterial film is applied to book paper composite and food packaging composite materials.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102825884A (en) * | 2012-09-11 | 2012-12-19 | 宿迁市金田塑业有限公司 | Composite book type sterilizing film and production process thereof |
| CN203557779U (en) * | 2013-09-17 | 2014-04-23 | 金田集团盘锦塑业有限公司 | Antibacterial thin film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102825884A (en) * | 2012-09-11 | 2012-12-19 | 宿迁市金田塑业有限公司 | Composite book type sterilizing film and production process thereof |
| CN203557779U (en) * | 2013-09-17 | 2014-04-23 | 金田集团盘锦塑业有限公司 | Antibacterial thin film |
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