CN109897574B - Pressure-sensitive adhesive and preparation method thereof, and adhesive label and preparation method thereof - Google Patents
Pressure-sensitive adhesive and preparation method thereof, and adhesive label and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of labels and preparation thereof, and provides a pressure-sensitive adhesive and a preparation method thereof, a self-adhesive label and a preparation method thereof; the preparation method of the pressure-sensitive adhesive comprises the following steps: under the condition of stirring, the water-based acrylic emulsion, the tackifying resin, the wetting agent, the defoaming agent and the deionized water are contacted and mixed, and the viscosity of the glue is adjusted to 200-400 cps. The self-adhesive label comprises a substrate layer (1), a pressure-sensitive adhesive layer (2) and a protective layer (3); the pressure-sensitive adhesive layer (2) is obtained by coating the pressure-sensitive adhesive or the pressure-sensitive adhesive prepared by the preparation method. The self-adhesive label obtained by the invention has the advantages of balanced three forces, excellent peel strength and permanent adhesion, and excellent aging resistance.
Description
Technical Field
The invention belongs to the technical field of labels and preparation thereof, and particularly relates to pressure-sensitive adhesive and a preparation method thereof, and a self-adhesive label and a preparation method thereof.
Background
It is well known that label adhesives play an important role in product identification, packaging, decoration, and the like. In many fields of application of label glue, the most common label is a permanent common label, such as an appearance package on a daily chemical product, an energy consumption mark on an electric appliance, a label on a shelf of a supermarket, and the like.
Patent document CN105505235A reports an adhesive for labels, which has excellent initial tack and aging resistance, but is not strong in adhesion (peel strength) and holding power (tack), and in particular, the adhesive uses toluene during the preparation process, which causes permanent damage to the environment and human body.
Patent document CN105969273A reports an environment-friendly hot-melt pressure-sensitive adhesive, which is prepared by mixing C5 petroleum resin, plasticizer, styrene-butadiene-styrene block copolymer, and auxiliary agent, and can satisfy the requirement of environmental protection, but its adhesive force (peel strength) is low.
At present, the phenomena of obvious upwarp, falling and the like of a permanent label used in daily life can be often seen, because the performance of an adhesive layer in an outdoor label is obviously reduced after the adhesive layer is aged under the natural environment, or the quality and the performance of the adhesive layer are unqualified. In the prior art, the three-force performance (initial adhesion, peeling strength and permanent adhesion) of the adhesive or pressure-sensitive adhesive for the label is not ideal, and the aging resistance also has a great problem; meanwhile, some label adhesives with excellent comprehensive performance are prepared from solvent adhesives, and substances harmful to the environment and human bodies are used in the preparation process of the label adhesives, so that the environment pollution is brought, and the health of people is influenced.
Disclosure of Invention
The invention aims to provide pressure-sensitive adhesive and a preparation method thereof, and also provides a self-adhesive label prepared by using the pressure-sensitive adhesive and a preparation method thereof, aiming at the problems in the prior art; the self-adhesive label prepared by using the pressure-sensitive adhesive has balanced three forces and excellent peeling strength and lasting viscosity.
In order to achieve the purpose, the invention provides pressure-sensitive glue which is prepared by reacting the following raw materials in parts by weight:
according to the pressure-sensitive adhesive provided by the invention, preferably, the aqueous acrylic emulsion is a pure acrylic aqueous pressure-sensitive adhesive emulsion;
preferably, the pure acrylic aqueous pressure-sensitive adhesive emulsion is prepared by taking one or more of Methyl Methacrylate (MMA), n-Butyl Acrylate (BA) and isooctyl acrylate (EHA) as a main monomer and taking one or more of hydroxyethyl acrylate (HEA), Acrylic Acid (AA), beta-acryloxypropionic acid (beta-CEA), hydroxyethyl methacrylate (HEMA) and methacrylic acid (MAA) as a functional monomer through emulsion polymerization. The mass ratio of the main monomer to the functional monomer is 90: 10-99: 1.
the preparation of the above pure acrylic aqueous pressure sensitive adhesive emulsion is carried out with reference to the patent document having application number 201610975302. X.
According to the pressure-sensitive glue provided by the invention, preferably, the tackifying resin is selected from water-based emulsified tackifying resins.
Preferably, the water-based emulsified tackifying resin is prepared by modifying and emulsifying natural rosin by using polyalcohol; the polyol is selected from glycerol and/or pentaerythritol.
More preferably, the aqueous emulsifying tackifying resin is selected from the group consisting of Guinox 5861, Guinox 6380 and AQUATACTMOne or more of E6180.
According to the pressure-sensitive glue provided by the invention, preferably, the wetting agent is selected from polysiloxane wetting agents, more preferably polyether modified polysiloxane wetting agents; further preferably selected from one or both of Tego KL 245 and BYK-349.
According to the pressure-sensitive adhesive provided by the invention, the defoaming agent is preferably a silicone defoaming agent, and more preferably one or more of BYK-022, BYK-024 and BYK-028.
Another object of the present invention is to provide a method for preparing the pressure-sensitive adhesive, which comprises the following steps:
under the condition of stirring, the water-based acrylic emulsion, the tackifying resin, the wetting agent, the defoaming agent and water are contacted and mixed, and the viscosity of the glue is adjusted to be 200-400 cps.
Preferably, the method comprises the steps of:
mixing the water-based acrylic emulsion with the tackifying resin under the condition that the rotation speed of a stirring shaft is 400-800 rpm, and stirring for 10-20 minutes; keeping the rotating speed unchanged, adding a defoaming agent, and stirring for 10-15 minutes; keeping the rotating speed unchanged, adding a wetting agent, and stirring for 10-15 minutes; then adding water and stirring for 15-25 minutes under the condition that the rotation speed of the stirring shaft is 300-500 rpm. Under the preparation condition, the components in the formula can be well dispersed, so that the functions of the components and the effect brought by good compatibility of the components are better exerted.
The invention also provides a self-adhesive label, which comprises: the pressure-sensitive adhesive comprises a substrate layer 1 and a pressure-sensitive adhesive layer 2 bonded on the substrate layer 1; the pressure-sensitive adhesive layer 2 is prepared by coating the pressure-sensitive adhesive or the pressure-sensitive adhesive prepared by the preparation method on the substrate layer 1.
Preferably, the thickness of the pressure-sensitive adhesive layer 2 is 15 to 30 μm, preferably 18 to 25 μm.
Preferably, the substrate layer 1 is selected from corona treated PET optical film or corona treated BOPP optical film.
Preferably, the self-adhesive label also comprises a protective layer 3, wherein the protective layer 3 is adhered to the pressure-sensitive adhesive layer 2; more preferably, the protective layer 3 is selected from glassine release paper or kraft release paper.
The invention also provides a preparation method of the self-adhesive label, which comprises the following steps:
a. and coating the pressure-sensitive adhesive on the substrate layer 1, and then drying the substrate layer 1 to obtain the substrate layer 1 coated with the pressure-sensitive adhesive layer 2.
Preferably, the method further comprises a step b of attaching the protective layer 3 to the pressure-sensitive adhesive layer 2 after the sample of the step a is cooled to the greenhouse.
Preferably, in the step a, the substrate layer 1 is laid on a glass plate, and the pressure sensitive adhesive is coated on the substrate layer 1 through a 50-80 μm wire rod, more preferably a 60 μm wire rod.
Preferably, the drying temperature is 70-90 ℃; the drying time is 3-5 minutes.
The technical scheme of the invention has the following excellent effects:
(1) the pure acrylic acid aqueous pressure-sensitive adhesive emulsion used in the invention has good compatibility with other components, and can act synergistically, so that the obtained self-adhesive label has the characteristics of balanced three forces and excellent peeling strength and lasting viscosity, has excellent aging resistance, and can meet the daily permanent use requirement;
(2) the preparation method of the self-adhesive label has the advantages of simple process and good operation stability, and can be suitable for large-scale production.
Drawings
Fig. 1 is a schematic structural diagram of the self-adhesive label of the invention.
The numbers in the above figures are illustrated as follows:
1-a substrate layer, 2-a pressure-sensitive adhesive layer and 3-a protective layer.
Detailed Description
In order that the technical features and contents of the present invention can be understood in detail, preferred embodiments of the present invention will be described in more detail below. While the preferred embodiments of the present invention have been described in the examples, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
Firstly, raw material sources are as follows:
1. substrate layer
A PET optical film with a thickness of 40 μm, currently packaged materials Ltd in Qingdao;
BOPP optical film, 25 μm thick, currently packaged materials ltd in Qingdao;
2. protective layer
Glassine release paper, white, 80g/m272 μm in thickness, Tuoqin Industrial appliances Co., Ltd;
kraft release paper, 85g/m2Dongguan, for example, Asahi composites, Inc.;
3. aqueous acrylic emulsion
The preparation process of the water-based acrylic emulsion comprises the following steps: (the parts of the components are added in parts by mass)
Firstly, mixing a main monomer and a functional monomer to form a mixed monomer (the added monomer amount is 100 parts), then adding the mixed monomer, 4 parts of water, 0.5 part of EF800 (anionic emulsifier, cyanite) and 0.2 part of RS-710 (anionic emulsifier, Rodiya) into a pre-emulsification kettle, and stirring and dispersing for 30min to prepare a pre-emulsion;
adding 80 parts of water and 0.3 part of sodium bicarbonate (buffering agent) into a reaction kettle, stirring and dispersing, adding 4% of pre-emulsion by mass into the reaction kettle, raising the temperature to 85 ℃, adding 0.5 part of ammonium persulfate (initiator) dissolved in 10 parts of water, and keeping the temperature for 15min to prepare seed emulsion;
uniformly dripping the rest pre-emulsion into the seed emulsion within 4 hours, simultaneously dripping 0.25 part of ammonium persulfate (initiator) dissolved in 10 parts of water within 4 hours, and preserving heat for 30min after finishing dripping; then 0.2 part of tert-butyl hydroperoxide and 1 part of 10 wt% aqueous solution of isoascorbic acid are added into the reaction kettle, and the temperature is kept for 1 hour; and when the temperature is reduced to be below 40 ℃, filtering and discharging to obtain the water-based acrylic emulsion.
(1) The pure acrylic aqueous pressure-sensitive adhesive emulsion I is prepared by self-preparing emulsion polymerization by taking 8 parts of Methyl Methacrylate (MMA), 43 parts of Butyl Acrylate (BA) and 45 parts of isooctyl acrylate (EHA) as main monomers and 1.5 parts of acrylic acid AA, 1 part of hydroxyethyl acrylate (HEA) and 1.5 parts of beta-acryloxypropionic acid beta-CEA as functional monomers;
(2) the pure acrylic aqueous pressure-sensitive adhesive emulsion II is prepared by self-preparing 5 parts of Methyl Methacrylate (MMA) and 90 parts of Butyl Acrylate (BA) as main monomers, and carrying out emulsion polymerization on 1.2 parts of methacrylic acid (MAA), 1.6 parts of hydroxyethyl methacrylate (HEMA) and 2.2 parts of beta-acryloxypropionic acid (beta-CEA) as functional monomers;
(3) the pure acrylic acid aqueous pressure-sensitive adhesive emulsion III is prepared by self-preparing emulsion polymerization by taking 6 parts of methyl methacrylate MMA, 40 parts of butyl acrylate BA and 50 parts of isooctyl acrylate EHA as main monomers and 1.5 parts of methacrylic acid MAA, 1 part of hydroxyethyl acrylate HEA and 1.5 parts of beta-acryloxypropionic acid beta-CEA as functional monomers;
4. tackifying resins
Guinox 5861, phoenix fimbrin products industries ltd;
guinox 6380, phoenix jejunum products industries ltd;
AQUATACTM E6180, Keteng high Performance polymers USA;
NS-110, Sterculia Michthysana chemical industry Co., Ltd;
5. wetting agent
Tego KL 245, winning industry group of germany;
BYK-349, Bick, Germany;
6. defoaming agent
BYK-022, Germany bike chemistry;
BYK-024, Byk chemistry, Germany;
BYK-028, Bick, Germany.
Secondly, a test method comprises the following steps:
1. the three force and aging (initial adhesion, peel strength, holding power) test criteria are as follows:
the initial adhesion is tested according to the national standard GB/T4852-2002 'method for testing initial adhesion of pressure-sensitive adhesive tapes';
the initial 180-degree peel strength and the final 180-degree peel strength are tested according to the national standard GB/T2792-1998 180-degree peel strength test method for pressure-sensitive adhesive tapes;
the permanent adhesion is tested according to the national standard GB/T4851-1998 method for testing the permanent adhesion of pressure-sensitive adhesive tapes;
the aging test standard is GB/T17875-1999 accelerated aging test method for pressure-sensitive adhesive tapes.
2. Method for testing thickness of adhesive layer
The thickness of the adhesive layer is measured according to the national standard GB/T7125-1999 test method for the thickness of pressure-sensitive adhesive tapes and adhesive tapes.
3. Measuring the viscosity of the pressure-sensitive adhesive:
the viscosity measurement was carried out according to the national Standard GB/T2794-.
Example 1:
the utility model provides a self-adhesive label, as shown in figure 1, includes substrate layer 1, pressure sensitive adhesive layer 2, protective layer 3, substrate layer 1 is the PET light membrane, pressure sensitive adhesive layer 2 is formed by the pressure sensitive adhesive preparation of following preparation, and thickness is 19.0 mu m, the protective layer be glassine release paper.
The pressure-sensitive adhesive for preparing the self-adhesive label comprises the following components in parts by weight:
the preparation method of the pressure-sensitive adhesive comprises the following steps: adding the pure acrylic pressure-sensitive adhesive emulsion into a stirring kettle, wherein the rotating speed of the stirring shaft is 500 revolutions per minute, and stirring for 5 minutes; then keeping the rotating speed unchanged, adding tackifying resin Guinox 5861, and stirring for 10 minutes; continuously keeping the rotating speed unchanged, adding a defoaming agent BYK-028, and stirring for 10 minutes; keeping the rotating speed unchanged, adding a wetting agent Tego KL 349, and stirring for 10 minutes; and then adjusting the rotating speed of a stirring shaft to 300, adding deionized water, stirring for 15 minutes, and adjusting the viscosity of the glue to 219 cps.
The preparation method of the self-adhesive label comprises the following steps: and flatly paving the PET substrate with the corona-treated right side upwards on a glass plate, coating the prepared pressure-sensitive adhesive on the PET substrate by using a 60-micrometer wire rod, then placing the coated PET substrate into a 70-DEG C oven, taking out after 5 minutes, naturally cooling, and then compounding the pressure-sensitive adhesive on the pressure-sensitive adhesive layer 2 by using glassine paper.
The prepared self-adhesive label is subjected to initial adhesion, 180-degree peel strength and permanent adhesion tests, the obtained results are shown in table 1, and the aging test results are shown in table 2.
Table 1 three strength test results of adhesive labels
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 14 | 16.23 | 17.85 | >100 |
TABLE 2 three-strength test results of the aged sticker label
The pressure-sensitive adhesive in the embodiment 1 is adopted to coat the PET substrate smoothly, the wetting leveling is good, the obtained self-adhesive label has balanced performance and outstanding peeling strength, and the performance label is still excellent after aging.
Example 2:
the utility model provides a self-adhesive label, as shown in figure 1, includes substrate layer 1, pressure sensitive adhesive layer 2, protective layer 3, the substrate layer is BOPP light film, pressure sensitive adhesive layer 2 is formed by the pressure sensitive adhesive preparation of following preparation, and thickness is 22.2 mu m, the protective layer be glassine base paper.
The pressure-sensitive adhesive for preparing the self-adhesive label comprises the following components in parts by weight:
the preparation method of the pressure-sensitive adhesive comprises the following steps: adding the pure acrylic pressure-sensitive adhesive emulsion into a stirring kettle, wherein the rotating speed of the stirring shaft is 500 revolutions per minute, and stirring for 5 minutes; then adjusting the rotating speed to 800 revolutions per minute, adding tackifying resin Guinox 6380, and stirring for 15 minutes; continuously keeping the rotating speed unchanged, adding a defoaming agent BYK-024, and stirring for 15 minutes; keeping the rotating speed unchanged, adding a wetting agent Tego KL 245, and stirring for 15 minutes; and then adjusting the rotating speed of the stirring shaft to 300, adding deionized water, stirring for 25 minutes, and adjusting the viscosity of the glue to 386 cps.
The preparation method of the self-adhesive label comprises the following steps: and flatly paving the BOPP substrate with the front side facing upwards after corona treatment on a glass plate, coating the prepared glue on the BOPP substrate by using a 60-micrometer wire rod, then placing the coated BOPP substrate into an oven at 80 ℃, taking out after 4 minutes, naturally cooling, and compounding the substrate on the pressure-sensitive adhesive layer 2 by using a release surface of glassine base paper.
The prepared self-adhesive label is subjected to initial adhesion, 180-degree peel strength and permanent adhesion tests, the obtained results are shown in table 3, and the aging test results are shown in table 4.
TABLE 3 three strength test results for self-adhesive labels
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 15 | 14.62 | 16.91 | >100 |
TABLE 4 three-strength test results of the aged sticker label
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 14 | 12.58 | 15.37 | >100 |
The pressure-sensitive adhesive in the embodiment 2 is adopted to coat a BOPP substrate, so that the wetting leveling is good, no shrinkage cavity or shrinkage condition of the adhesive exists, the obtained self-adhesive label has balanced performance, and the performance label is still excellent after aging.
Example 3:
the adhesive sticker label comprises a substrate layer 1, a pressure-sensitive adhesive layer 2 and a protective layer 3, wherein the substrate layer is a BOPP film, the pressure-sensitive adhesive layer is prepared from pressure-sensitive adhesive prepared as follows, the thickness of the pressure-sensitive adhesive layer is 20.1 micrometers, and the protective layer is glassine base paper.
The pressure-sensitive adhesive for preparing the self-adhesive label comprises the following components in parts by weight:
the preparation method of the pressure-sensitive adhesive comprises the following steps: adding the pure acrylic pressure-sensitive adhesive emulsion into a stirring kettle, wherein the rotating speed of the stirring shaft is 500 revolutions per minute, and stirring for 5 minutes; then, the rotating speed is adjusted to 600 revolutions per minute, and AQUATACTM E6180 of tackifying resin arizona chemical company is added and stirred for 20 minutes; continuously keeping the rotating speed unchanged, adding a defoaming agent BYK-022, and stirring for 15 minutes; keeping the rotating speed unchanged, adding a wetting agent Tego KL 245, and stirring for 15 minutes; and then adjusting the rotating speed of the stirring shaft to be 500, adding deionized water, stirring for 25 minutes, and adjusting the viscosity of the glue to be 390 cps.
The preparation method of the self-adhesive label comprises the following steps: and flatly paving the BOPP substrate with the front side facing upwards after corona treatment on a glass plate, coating the prepared glue on the BOPP substrate by using a 60-micrometer wire rod, then placing the coated BOPP substrate into a 90-DEG C oven, taking out after 3 minutes, naturally cooling, and compounding the substrate on the pressure-sensitive adhesive layer 2 by using a glassine release surface.
The prepared self-adhesive label was subjected to initial adhesion, 180 ° peel strength, and permanent adhesion tests, and the obtained results are shown in table 5, and the aging test results are shown in table 6.
TABLE 5 three strength test results for self-adhesive labels
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 16 | 12.79 | 14.31 | >100 |
Table 6 three strength test results of the aged sticker label
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 15 | 12.18 | 13.83 | >100 |
The pressure-sensitive adhesive in the embodiment 3 is adopted to coat a BOPP substrate, so that the wetting leveling is good, no shrinkage cavity or shrinkage condition of the adhesive exists, the obtained self-adhesive label has balanced performance and excellent initial viscosity, and the performance label is still excellent after aging and is not obviously reduced.
Comparative example 1:
the preparation process of the pressure-sensitive adhesive and the self-adhesive label is as in example 1, except that no tackifying resin is added in the preparation process, the pure acrylic aqueous pressure-sensitive adhesive emulsion I, the pure acrylic aqueous pressure-sensitive adhesive emulsion II, the pure acrylic aqueous pressure-sensitive adhesive emulsion III and the commercially available pressure-sensitive adhesive emulsion (JN AA-3150, Guangzhou Jun energy chemical Co., Ltd.) are respectively used as the aqueous acrylic emulsion, and the thicknesses of the corresponding pressure-sensitive adhesive layers 2 are 22.8 μm, 23.3 μm and 21.7 μm respectively.
The prepared self-adhesive labels I, II, III and 3150 were subjected to initial adhesion, 180 ° peel strength and permanent adhesion tests, the results are shown in Table 7, and the results of aging tests are shown in Table 8.
TABLE 7 three strength test results for self-adhesive labels
| Sample name | Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| I | 11 | 11.39 | 12.11 | >100 |
| Ⅱ | 12 | 11.66 | 11.93 | >100 |
| Ⅲ | 12 | 9.82 | 10.08 | >100 |
| 3150 | 11 | 7.38 | 7.55 | >100 |
Table 8 three strength test results of the adhesive label after aging
| Sample name | Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| I | 11 | 9.19 | 11.83 | >100 |
| Ⅱ | 11 | 9.02 | 9.90 | >100 |
| Ⅲ | 12 | 7.42 | 9.01 | >100 |
| 3150 | 9 | 4.77 | 5.35 | >100 |
From the test results, compared with JN AA-3150, the self-made pure acrylic aqueous pressure-sensitive adhesive emulsions I, II and III have the advantages of initial adhesion and peeling strength, particularly the peeling strength, the aging performance of the self-made emulsion is better than that of 3150 after aging, and meanwhile, the loss of the peeling strength of 3150 after aging is larger than that of the self-made emulsion. Compared with the adhesive label without the tackifying resin, the adhesive label with the tackifying resin (examples 1 to 3) added in the system is better and more excellent.
Comparative example 2:
the preparation process of the pressure-sensitive adhesive and the self-adhesive label is as in example 2, except that JN AA-3150, Guangzhou Junneng chemical industry Co., Ltd, is adopted to replace pure acrylic acid aqueous pressure-sensitive adhesive emulsion to prepare the pressure-sensitive adhesive, the thickness of the obtained pressure-sensitive adhesive layer is 20.3 μm, the viscosity of the pressure-sensitive adhesive is 331cps, and the performance test data is shown in tables 9 and 10.
TABLE 9 three-strength test results for self-adhesive labels
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 14 | 8.93 | 9.05 | 83 |
Table 10 three-force test results for pressure-sensitive adhesive labels after aging
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 13 | 6.17 | 6.01 | >100 |
The pressure-sensitive adhesive in the comparative example 2 is adopted to coat a BOPP substrate smoothly, the wetting leveling is good, but because the main pressure-sensitive adhesive emulsions are different, compared with the example 2, the peel strength and the permanent adhesion of the pressure-sensitive adhesive in the comparative example 2 are obviously reduced, the performance after aging is greatly reduced, and compared with the data in the comparative example 2, the performance improvement of the pressure-sensitive adhesive label of the example 2 using the self-prepared pure acrylic acid water-based pressure-sensitive adhesive emulsion II is obviously higher than that of the pressure-sensitive adhesive label using JN AA-3150 in a whole body.
Comparative example 3
The preparation process of the pressure-sensitive adhesive and the self-adhesive label is as in example 2, except that the amount of the added water-based emulsified tackifying resin Guinox 6380 is 40g, the thickness of the obtained pressure-sensitive adhesive layer is 21.1 μm, and the viscosity of the pressure-sensitive adhesive is 310 cps. The performance test data are shown in tables 11 and 12.
TABLE 11 three-strength test results for self-adhesive labels
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 17 | 10.15 | 11.34 | 58 |
Table 12 three-strength test results of self-adhesive label after aging
| Initial viscosity # | Initial peel strength (N/25mm)) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 16 | 9.85 | 11.01 | 96 |
The pressure-sensitive adhesive in the comparative example 3 is smoothly coated on the BOPP substrate, and the wetting leveling is good, but the initial adhesion is improved to some extent, the peel strength and the lasting adhesion are both obviously reduced, and the good three-force balance cannot be achieved because the used tackifying resin is too large in amount compared with the example 2.
Comparative example 4
The preparation process of the pressure-sensitive adhesive and the self-adhesive label is as in example 2, except that the amount of the added water-based emulsified tackifying resin Guinox 6380 is 12g, the thickness of the obtained pressure-sensitive adhesive layer is 21.4 μm, and the viscosity of the pressure-sensitive adhesive is 281 cps. The performance test data are shown in tables 13 and 14.
TABLE 13 three strength test results for self-adhesive label
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 11 | 10.69 | 12.82 | >100 |
Table 14 three-strength test results of self-adhesive label after aging
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 11 | 8.55 | 10.17 | >100 |
The pressure-sensitive adhesive in the comparative example 4 is smoothly coated on the BOPP substrate, and the wetting leveling is good, but because the amount of the tackifying resin used is too small, compared with the pressure-sensitive adhesive in the example 2, the initial adhesion, the initial peeling strength and the final peeling strength are deviated, and the overall performance after aging is lower.
As can be seen from comparison between example 2 and comparative examples 2, 3 and 4, the amount of the tackifying resin has a great influence on three forces of the self-adhesive label, and the appropriate amount of the tackifying resin is very critical to obtain a self-adhesive label with balanced three forces.
Comparative example 5
The preparation process of the pressure-sensitive adhesive and the self-adhesive label is as in example 3, except that the aqueous emulsification tackifying resin is NS-110, the thickness of the obtained pressure-sensitive adhesive layer is 19.7 μm, and the viscosity of the pressure-sensitive adhesive is 209 cps. The performance test data are shown in tables 15 and 16.
Table 15 three strength test results of adhesive label
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 13 | 10.53 | 11.27 | 67 |
Table 16 three-strength test results of the adhesive label after aging
| Initial viscosity # | Initial peel strength (N/25mm) | Ultimate peel strength (N/25mm) | Permanent adhesive force (h) |
| 11 | 7.53 | 8.27 | 96 |
The pressure-sensitive adhesive in comparative example 5 was applied smoothly on a BOPP substrate, and the wetting and leveling were good, but the performance test results were much smaller than those in example 3, and the initial tack and peel strength after aging were also reduced faster, because of the different types of tackifying resins used.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (18)
1. The pressure-sensitive adhesive is characterized by being prepared by reacting the following raw materials in parts by weight:
the water-based acrylic emulsion is pure acrylic water-based pressure-sensitive adhesive emulsion; the pure acrylic acid water-based pressure-sensitive adhesive emulsion is generated by emulsion polymerization reaction by taking one or more of methyl methacrylate, n-butyl acrylate and isooctyl acrylate as main monomers and taking one or more of hydroxyethyl acrylate, acrylic acid, beta-acryloxypropionic acid, hydroxyethyl methacrylate and methacrylic acid as functional monomers;
the tackifying resin is selected from water-based emulsified tackifying resin, the water-based emulsified tackifying resin is prepared by modifying and emulsifying natural rosin by using polyhydric alcohol, and the polyhydric alcohol is selected from glycerol and/or pentaerythritol.
2. The pressure-sensitive adhesive according to claim 1, wherein the pressure-sensitive adhesive is prepared by reacting raw materials comprising the following components in parts by weight:
3. the pressure-sensitive adhesive according to claim 1, wherein said aqueous emulsion tackifying resin is selected from the group consisting of Guinox 5861, Guinox 6380 and AQUATACTMOne or more of E6180.
4. The pressure-sensitive glue according to any one of claims 1-3, characterised in that the wetting agent is selected from silicone based wetting agents.
5. The pressure-sensitive adhesive according to claim 4, wherein the wetting agent is selected from polyether-modified polysiloxane wetting agents.
6. The pressure-sensitive glue according to claim 5, wherein the wetting agent is selected from one or both of Tego KL 245 and BYK-349.
7. The pressure-sensitive adhesive according to any one of claims 1 to 3 and 5 to 6, wherein the defoaming agent is a silicone-based defoaming agent.
8. The pressure sensitive glue of claim 7, wherein the defoaming agent is selected from one or more of BYK-022, BYK-024 and BYK-028.
9. A process for the preparation of a pressure-sensitive adhesive according to any one of claims 1 to 8, which comprises:
under the condition of stirring, the water-based acrylic emulsion, the tackifying resin, the wetting agent, the defoaming agent and water are contacted and mixed, and the viscosity of the glue is adjusted to be 200-400 cps.
10. The method of claim 9, comprising the steps of:
mixing the water-based acrylic emulsion with the tackifying resin under the condition that the rotation speed of a stirring shaft is 400-800 rpm, and stirring for 10-20 minutes; keeping the rotating speed unchanged, adding a defoaming agent, and stirring for 10-15 minutes; keeping the rotating speed unchanged, adding a wetting agent, and stirring for 10-15 minutes; then adding water and stirring for 15-25 minutes under the condition that the rotation speed of the stirring shaft is 300-500 rpm.
11. A self-adhesive label, comprising: the pressure-sensitive adhesive comprises a base material layer (1) and a pressure-sensitive adhesive layer (2) bonded to the base material layer (1); characterized in that the pressure-sensitive adhesive layer (2) is the pressure-sensitive adhesive according to any one of claims 1 to 8 or the pressure-sensitive adhesive prepared by the preparation method according to any one of claims 9 to 10, and is prepared by coating the pressure-sensitive adhesive on the substrate layer (1).
12. The self-adhesive label according to claim 11, characterized in that the substrate layer (1) is selected from corona treated PET optical film or corona treated BOPP optical film.
13. The self-adhesive label according to claim 11 or 12, characterized in that it further comprises a protective layer (3), said protective layer (3) being adhered to said pressure-sensitive adhesive layer (2).
14. The self-adhesive label according to claim 13, characterized in that the protective layer (3) is selected from glassine release paper or kraft release paper.
15. A method for preparing the self-adhesive label as set forth in any one of claims 11 to 14, wherein the method comprises the steps of:
a. and coating the pressure-sensitive adhesive on the substrate layer (1), and then drying the substrate layer to obtain the substrate layer (1) coated with the pressure-sensitive adhesive layer (2).
16. The method of claim 15, further comprising step b: and (c) after the sample in the step (a) is cooled to room temperature, attaching the protective layer (3) to the pressure-sensitive adhesive layer (2).
17. The method for preparing according to claim 15, wherein in the step a, the substrate layer (1) is laid on a glass plate, and the pressure sensitive adhesive is coated on the substrate layer (1) by a 50-80 μm wire rod.
18. The preparation method according to claim 15, wherein in the step a, the temperature for drying is 70-90 ℃; the drying time is 3-5 minutes.
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| CN110951424B (en) * | 2019-12-06 | 2021-08-20 | 四川羽玺新材料股份有限公司 | Adhesive for mobile phone frame shading adhesive tape and preparation method and application thereof |
| CN111154415B (en) * | 2020-01-08 | 2021-09-17 | 江苏耐斯数码科技股份有限公司 | Thermal sublimation printing adhesive label |
| CN113621322A (en) * | 2021-07-19 | 2021-11-09 | 宁波卓越印务有限公司 | Multifunctional adhesive label and preparation method thereof |
| CN113897141A (en) * | 2021-09-16 | 2022-01-07 | 太仓隽旺电子科技有限公司 | Anti-counterfeiting adhesive label and preparation method thereof |
| CN115156001B (en) * | 2022-08-08 | 2023-04-18 | 湖南恒创新材料有限公司 | Preparation process and processing equipment of small water-soluble pressure-sensitive adhesive |
| CN116515408B (en) * | 2023-04-13 | 2023-10-24 | 江苏金大包装材料科技有限公司 | Preparation process of oil-resistant high-viscosity self-adhesive label |
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| WO2012133268A1 (en) * | 2011-03-30 | 2012-10-04 | リンテック株式会社 | Emulsion adhesive composition and re-peelable adhesive sheet |
| BR112015013398A2 (en) * | 2012-12-10 | 2017-07-11 | Avery Dennison Corp | rf activatable adhesives and their applications |
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