CN114350279A - Three-component composite pressure-sensitive adhesive, preparation method and adhesive tape - Google Patents
Three-component composite pressure-sensitive adhesive, preparation method and adhesive tape Download PDFInfo
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Abstract
The invention discloses a three-component composite pressure-sensitive adhesive, a preparation method and an adhesive tape, wherein the adhesive comprises the following raw materials in percentage by mass: 25-45% of the component A, 45-65% of the component B and 10% of the component C; wherein the component A comprises pangolin rubber, smoked sheet rubber, low-temperature polymerized styrene-butadiene rubber 1012, hydrogenated C5 petroleum resin LH100, C5 petroleum resin Y100, terpene resin T100, antioxidant 264, antioxidant DLTDP and toluene; the component B comprises smoked sheet rubber, low-temperature polymerized styrene-butadiene rubber 1012, butyl rubber 1751, polymerized terpene resin 7042, terpene phenolic resin 138, anti-aging agent 264, anti-aging agent RD, magnesium oxide and toluene; the component C comprises methyl methacrylate, butyl acrylate, benzoyl peroxide, styrene-butadiene rubber 303, an accelerator DM and toluene. According to the invention, the formulas of various basic components are determined, and then the matching is carried out according to the formulas, and the multiple basic formulas act synergistically, so that the performance of the obtained composite pressure-sensitive adhesive is obviously improved.
Description
Technical Field
The invention relates to the field of adhesive tapes, in particular to a three-component composite pressure-sensitive adhesive, a preparation method and an adhesive tape.
Background
With the development of social economy, the requirements of consumers on the product quality are higher and higher, and the requirements of market personalization are higher and higher, so that in order to meet the requirements, a production enterprise needs to invest a great deal of effort to improve or redevelop products in a targeted manner.
The conventional common PVC pressure-sensitive adhesive tape in the civil market is developed aiming at a soft PVC film taking DOP as a main plasticizer, and the performance of the adhesive tape has limitation in a high-temperature area or a low-temperature area. At low temperature, the adhesive tape has poor cold resistance, poor viscosity and hard base material; at high temperature, the adhesive tape is easy to generate the phenomena of adhesive overflow, adhesive transfer and adherend pollution; these all affect the user experience.
In order to solve these problems, some special plasticizers are needed for PVC films to adapt to different climatic conditions, but the adhesives are not matched with the PVC films, and the adjustment of the formulation is easy to be lost, so that it is difficult to achieve the optimal balance state, and therefore, there is a need to develop adhesives well matched with different plasticizers.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a three-component composite pressure-sensitive adhesive, a preparation method and an adhesive tape so as to solve the problems in the technical background.
In order to achieve the purpose, the invention is realized by the following technical scheme:
on one hand, the invention provides a three-component composite pressure-sensitive adhesive which comprises the following raw materials in percentage by mass: 25-45% of the component A, 45-65% of the component B and 10% of the component C; wherein the component A comprises pangolin rubber, smoked sheet rubber, low-temperature polymerized styrene-butadiene rubber 1012, hydrogenated C5 petroleum resin LH100, C5 petroleum resin Y100, terpene resin T100, antioxidant 264, antioxidant DLTDP and toluene;
the component B comprises smoked sheet rubber, low-temperature polymerized styrene-butadiene rubber 1012, butyl rubber 1751, polymerized terpene resin 7042, terpene phenolic resin 138, anti-aging agent 264, anti-aging agent RD, magnesium oxide and toluene;
the component C comprises methyl methacrylate, butyl acrylate, benzoyl peroxide, styrene-butadiene rubber 303, an accelerator DM and toluene.
In the technical scheme, the component A comprises 20-30 parts of natural nail rubber, 65 parts of tobacco flake rubber, 101255-65 parts of low-temperature polymerized styrene-butadiene rubber, LH 10070-80 parts of hydrogenated C5 petroleum resin, Y10060-70 parts of C5 petroleum resin, T10010 parts of terpene resin, 2641 parts of anti-aging agent, 1 part of antioxidant DLTDP and 700 parts of toluene.
In the technical scheme, the component B comprises 85-95 parts of tobacco flake glue, 101240-50 parts of low-temperature polymerized styrene-butadiene rubber, 175115 parts of butyl rubber, 7042115-125 parts of polymerized terpene resin, 13825-35 parts of terpene phenolic resin, 2641 parts of anti-aging agent, RD 1 part of anti-aging agent, 5 parts of magnesium oxide and 700 parts of toluene.
In the technical scheme, the component C comprises 120-140 parts of methyl methacrylate, 30-50 parts of butyl acrylate, 7 parts of benzoyl peroxide, 303100 parts of styrene butadiene rubber, 3 parts of an accelerator DM and 1500 parts of toluene.
On the other hand, the invention also provides a preparation method of the three-component compound pressure-sensitive adhesive, which comprises the following steps:
step one, preparing a component A; the method specifically comprises the following steps:
1.1 adjusting the roll spacing of an open mill to 4mm, roughly refining the nomex rubber and the low-temperature polymerized styrene-butadiene rubber 1012 on the open mill for 5-6 times, reducing the roll spacing to 1mm, finely refining for 3 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
1.2 adjusting the roller distance of the open mill to 2mm, finely milling the tobacco flake glue for 2 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
1.3, injecting toluene into a reaction kettle, starting stirring, sequentially adding the refined natural rubber of the step 1.1, the low-temperature polymerized styrene-butadiene rubber 1012 and the refined smoked sheet rubber of the step 1.2, stirring for 4 hours until the glue solution is uniform, and continuously introducing cooling water in the stirring process to prevent the temperature of the glue solution from being higher;
1.4 adding hydrogenated C5 petroleum resin LH100, C5 petroleum resin Y100, terpene resin T100, antioxidant 264 and antioxidant DLTDP, and stirring for 2 hours;
1.5, stopping the machine, filtering and discharging to obtain a component A for later use;
step two, preparing the component B; the method specifically comprises the following steps:
2.1 adjusting the roller spacing of the open mill to 4mm, roughly milling the tobacco flake glue on the open mill for 5-6 times, reducing the roller spacing to 1mm, finely milling for 3 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
2.2 adjusting the roll spacing of the open mill to 2mm, finely milling the low-temperature polymerized styrene-butadiene rubber 1012 and the butyl rubber 1751 for 2 times, and then discharging and airing the sheets with the size of about 60cm multiplied by 40 cm;
2.3, injecting toluene into the reaction kettle, starting stirring, sequentially adding the smoked sheet rubber refined in the step 2.1 and the low-temperature polymerized styrene-butadiene rubber 1012 and the butyl rubber 1751 refined in the step 2.2, stirring for 4 hours until the glue solution is uniform, and continuously introducing cooling water in the stirring process to ensure that the temperature of the glue solution is not more than 45 ℃;
2.4 adding polymerized terpene resin 7042, antioxidant 264, antioxidant RD and magnesium oxide, and stirring for 2 hours;
2.5 checking the temperature of the glue solution, putting the terpene phenolic resin 138 into the glue solution at the temperature below 45 ℃, and stirring for 1 hour;
2.6, stopping the machine, filtering and discharging to obtain a component B for later use;
step three, preparing the component C; the method specifically comprises the following steps:
3.1 adjusting the roll spacing of the open mill to 2mm, finely milling the styrene-butadiene rubber 303 for 2 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
3.2 sequentially injecting 1/5 methyl methacrylate, 1/5 butyl acrylate and 2/7 benzoyl peroxide into the first pre-reaction kettle, and stirring for 30 minutes to obtain a first mixed solution for later use;
3.3 sequentially injecting the rest methyl methacrylate, butyl acrylate and benzoyl peroxide into the second pre-reaction kettle, and stirring for 30 minutes to obtain a second mixed solution for later use;
3.4, injecting toluene into the reaction kettle, starting stirring, adding the butadiene styrene rubber 303 refined in the step 3.1, stirring for 1 hour, and standing for 1 hour;
3.5 adding the accelerator DM into the reaction kettle after standing in the step 3.4, stirring for 5 minutes, and then heating to 80 ℃ and stabilizing for 5 minutes;
3.6 dropwise adding the first mixed solution obtained in the first pre-reaction kettle in the step 3.2 into the reaction kettle in the step 3.4, wherein the dropping is completed within 1 hour, the temperature is kept at 80-82 ℃ in the whole process, and then the temperature is kept at 82-84 ℃ for 1 hour;
3.7 dropwise adding the second mixed solution obtained in the second pre-reaction kettle in the step 3.3 into the reaction kettle after heat preservation in the step 3.6, finishing dropwise adding for 3 hours, keeping the temperature at 82-84 ℃ in the whole process, and then preserving the heat for 1 hour at 84-86 ℃;
3.8 cooling to below 40 ℃, filtering and discharging to obtain a component C for later use;
and step four, adding the component A, the component B and the component C into a mixing kettle according to the proportion of 25-45% of the component A, 45-65% of the component B and 10% of the component C, stirring for 2 hours, and discharging to obtain the three-component composite pressure-sensitive adhesive.
On the other hand, the invention also provides an adhesive tape, which is obtained by coating the three-component compound pressure-sensitive adhesive on a PVC film taking DOS, high molecular polyester or DOP as a main plasticizer.
In the technical scheme, when the adhesive is coated on a PVC film taking DOS as a main plasticizer, the three-component compound pressure-sensitive adhesive comprises 45% of a component A, 45% of a component B and 10% of a component C.
In the technical scheme, when the three-component composite pressure-sensitive adhesive is coated on a PVC film taking high polymer polyester as a main plasticizer, the A component is 25%, the B component is 65% and the C component is 10%.
In the technical scheme, when the adhesive is coated on a PVC film taking DOP as a main plasticizer, the three-component compound pressure-sensitive adhesive comprises 35% of a component A, 55% of a component B and 10% of a component C.
In the invention, the applicant obtains three empirical formulas of the component A, the component B and the component C in the work research and accumulation for many years, the three components are different in performance, the preparation process is greatly different, and the preparation process needs to be strictly controlled according to the process requirements. In addition to the detection index in the standard environment, different components have different characteristics in different environments. The preparation process of the component A is a physical mixing process, the performance cannot be improved through post-treatment after the component A is prepared, the Tg temperature of the component A is moderate, the component A has good bonding performance at normal temperature (0-40 ℃), but tends to be in a glass state at low temperature (below 0 ℃), and the viscosity is lost or poor. The component A pressure-sensitive adhesive is coated with a PVC film taking a high-molecular plasticizer as a main plasticizer and is not sticky; when a PVC film taking a cold-resistant plasticizer as a main plasticizer is coated, the adhesion performance is low due to the migration of the plasticizer; when coated with ordinary PVC film (DOP is used as main plasticizer), the film can obtain more balanced performance at normal temperature.
The preparation process of the component B is a physical mixing process, and the component B can be subjected to subsequent heat treatment after preparation due to the cross-linking component, the adhesive can be cross-linked and cured to a certain extent so as to improve the performance, the Tg temperature of the adhesive is lower, the adhesive has good bonding performance at low temperature (below 0 ℃) when not subjected to heat treatment, the adhesive tends to viscous state at normal temperature (0-40 ℃), the performance is not good, and the performance is obviously improved after heat treatment. When the component B pressure-sensitive adhesive is coated on a PVC film taking a high-molecular plasticizer as a main plasticizer, good performance can be obtained after heat treatment, but the low-temperature performance of the adhesive tape is poor; when a PVC film taking a cold-resistant plasticizer as a main plasticizer is coated, the initial viscosity is too large, so that the pressure sensitivity is lost; the coating of ordinary PVC film (based on DOP as the main plasticizer) is poor in pressure-sensitivity because of its relatively high initial tack.
The component C is prepared by a grafting reaction, has a higher Tg temperature, can shield the PVC film and the surface coating layer, prevents the plasticizer from migrating into the adhesive layer, can solidify the adhesive and improves the performance.
The three components of the adhesive are compounded and act synergistically, and the component A can further increase the peel strength of the component B; the sustained viscosity of the component A can be further enhanced after the component B is crosslinked; the component C can further cure the component A and the component B, can improve the peeling strength and the lasting viscosity, but the quality problem of adhesive loss is caused by hardening the adhesive layer due to excessive addition of the component C.
Compared with the prior art, the invention has the beneficial effects that:
1. in the invention, the higher the molecular weight of the plasticizer used for the PVC film is, the lower the dosage of the component A is, and the higher the dosage of the component B is; the lower the molecular weight of the plasticizer, the higher the amount of the component A and the lower the amount of the component B.
2. After the basic component formula is determined, the test is carried out according to the rule according to the type of the base material plasticizer, so that the test times can be greatly reduced, and a more appropriate formula can be obtained. Meanwhile, the three-component adhesive is compounded and acts synergistically, and the performance of the obtained three-component compound pressure-sensitive adhesive is remarkably improved.
3. Because the preparation process of each component has large difference, the preparation process needs to strictly comply with corresponding process regulations.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict.
The invention provides a three-component composite pressure-sensitive adhesive which comprises the following raw materials in percentage by mass: 25-45% of the component A, 45-65% of the component B and 10% of the component C; the component A comprises 20-30 parts of natural nail rubber, 65 parts of tobacco flake rubber, 101255-65 parts of low-temperature polymerized styrene-butadiene rubber, LH 10070-80 parts of hydrogenated C5 petroleum resin, Y10060-70 parts of C5 petroleum resin, T10010 parts of terpene resin, 2641 parts of an anti-aging agent, 1 part of an antioxidant DLTDP and 700 parts of toluene. The component B comprises 85-95 parts of tobacco flake glue, 101240-50 parts of low-temperature polymerized styrene-butadiene rubber, 175115 parts of butyl rubber, 7042115-125 parts of polymerized terpene resin, 13825-35 parts of terpene phenolic resin, 2641 parts of an anti-aging agent, RD 1 part of the anti-aging agent, 5 parts of magnesium oxide and 700 parts of toluene. The component C comprises 120-140 parts of methyl methacrylate, 30-50 parts of butyl acrylate, 7 parts of benzoyl peroxide, 303100 parts of styrene butadiene rubber, 3 parts of an accelerator DM and 1500 parts of toluene. Further, the smoked sheet glue is No. 1 smoked sheet glue.
Example 1
In a first aspect, the present embodiment provides a three-component composite pressure-sensitive adhesive, which comprises the following raw materials by mass: 25% of component A, 65% of component B and 10% of component C; the component A comprises 30 parts of natural armor rubber, 65 parts of No. 1 smoked sheet rubber, 101255 parts of low-temperature polymerized styrene-butadiene rubber, LH10070 parts of hydrogenated C5 petroleum resin, Y10070 parts of C5 petroleum resin, T10010 parts of terpene resin, 2641 parts of anti-aging agent, 1 part of antioxidant DLTDP and 700 parts of toluene.
The component B comprises 95 parts of No. 1 smoked sheet rubber, 101240 parts of low-temperature polymerized styrene-butadiene rubber, 175115 parts of butyl rubber, 7042115 parts of polymerized terpene resin, 13835 parts of terpene phenolic resin, 2641 parts of anti-aging agent, RD 1 part of anti-aging agent, 5 parts of magnesium oxide and 700 parts of toluene.
The component C comprises 140 parts of methyl methacrylate, 30 parts of butyl acrylate, 7 parts of benzoyl peroxide, 303100 parts of styrene butadiene rubber, 3 parts of an accelerator DM and 1500 parts of toluene.
In a second aspect, this embodiment further provides a method for preparing the three-component composite pressure-sensitive adhesive, including the following steps:
step one, preparing a component A; the method specifically comprises the following steps:
1.1 adjusting the roll spacing of an open mill to 4mm, roughly refining the nomex rubber and the low-temperature polymerized styrene-butadiene rubber 1012 on the open mill for 5-6 times, reducing the roll spacing to 1mm, finely refining for 3 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
1.2 adjusting the roller distance of the open mill to 2mm, finely milling No. 1 smoked sheet rubber for 2 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
1.3, injecting toluene into a reaction kettle, starting stirring, sequentially adding the refined Tianjia rubber of the step 1.1, the low-temperature polymerized styrene-butadiene rubber 1012 and the refined No. 1 smoked sheet rubber of the step 1.2, stirring for 4 hours until the glue solution is uniform, and continuously introducing cooling water in the stirring process to prevent the glue solution from being at a high temperature;
1.4 adding hydrogenated C5 petroleum resin LH100, C5 petroleum resin Y100, terpene resin T100, antioxidant 264 and antioxidant DLTDP, and stirring for 2 hours;
1.5, stopping the machine, filtering and discharging to obtain a component A for later use;
step two, preparing the component B; the method specifically comprises the following steps:
2.1 adjusting the roller spacing of the open mill to 4mm, roughly milling No. 1 smoked sheet glue on the open mill for 5-6 times, reducing the roller spacing to 1mm, finely milling for 3 times, discharging and airing, and the size is about 60cm multiplied by 40 cm;
2.2 adjusting the roll spacing of the open mill to 2mm, finely milling the low-temperature polymerized styrene-butadiene rubber 1012 and the butyl rubber 1751 for 2 times, and then discharging and airing the sheets with the size of about 60cm multiplied by 40 cm;
2.3, injecting toluene into the reaction kettle, starting stirring, sequentially adding the smoked sheet rubber No. 1 refined in the step 2.1, the low-temperature polymerized styrene-butadiene rubber 1012 refined in the step 2.2 and the butyl rubber 1751 refined in the step 2, stirring for 4 hours until the glue solution is uniform, and continuously introducing cooling water in the stirring process to ensure that the temperature of the glue solution is not more than 45 ℃;
2.4 adding polymerized terpene resin 7042, antioxidant 264, antioxidant RD and magnesium oxide, and stirring for 2 hours;
2.5 checking the temperature of the glue solution, putting the terpene phenolic resin 138 into the glue solution at the temperature below 45 ℃, and stirring for 1 hour;
2.6, stopping the machine, filtering and discharging to obtain a component B for later use;
step three, preparing the component C; the method specifically comprises the following steps:
3.1 adjusting the roll spacing of the open mill to 2mm, finely milling the styrene-butadiene rubber 303 for 2 times, discharging and airing, wherein the size is about 60cm multiplied by 40 cm;
3.2 sequentially injecting 1/5 methyl methacrylate, 1/5 butyl acrylate and 2/7 benzoyl peroxide into the first pre-reaction kettle, and stirring for 30 minutes to obtain a first mixed solution for later use;
3.3 sequentially injecting the rest methyl methacrylate, butyl acrylate and benzoyl peroxide into the second pre-reaction kettle, and stirring for 30 minutes to obtain a second mixed solution for later use;
3.4, injecting toluene into the reaction kettle, starting stirring, adding the butadiene styrene rubber 303 refined in the step 3.1, stirring for 1 hour, and standing for 1 hour;
3.5 adding the accelerator DM into the reaction kettle after standing in the step 3.4, stirring for 5 minutes, and then heating to 80 ℃ and stabilizing for 5 minutes;
3.6 dropwise adding the first mixed solution obtained in the first pre-reaction kettle in the step 3.2 into the reaction kettle in the step 3.4, wherein the dropping is completed within 1 hour, the temperature is kept at 80-82 ℃ in the whole process, and then the temperature is kept at 82-84 ℃ for 1 hour;
3.7 dropwise adding the second mixed solution obtained in the second pre-reaction kettle in the step 3.3 into the reaction kettle after heat preservation in the step 3.6, finishing dropwise adding for 3 hours, keeping the temperature at 82-84 ℃ in the whole process, and then preserving the heat for 1 hour at 84-86 ℃;
3.8 cooling to below 40 ℃, filtering and discharging to obtain a component C for later use;
and step four, adding the component A, the component B and the component C into a mixing kettle according to the proportion of 25-45% of the component A, 45-65% of the component B and 10% of the component C, stirring for 2 hours, and discharging to obtain the three-component composite pressure-sensitive adhesive.
Examples 2 to 3
Examples 2 to 3 similar to example 1, the respective components of the component A, the component B and the component C are unchanged, wherein the component A comprises 30 parts of natural rubber, 65 parts of No. 1 tobacco sheet rubber, 101255 parts of low-temperature polymerized styrene-butadiene rubber, LH10070 parts of hydrogenated C5 petroleum resin, Y10070 parts of C5 petroleum resin, T10010 parts of terpene resin, 2641 parts of anti-aging agent, 1 part of antioxidant DLTDP and 700 parts of toluene.
The component B comprises 95 parts of No. 1 smoked sheet rubber, 101240 parts of low-temperature polymerized styrene-butadiene rubber, 175115 parts of butyl rubber, 7042115 parts of polymerized terpene resin, 13835 parts of terpene phenolic resin, 2641 parts of anti-aging agent, RD 1 part of anti-aging agent, 5 parts of magnesium oxide and 700 parts of toluene.
The component C comprises 140 parts of methyl methacrylate, 30 parts of butyl acrylate, 7 parts of benzoyl peroxide, 303100 parts of styrene butadiene rubber, 3 parts of an accelerator DM and 1500 parts of toluene. Except that the contents (or ratios) of the component A and the component B are different, as shown in Table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | |
| Component A | 25 | 35 | 45 |
| Component B | 65 | 55 | 45 |
| Component C | 10 | 10 | 10 |
Examples 4 to 7
Examples 4 to 7 are similar to example 1, and the respective components of component A, component B and component C were unchanged except that the contents of component A, component B and component C were different, wherein examples 4 to 7 were the contents of component C, and component A and component B were set in the ratio of example 1; in examples 4 to 5, the content of the component C was constant, and the ratio of the component A to the component B was varied, as shown in Table 2.
TABLE 2
| Example 1 | Example 4 | Example 5 | Example 6 | Example 7 | |
| Component A | 25 | 22.2 | 26.4 | 55 | 15 |
| Component B | 65 | 57.8 | 68.6 | 35 | 75 |
| Component C | 10 | 20 | 5 | 10 | 10 |
Application example 1
The adhesives obtained in examples 1 to 3 were coated on a 0.15mm PVC film with a plasticizer of high molecular polyester to obtain corresponding adhesive tapes, thickness of the applied adhesive (dry adhesive): 25 μm, constant temperature treatment of adhesive tape: 90 ℃ for 12 h. Then, an electronic peel tester, an initial adhesion tester and a permanent adhesion tester were used for the test, and the test results are shown in table 3.
TABLE 3
As can be seen from Table 3, the adhesive formulation provided in example 1 matches the PVC film properties of the high molecular polyester plasticizer best when applied to PVC films having high molecular polyester as the primary plasticizer, 25% of component A, 65% of component B and 10% of component C in the three-component composite pressure sensitive adhesive.
Application example 2
The adhesives obtained in examples 1 to 3 were applied to a 0.15mm PVC film with the plasticizer DOP to give corresponding adhesive tapes, the thickness of the applied adhesive (dry adhesive): 25 μm, constant temperature treatment of adhesive tape: 80 ℃ for 10 h. Then, an electronic peel tester, an initial tack tester and a permanent tack tester were used for testing, and the test results are shown in table 4.
TABLE 4
As can be seen from Table 4, the adhesive formulation provided in example 2 best matches the PVC film properties of the DOP plasticizer when applied to the PVC film having DOP as the major plasticizer, in which the A component was 35%, the B component was 55%, and the C component was 10%.
Application example 3
The adhesives obtained in examples 1 to 3 were applied to a 0.15mm PVC film with DOS as plasticizer to give corresponding adhesive tapes, thickness of applied (dry glue): 25 μm, constant temperature treatment of adhesive tape: 80 ℃ for 10 h. Then, an electronic peel tester, an initial tack tester and a permanent tack tester were used for testing, and the test results are shown in table 5.
TABLE 5
As can be seen from Table 5, the adhesive formulation provided in example 3 matches the PVC film properties of the DOS plasticizer best when applied to PVC films having DOS as the primary plasticizer, in which the A component is 45%, the B component is 45%, and the C component is 10%.
Application example 4
The adhesion obtained by coating the adhesive on a 0.15mm PVC film taking the plasticizer as the high-molecular polyester brings about the influence of the contents of the component A, the component B and the component C on the performance of the three-component composite pressure-sensitive adhesive.
The adhesives obtained in examples 4 to 7 were coated on a 0.15mm PVC film of a high molecular polyester as plasticizer to give the corresponding adhesive tapes, thickness of the applied adhesive (dry adhesive): 25 μm, constant temperature treatment of adhesive tape: 90 ℃ for 12 h. Then, an electronic peel tester, an initial tack tester, and a permanent tack tester were used to perform the tests, and the test results are shown in table 6.
TABLE 6
As can be seen from Table 6, in example 1, compared with examples 4-5, when the proportion of the component A to the component B is unchanged, and the content of the component C is 20% or 5%, the peel strength and the tack of the adhesive are obviously lower than those of an adhesive with the content of the component C being 10%, the addition of the component C is too much, so that the adhesive layer is easily hardened, and the quality problem of adhesive failure is caused, and the addition of the component C is too little, so that the component A and the component B cannot be further cured; when the content of the C component is unchanged and the ratio of the A component to the B component is less than 25/65 or more than 45/45, the peel strength and tack of example 1 are significantly reduced as compared with examples 6 to 7. In the invention, the three components of the adhesive are compounded and act synergistically, and the component A can further increase the peel strength of the component B; the sustained viscosity of the component A can be further enhanced after the component B is crosslinked; the C component can further cure the A component and the B component, and can improve the peel strength and the permanent tack, but when the proportion of the A component to the B component is between 25/65 and 45/45 and the content of the C component is 10 percent, the performance of the adhesive obtained by the invention is optimal.
In the research and accumulation of many years, the applicant obtains three empirical formulas of the component A, the component B and the component C, the three components are different in performance, the preparation processes are greatly different, and the preparation process needs to be strictly controlled according to the process requirements. The component A and the component B are suitable for PVC films of different plasticizers, the component C mainly has the functions of proper curing and plasticizer migration retardation and can adapt to different climatic conditions after combination, wherein the plasticizer is more component A in the adhesive matched with the PVC film of DOS (cold resistance), the plasticizer is more component B in the adhesive matched with the PVC film of macromolecular polyester (heat resistance), and the dosage of the component A and the component B in the adhesive matched with the PVC film of DOP (common climate) is approximately equal. But the single formula adhesive has poor viscosity of the obtained adhesive tape, so the advantages of the three-component adhesive are combined, the advantages of the three-component adhesive are mutually made up for the disadvantages, the times of tests for obtaining the balance performance of the adhesive tape can be greatly reduced, the three-component adhesive is compounded and has synergistic effect, and the performance of the obtained three-component compound pressure-sensitive adhesive is obviously improved.
The technical solution of the present invention is further illustrated below with reference to a comparative example (single component).
Comparative example 1
The embodiment provides an adhesive, which comprises a component A, wherein the preparation method of the component A is similar to that of the component A in the embodiment 1; this example provides several a-component formulations, as shown in table 7.
TABLE 7
The adhesives obtained from 3 formulations in table 7 were coated on a PVC film 0.15mm in thickness (dry glue) with DOS as plasticizer to obtain the corresponding adhesive tapes: 25 μm; then, an electronic peel tester, an initial tack tester, and a permanent tack tester were used to perform the tests, and the test results are shown in table 8.
TABLE 8
| Item | Formulation I | Formulation II | Formulation III | Test method |
| Peel strength (N/cm) | 1.0 | 1.1 | 1.3 | GB/T2792-2014 |
| Initial viscosity (maximum ball number #) | 21 | 23 | 22 | GB/T4852-2002 |
| Viscosity (min) | 85 | 75 | 90 | GB/T4851-1998 |
As can be seen from Table 8, the initial viscosity of formula III is slightly lower than that of formula II, the other indexes are better than those of other formulas, and the comprehensive performance formula III is the best. However, the adhesive tape obtained in this example was far inferior to the adhesive tape obtained by the three-component dispenser of the present invention in peel strength and holding power, compared to the adhesive tape obtained in application example 3.
Comparative example 2
The embodiment provides an adhesive, which comprises a component B, wherein the preparation method of the component B is similar to that of the component B in the embodiment 1; this example provides several B-component formulations, as shown in table 9.
TABLE 9
The adhesive obtained from 3 formulations in table 9 was coated on a PVC film 0.15mm in thickness (dry adhesive) whose plasticizer was high molecular polyester to obtain the corresponding adhesive tape: 25 μm; then, an electronic peel tester, an initial tack tester, and a permanent tack tester were used to perform the tests, and the test results are shown in table 10.
Watch 10
| Item | Formulation I | Formulation II | Formulation III | Test method |
| Peel strength (N/cm) | 1.4 | 1.1 | 1.0 | GB/T2792-2014 |
| Initial viscosity (maximum ball number #) | 21 | 18 | 20 | GB/T4852-2002 |
| Viscosity (min) | 45 | 52 | 60 | GB/T4851-1998 |
As can be seen from Table 10, each index of the formulation is superior to that of the other formulations, and the combination property formulation is the best. However, the adhesive tape obtained in this example was far inferior to the adhesive tape obtained by the three-component dispenser of the present invention in peel strength and holding power, compared to the adhesive tape obtained in application example 1.
Comparative example 3
The embodiment provides an adhesive, which comprises a component C, wherein the preparation method of the component C is similar to that of the component C in the embodiment 1; this example provides several C-component formulations, as shown in table 11.
TABLE 11
The component C mainly acts as a moderate curing adhesive and retards the migration of a plasticizer, and the peel strength, initial viscosity and viscosity retention of the component C are difficult to obtain reliable data. The performance was evaluated as its ability to resist plasticizer migration under conditions of high temperature accelerated aging.
The adhesive obtained from the 3 formulations in table 11 was coated on a 0.15mm PVC film with the plasticizer DOP as a primer, and then coated with the same surface coating agent to obtain the corresponding adhesive tape, thickness of the coated adhesive (dry adhesive): 25 μm; then, three adhesive tapes are attached to the same standard steel plate, the steel plate is placed in a constant-temperature drying oven, aging is accelerated at the temperature of 80 ℃ for different time, the steel plate is cooled to room temperature after the aging is finished, the adhesive tapes are removed from the steel plate at the angle of 135 degrees at the speed of 100mm/min, the proportion of the residual adhesive area on the steel plate to the adhering area is judged by millimeter paper, the adhesive layer residual condition is observed, and the test results are shown in table 12.
TABLE 12
| Item | Formulation I | Formulation II | Formulation III |
| 80 ℃ for 3h (residual glue area ratio) (%) | 0 | 3 | 10 |
| 80 ℃ for 12h (residual glue area ratio) (%) | 0 | 10 | 25 |
| 80 ℃ for 24h (residual glue area ratio) (%) | 0 | 18 | 40 |
As can be seen from Table 12, formulation one is superior to the other formulations, and the combination property formulation one is the best.
The above-mentioned embodiments only express the specific embodiments of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (9)
1. The three-component composite pressure-sensitive adhesive is characterized by comprising the following raw materials in percentage by mass: 25-45% of the component A, 45-65% of the component B and 10% of the component C; wherein the component A comprises pangolin rubber, smoked sheet rubber, low-temperature polymerized styrene-butadiene rubber 1012, hydrogenated C5 petroleum resin LH100, C5 petroleum resin Y100, terpene resin T100, antioxidant 264, antioxidant DLTDP and toluene;
the component B comprises smoked sheet rubber, low-temperature polymerized styrene-butadiene rubber 1012, butyl rubber 1751, polymerized terpene resin 7042, terpene phenolic resin 138, anti-aging agent 264, anti-aging agent RD, magnesium oxide and toluene;
the component C comprises methyl methacrylate, butyl acrylate, benzoyl peroxide, styrene-butadiene rubber 303, an accelerator DM and toluene.
2. The three-component composite pressure-sensitive adhesive as claimed in claim 1, wherein the component A comprises 20-30 parts of natural nail rubber, 65 parts of tobacco flake adhesive, 101255-65 parts of low-temperature polymerized styrene-butadiene rubber, LH 10070-80 parts of hydrogenated C5 petroleum resin, Y10060-70 parts of C5 petroleum resin, T10010 parts of terpene resin, 2641 parts of anti-aging agent, DLTDP 1 part of antioxidant and 700 parts of toluene.
3. The three-component composite pressure-sensitive adhesive according to claim 1, wherein the component B comprises 85 to 95 parts of smoked sheet rubber, 101240 to 50 parts of low-temperature polymerized styrene-butadiene rubber, 175115 parts of butyl rubber, 7042115 to 125 parts of polymerized terpene resin, 13825 to 35 parts of terpene phenolic resin, 2641 parts of anti-aging agent, 1 part of anti-aging agent RD, 5 parts of magnesium oxide and 700 parts of toluene.
4. The three-component composite pressure-sensitive adhesive as claimed in claim 1, wherein the component C comprises 120-140 parts of methyl methacrylate, 30-50 parts of butyl acrylate, 7 parts of benzoyl peroxide, 303100 parts of styrene-butadiene rubber, 3 parts of accelerator DM and 1500 parts of toluene.
5. A process for the preparation of a three-component, pressure-sensitive adhesive composite according to any of claims 1 to 4, comprising the steps of:
step one, preparing a component A; the method specifically comprises the following steps:
1.1 adjusting the roll spacing of the open mill to 4mm, roughly refining the nomenclat rubber and the low-temperature polymerized styrene-butadiene rubber 1012 on the open mill for 5-6 times, reducing the roll spacing to 1mm, finely refining for 3 times, discharging and airing;
1.2 adjusting the roller spacing of the open mill to 2mm, finely milling the tobacco flake glue for 2 times, discharging and airing;
1.3, injecting toluene into a reaction kettle, starting stirring, sequentially adding the refined natural rubber of the step 1.1, the low-temperature polymerized styrene-butadiene rubber 1012 and the refined smoked sheet rubber of the step 1.2, stirring for 4 hours until the glue solution is uniform, and continuously introducing cooling water in the stirring process to prevent the temperature of the glue solution from being higher;
1.4 adding hydrogenated C5 petroleum resin LH100, C5 petroleum resin Y100, terpene resin T100, antioxidant 264 and antioxidant DLTDP, and stirring for 2 hours;
1.5, stopping the machine, filtering and discharging to obtain a component A for later use;
step two, preparing the component B; the method specifically comprises the following steps:
2.1 adjusting the roll spacing of the open mill to 4mm, roughly refining the tobacco flake glue on the open mill for 5-6 times, reducing the roll spacing to 1mm, finely refining for 3 times, discharging and airing;
2.2 adjusting the roll spacing of the open mill to 2mm, finely milling the low-temperature polymerized styrene-butadiene rubber 1012 and the butyl rubber 1751 for 2 times, discharging and airing;
2.3, injecting toluene into the reaction kettle, starting stirring, sequentially adding the smoked sheet rubber refined in the step 2.1 and the low-temperature polymerized styrene-butadiene rubber 1012 and the butyl rubber 1751 refined in the step 2.2, stirring for 4 hours until the glue solution is uniform, and continuously introducing cooling water in the stirring process to ensure that the temperature of the glue solution is not more than 45 ℃;
2.4 adding polymerized terpene resin 7042, antioxidant 264, antioxidant RD and magnesium oxide, and stirring for 2 hours;
2.5 checking the temperature of the glue solution, putting the terpene phenolic resin 138 into the glue solution at the temperature below 45 ℃, and stirring for 1 hour;
2.6, stopping the machine, filtering and discharging to obtain a component B for later use;
step three, preparing the component C; the method specifically comprises the following steps:
3.1 adjusting the roll spacing of the open mill to 2mm, finely milling the styrene-butadiene rubber 303 for 2 times, discharging and airing;
3.2 sequentially injecting 1/5 methyl methacrylate, 1/5 butyl acrylate and 2/7 benzoyl peroxide into the first pre-reaction kettle, and stirring for 30 minutes to obtain a first mixed solution for later use;
3.3 sequentially injecting the rest methyl methacrylate, butyl acrylate and benzoyl peroxide into the second pre-reaction kettle, and stirring for 30 minutes to obtain a second mixed solution for later use;
3.4, injecting toluene into the reaction kettle, starting stirring, adding the butadiene styrene rubber 303 refined in the step 3.1, stirring for 1 hour, and standing for 1 hour;
3.5 adding the accelerator DM into the reaction kettle after standing in the step 3.4, stirring for 5 minutes, and then heating to 80 ℃ and stabilizing for 5 minutes;
3.6 dropwise adding the first mixed solution obtained in the first pre-reaction kettle in the step 3.2 into the reaction kettle in the step 3.4, wherein the dropping is completed within 1 hour, the temperature is kept at 80-82 ℃ in the whole process, and then the temperature is kept at 82-84 ℃ for 1 hour;
3.7 dropwise adding the second mixed solution obtained in the second pre-reaction kettle in the step 3.3 into the reaction kettle after heat preservation in the step 3.6, finishing dropwise adding for 3 hours, keeping the temperature at 82-84 ℃ in the whole process, and then preserving the heat for 1 hour at 84-86 ℃;
3.8 cooling to below 40 ℃, filtering and discharging to obtain a component C for later use;
and step four, adding the component A, the component B and the component C into a mixing kettle according to the proportion of 25-45% of the component A, 45-65% of the component B and 10% of the component C, stirring for 2 hours, and discharging to obtain the three-component composite pressure-sensitive adhesive.
6. An adhesive tape, characterized in that the three-component composite pressure-sensitive adhesive according to any one of claims 1 to 7 is coated on a PVC film containing DOS, high molecular polyester or DOP as a main plasticizer.
7. The use according to claim 1, wherein said three-component compounded pressure-sensitive adhesive comprises 45% of component A, 45% of component B and 10% of component C when applied to a PVC film containing DOS as a main plasticizer.
8. The use according to claim 1, wherein the three-component pressure-sensitive adhesive composition comprises 25% of component A, 65% of component B and 10% of component C when applied to a PVC film comprising a high molecular weight polyester as a main plasticizer.
9. The use according to claim 1, wherein the three-component compounded pressure-sensitive adhesive comprises 35% of the A component, 55% of the B component and 10% of the C component when coated on a PVC film mainly comprising DOP as a plasticizer.
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| CN116355555A (en) * | 2023-04-10 | 2023-06-30 | 舒氏集团有限公司 | Adhesive, rubber layer and waterproof leak-repairing adhesive tape |
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|---|---|---|---|---|
| EP2818527A1 (en) * | 2013-06-24 | 2014-12-31 | Coroplast Fritz Müller GmbH & Co. KG | Adhesive tape, in particular double-sided adhesive tape, and its use as adhesive for non-polar surfaces |
| CN109762486A (en) * | 2018-11-30 | 2019-05-17 | 万洲胶粘制品(江苏)有限公司 | A kind of pressure-sensitive adhesive making flexible PVC electrical adhesive tape and its processing method |
| CN112409944A (en) * | 2020-11-17 | 2021-02-26 | 襄阳三沃航天薄膜材料有限公司 | Rubber type pressure-sensitive adhesive and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2818527A1 (en) * | 2013-06-24 | 2014-12-31 | Coroplast Fritz Müller GmbH & Co. KG | Adhesive tape, in particular double-sided adhesive tape, and its use as adhesive for non-polar surfaces |
| CN109762486A (en) * | 2018-11-30 | 2019-05-17 | 万洲胶粘制品(江苏)有限公司 | A kind of pressure-sensitive adhesive making flexible PVC electrical adhesive tape and its processing method |
| CN112409944A (en) * | 2020-11-17 | 2021-02-26 | 襄阳三沃航天薄膜材料有限公司 | Rubber type pressure-sensitive adhesive and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116355555A (en) * | 2023-04-10 | 2023-06-30 | 舒氏集团有限公司 | Adhesive, rubber layer and waterproof leak-repairing adhesive tape |
| CN116355555B (en) * | 2023-04-10 | 2023-09-19 | 舒氏集团有限公司 | Adhesive, rubber layer and waterproof leak-repairing adhesive tape |
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