A low temperature resistant Mopp tape and preparation method thereof
By using MOPP film and specific pressure-sensitive adhesives in low-temperature tape, the problem of unstable tape performance in low-temperature environments is solved, and higher low-temperature resistance and bonding performance are achieved.
Patent Information
- Application Number
- CN202411058832.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-02
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2044-08-02
AI Technical Summary
Existing low-temperature tapes are prone to rapid adhesion climbing, brittleness of the adhesive layer, poor bonding effect, loss of flexibility of the substrate, easy to break or tear during peeling, and poor storage and unstable performance.
A MOPP film is used as a substrate and a pressure-sensitive adhesive composed of specific components is coated on its surface. By selecting SIS, tackifying resin modification, and the combination of polyisobutylene and cycloane oil, a low-temperature resistant Mopp tape is prepared.
Within a wider operating temperature range, the smooth peeling performance and peeling state of the tape are maintained, which improves the low-temperature resistance and bonding properties of the tape, and reduces glue loss and residual glue.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of low-temperature adhesive tapes, in particular to a low-temperature resistant Mopp adhesive tape and a preparation method thereof. Background Art
[0002] With the development of economy and the progress of science and technology, the tape industry has made great progress. The tape consists of two parts: the substrate and the adhesive. It uses the bonding effect of the adhesive to connect two or more objects. According to the application environment temperature, it can be divided into low-temperature tape, normal temperature tape and high-temperature tape. However, some existing low-temperature tapes are prone to the following problems at extremely low temperatures: 1. The soft components in the adhesive tend to be in a glassy state, resulting in a sharp increase in adhesion, and the adhesive strength of the tape is close to the maximum value, which makes it easy to produce residual glue when peeling; 2. The compatibility of the free molecules inside the adhesive deteriorates, precipitates, and freezes, making the adhesive layer brittle and losing its pressure-sensitive properties; 3. Low temperature makes the bonding effect between the adhesive layer and the substrate worse, and it is easy to fall off; 4. The tape substrate loses its flexibility at low temperatures, and it is easy to break or tear when peeling and bending. Poor cutting of the tape edge makes it easier to tear when peeling; 5. Poor storage of the tape leads to unstable performance of the adhesive layer and substrate, which leads to aggravation of the undesirable phenomenon when peeling at extremely low temperatures. Therefore, we propose a low-temperature resistant Mopp tape and a preparation method thereof. Summary of the invention
[0003] The object of the present invention is to provide a low-temperature resistant Mopp tape and a preparation method thereof, so as to solve the problems raised in the above background technology.
[0004] In order to solve the above technical problems, the present invention provides the following technical solutions: A low temperature resistant Mopp tape, comprising a MOPP film and a pressure sensitive adhesive arranged on the surface of the MOPP film, wherein the pressure sensitive adhesive is obtained by coating and aging an adhesive solution;
[0005] The adhesive solution comprises the following components by weight: 10 parts of synthetic rubber, 4 to 6 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, and 10 parts of additives.
[0006] Furthermore, the synthetic rubber is a mixture of one or more of SEBS (hydrogenated styrene-butadiene block copolymer), SBS (styrene-butadiene-styrene block copolymer), and SIS (styrene-isoprene-styrene block copolymer).
[0007] In the above technical solution, the substrate of the low-temperature tape is MOPP film (longitudinal stretched polypropylene film), which has high longitudinal tensile strength and is resistant to low temperatures. It eliminates the negative impact caused by substrate performance in low-temperature environments and is more suitable for application on low-temperature tapes.
[0008] In the above technical solution, SIS is selected as the synthetic rubber. SIS has the characteristics of low modulus, low viscosity, good processing performance, etc. The methyl side chain characteristics of the olefin structure give it better cohesion and excellent bonding performance. The prepared pressure-sensitive adhesive layer can obtain a lower glass transition temperature (Tg) and better cold resistance, making the prepared tape more adaptable to low temperatures.
[0009] Furthermore, the tackifying resin is a mixture of one or more of epoxy resin, silicone resin, polyurethane, chlorinated polyolefin, petroleum resin, terpene resin, rosin resin, and coumarone resin.
[0010] Further, the auxiliary agent includes 8.0 to 8.9 parts of toluene, 1.0 to 1.5 parts of ethyl acetate and 0.1 to 0.5 parts of a leveling agent;
[0011] Polyisobutylene is a low molecular weight polyisobutylene;
[0012] Naphthenic oil: 4010, industrial grade.
[0013] In the above technical solution, low molecular weight polyisobutylene is selected, which has good compatibility with the adhesive material, has low temperature dispersibility, and can improve the lubricity and low temperature resistance of the pressure sensitive adhesive layer. Naphthenic oil can reduce the glass transition temperature of the adhesive polymer, improve the brittleness of the pressure sensitive adhesive layer, and improve its flexibility; it has good compatibility with SIS rubber, improves the wettability of the pressure sensitive adhesive layer on the surface of the bonded material, and is conducive to improving the adhesion of the tape.
[0014] A method for preparing a low-temperature resistant Mopp tape comprises the following process steps:
[0015] Step 1, preparing glue solution: mixing tackifying resin with polyisobutylene and cyclohexane oil, stirring and heating to 150-200° C. under nitrogen atmosphere protection, adding synthetic rubber, stirring until the system becomes transparent; cooling, adding additives, and obtaining glue solution;
[0016] Step 2: Apply the adhesive solution on the surface of the MOPP film, cure it, form a pressure-sensitive adhesive, and obtain a MOPP tape.
[0017] Furthermore, the aging process conditions are: baking at 110-130°C for 2-3 minutes; aging at 30-35°C for 2-3 days.
[0018] Furthermore, the thickness of the MOPP film is 25 to 80 μm; the coating amount of the adhesive is 100 to 150 g / m 2 .
[0019] Furthermore, one side of the MOPP film (non-glue coating side) is provided with a release layer, and the release layer is obtained by coating with organic silicone oil, and the coating amount of the organic silicone oil is 6 to 15 g / m 2.
[0020] Furthermore, before the adhesive is applied, the surface of the MOPP film is pre-coated with a primer; the amount of the primer applied is 8 to 15 g / m 2 ;
[0021] The MOPP tape includes the following structures from top to bottom: release layer, MOPP film, primer and pressure-sensitive adhesive.
[0022] Further, the tackifying resin is prepared by the following process:
[0023] The rosin ester is ground into powder, a long-chain acid is added, the temperature is raised to 250-260°C, and the reaction is kept at this temperature for 5-7 hours to obtain a tackifying resin.
[0024] Furthermore, the rosin ester is one of rosin glycerol ester (CAS No.: 8050-31-5) and rosin pentaerythritol ester (CAS No.: 64365-17-9).
[0025] Further, rosin ester is prepared by the following process:
[0026] Mix rosin, antioxidant 300 and catalyst Z501, raise the temperature to 220-230°C under nitrogen atmosphere, slowly add unsaturated polyol within 30 minutes, raise the temperature to 260-270°C, keep the temperature for 6-8 hours to obtain rosin ester;
[0027] The antioxidant is 300, and the dosage is 0.5% to 1.0% of the mass of rosin;
[0028] The catalyst is Z501, and the dosage is 0.8% to 1.5% of the mass of rosin.
[0029] Furthermore, the mass ratio of unsaturated polyol to rosin is (2.3-5.0):1.
[0030] Furthermore, the long-chain acid is one of stearic acid and carboxyl-terminated polydimethylsiloxane;
[0031] The mass of the long-chain acid is 32% to 50% of the mass of the rosin ester.
[0032] In the above technical scheme, rosin ester resin has a good tackifying effect, can improve the wettability, cohesion, peel strength and shear strength of the glue polymer, enhance its initial cohesion and long-term bonding strength, reduce the viscosity of the pressure-sensitive adhesive, and improve the wetting and bonding properties between the adhered material and the tape. Rosin ester selects rosin glycerol ester or rosin pentaerythritol ester, and its structure contains hydroxyl groups. The hydroxyl groups in the rosin ester are esterified with long-chain acids, and dehydration reaction is performed to obtain a tackifying resin. The long-chain acid is stearic acid or carboxyl-terminated polydimethylsiloxane. Introducing long-chain fatty acids (stearic acid) into the rosin resin structure can adjust the viscosity of the glue, reduce the softening point and viscosity of the tackifying resin; and can weaken the interaction between the molecular chains of the glue, reduce Tg and processing temperature, thereby achieving an improvement in the low temperature resistance of the pressure-sensitive adhesive layer.
[0033] The introduced silicone segment (carboxyl-terminated polydimethylsiloxane) has better molecular flexibility and low-temperature resistance, and weaker intermolecular forces. In addition to better low-temperature resistance, due to its low surface tension characteristics, it can reduce the surface tension of the adhesive and promote film formation. It has better adhesion and adsorption with the base glue, and can better bond the pressure-sensitive adhesive layer to the substrate (MOPP film), which helps it to wetting the surface of the substrate and the bonded material, thereby obtaining better adhesion performance and being less likely to be peeled off from the substrate surface.
[0034] Further, the unsaturated polyol is prepared by the following process:
[0035] Mix 1,3,5-tris(2-hydroxyethyl)cyanuric acid and a catalyst, add propylene oxide and glycidol under nitrogen atmosphere, heat to 130-135°C, and react until the pressure gauge does not drop; perform rotary evaporation to obtain a branched polyether;
[0036] The branched polyether, potassium metal and tetrahydrofuran are mixed, stirred and heated to 50-60°C, and reacted for 8-10 hours; cooled to room temperature, epichlorohydrin is added, and stirred to react for 3-4 hours; allowed to stand, the precipitate is filtered off, vacuum distilled, washed, and vacuum dried to obtain an epoxy-terminated polyether;
[0037] The epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide are mixed, and the temperature is raised to 120-130° C. under the protection of nitrogen atmosphere, and the reaction is performed until the epoxy value of the system is less than 0.1% to obtain an unsaturated polyol.
[0038] Further, the mass ratio of 1,3,5-tris(2-hydroxyethyl)cyanuric acid, propylene oxide and glycidol is 10:(0-6.7):(0-8.7);
[0039] The catalyst is double metal cyanide (DMC), and the dosage is 0.5% to 1.2% of the mass of 1,3,5-tris(2-hydroxyethyl)cyanuric acid.
[0040] Further, the ratio of branched polyether, potassium metal, and tetrahydrofuran is 10 g:(2.4-4.0) g:20 mL;
[0041] The mass ratio of branched polyether to epichlorohydrin is 10:(6.4-11.5).
[0042] Furthermore, the mass ratio of epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide is 10:(14.9-23.5):(0.12-0.20).
[0043] In the above technical scheme, rosin ester can also be obtained by reacting rosin and unsaturated polyols. Unsaturated polyols are obtained by reacting epoxy-terminated polyethers and ricinoleic acid, and carboxyl groups react with epoxy groups to generate hydroxyl groups and epoxy ester structures. Ricinoleic acid is an unsaturated fatty acid, and carbon-carbon double bonds are introduced through the above reaction. While obtaining hydroxyl groups, flexible chains (ricinoleic acid residues) and epoxy resin properties (excellent adhesion and water resistance) are obtained, which is beneficial to the improvement of low temperature resistance and adhesion of pressure-sensitive adhesives. Epoxy-terminated polyethers are obtained by reacting branched polyethers and epichlorohydrin, and branched polyethers are prepared from 1,3,5-tris(2-hydroxyethyl)cyanuric acid, propylene oxide, and glycidol. By reacting the hydroxyl group in 1,3,5-tris(2-hydroxyethyl)cyanuric acid with the epoxy group to form a branched structure, generate ether bonds, and introduce heteroatoms, the structural flexibility is improved and the low-temperature resistance of the adhesive layer is improved; and the obtained tackifying resin has a macromolecular characteristic and has good compatibility with other components of the adhesive solution, which can avoid its precipitation at low temperatures.
[0044] Furthermore, the MOPP film can be subjected to corona treatment to reduce the surface tension of the film, enhance the bonding performance between the tape substrate and the pressure-sensitive adhesive, and help eliminate the adhesive peeling phenomenon.
[0045] Compared with the prior art, the present invention has the following beneficial effects:
[0046] 1. The low-temperature resistant Mopp tape described in the present invention can maintain stable peeling performance and peeling state in a wider operating temperature range by screening the adhesive liquid components and adjusting the material ratio.
[0047] 2. The present invention describes a method for preparing a low-temperature resistant Mopp tape, which reduces the Tg and processing temperature of the tackifying resin and weakens the interaction between the molecular chains of the adhesive, thereby improving the low-temperature resistance and peeling performance of the pressure-sensitive adhesive layer through modification and preparation of the tackifying resin and introduction of a branched structure and a flexible molecular chain. DETAILED DESCRIPTION
[0048] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0049] In the following specific implementations,
[0050] SIS: 1105, from Sinopec Baling Petrochemical Co., Ltd.;
[0051] Naphthenic oil: 4010, industrial grade, sourced from Xinjiang Karamay Petrochemical Co., Ltd.;
[0052] Polyisobutylene: PB300, Mn=1300, from Daelim Co., Ltd., South Korea;
[0053] Leveling agent: BYK373, from BYK, Germany;
[0054] The catalyst was double metal cyanide (DMC), which was sourced from Qingdao Xinyutian Chemical Co., Ltd.;
[0055] Carboxyl-terminated polydimethylsiloxane: Carboxypropyl-terminated polydimethylsiloxane, sourced from Shanghai Yuanye Biotechnology Co., Ltd.
[0056] The thickness of the MOPP film is 50 μm, and it comes from Guangdong Huaducheng Group Co., Ltd. The surface to be coated with the adhesive is corona treated before use, and the surface tension off the machine is 44 dynes.
[0057] One side of the MOPP film (non-glue coated side) is provided with a release layer, which is coated with organic silicone oil. The coating amount of organic silicone oil is 10g / m 2 ; Silicone oil: SYL-OFF TM EM-7934, from Dow Chemical;
[0058] Before the adhesive is applied, the surface of the MOPP film is pre-coated with a primer; the amount of primer applied is 8g / m 2 ; Primer: 3M TM 94, from 3M China;
[0059] Rosin resin: GHR-80, sourced from Guangzhou Shixian Chemical Co., Ltd.
[0060] Embodiment 1: A method for preparing a low-temperature resistant Mopp tape, comprising the following process steps:
[0061] Step 1: Prepare glue solution:
[0062] 1.1. Mix 1,3,5-tris(2-hydroxyethyl)cyanuric acid and 0.5% catalyst, add propylene oxide under nitrogen atmosphere, heat to 130°C, and react until the pressure gauge does not drop; rotary evaporation to obtain branched polyether; the mass ratio of 1,3,5-tris(2-hydroxyethyl)cyanuric acid to propylene oxide is 10:6.7;
[0063] The branched polyether, potassium metal and tetrahydrofuran were mixed, stirred and heated to 50°C, and reacted for 8 hours; cooled to room temperature, epichlorohydrin was added, and stirred for reaction for 3 hours; allowed to stand, the precipitate was filtered off, vacuum distilled, washed, and vacuum dried to obtain an epoxy-terminated polyether; the ratio of branched polyether, potassium metal and tetrahydrofuran was 10g:2.4g:20mL; the mass ratio of branched polyether and epichlorohydrin was 10:6.4;
[0064] The epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide are mixed, and the temperature is raised to 120° C. under the protection of nitrogen atmosphere, and the reaction is carried out until the epoxy value of the system is less than 0.1% to obtain an unsaturated polyol; the mass ratio of the epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide is 10:14.9:0.12;
[0065] 1.2. Mix rosin, antioxidant 300 and catalyst Z501, raise the temperature to 220°C under nitrogen atmosphere, slowly add unsaturated polyol, add within 30 minutes, raise the temperature to 260°C, keep the temperature for 6 hours to obtain rosin ester; the mass ratio of unsaturated polyol to rosin is 4.96:1;
[0066] Grind the rosin ester into powder, add stearic acid, heat to 250°C, and keep the temperature for 5 hours to obtain a tackifying resin; the mass of the stearic acid is 32.0% of the mass of the rosin ester;
[0067] 1.3. Mix the tackifying resin with polyisobutylene and cyclohexane oil, stir and heat to 150°C under the protection of nitrogen atmosphere, add synthetic rubber, stir until the system becomes transparent; cool, add additives to obtain glue solution; the glue solution includes the following mass components: 10 parts of synthetic rubber SIS, 4 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, 10 parts of additives; the additives include 8.9 parts of toluene, 1.0 parts of ethyl acetate and 0.1 parts of leveling agent;
[0068] Step 2: Apply the adhesive on the surface of the MOPP film. The coating amount of the adhesive is 100g / m 2 ; Ripening, aging process conditions: baking at 110°C for 2 minutes; aging at 30°C for 2 days to form a pressure-sensitive adhesive and obtain a MOPP tape.
[0069] Embodiment 2: A method for preparing a low-temperature resistant Mopp tape, comprising the following process steps:
[0070] Step 1: Prepare glue solution:
[0071] 1.1. Mix 1,3,5-tris(2-hydroxyethyl)cyanuric acid and 0.8% catalyst, add propylene oxide and glycidol under nitrogen atmosphere, heat to 132°C, and react until the pressure gauge does not drop; rotary evaporation to obtain branched polyether; the mass ratio of 1,3,5-tris(2-hydroxyethyl)cyanuric acid, propylene oxide and glycidol is 10:2.3:5.8;
[0072] The branched polyether, potassium metal and tetrahydrofuran were mixed, stirred and heated to 55°C, and reacted for 9 hours; cooled to room temperature, epichlorohydrin was added, and stirred for reaction for 3.5 hours; allowed to stand, the precipitate was filtered off, vacuum distilled, washed, and vacuum dried to obtain epoxy-terminated polyether; the ratio of branched polyether, potassium metal and tetrahydrofuran was 10g:3.2g:20mL; the mass ratio of branched polyether and epichlorohydrin was 1:1;
[0073] The epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide are mixed, and the temperature is raised to 125° C. under the protection of nitrogen atmosphere, and the reaction is carried out until the epoxy value of the system is less than 0.1% to obtain an unsaturated polyol; the mass ratio of the epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide is 10:20:0.16;
[0074] 1.2. Mix rosin, 0.8% antioxidant 300 and 1.2% catalyst Z501, heat to 225°C under nitrogen atmosphere, slowly add unsaturated polyol, add within 30 minutes, heat to 265°C, keep warm for 7 hours to obtain rosin ester; the mass ratio of unsaturated polyol to rosin is 3.70:1;
[0075] Grind the rosin ester into powder, add carboxyl-terminated polydimethylsiloxane, raise the temperature to 255°C, and keep the temperature for 6 hours to obtain a tackifying resin; the mass of the carboxyl-terminated polydimethylsiloxane is 49.2% of the mass of the rosin ester;
[0076] 1.3. Mix the tackifying resin with polyisobutylene and cyclohexane oil, stir and heat to 175°C under the protection of nitrogen atmosphere, add synthetic rubber, stir until the system becomes transparent; cool, add additives to obtain glue solution; the glue solution includes the following mass components: 10 parts of synthetic rubber SIS, 5 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, 10 parts of additives; the additives include 8.5 parts of toluene, 1.2 parts of ethyl acetate and 0.3 parts of leveling agent;
[0077] Step 2: Apply the adhesive on the surface of the MOPP film. The coating amount of the adhesive is 125g / m 2 ; Ripening, aging process conditions: baking at 120°C for 2.5 minutes; aging at 32°C for 2.5 days to form a pressure-sensitive adhesive and obtain a MOPP tape.
[0078] Embodiment 3: A method for preparing a low temperature resistant Mopp tape, comprising the following process steps:
[0079] Step 1: Prepare glue solution:
[0080] 1.1. Mix 1,3,5-tris(2-hydroxyethyl)cyanuric acid and 1.2% catalyst, add propylene oxide and glycidol under nitrogen atmosphere, heat to 135°C, and react until the pressure gauge does not drop; perform rotary evaporation to obtain branched polyether; the mass ratio of 1,3,5-tris(2-hydroxyethyl)cyanuric acid to glycidol is 10:8.7;
[0081] The branched polyether, potassium metal and tetrahydrofuran were mixed, stirred and heated to 60°C, and reacted for 10 hours; cooled to room temperature, epichlorohydrin was added, and stirred for 4 hours; allowed to stand, the precipitate was filtered off, vacuum distilled, washed, and vacuum dried to obtain an epoxy-terminated polyether; the ratio of branched polyether, potassium metal and tetrahydrofuran was 10g:4.0g:20mL; the mass ratio of branched polyether and epichlorohydrin was 10:11.5;
[0082] The epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide are mixed, and the temperature is raised to 130° C. under the protection of nitrogen atmosphere, and the reaction is carried out until the epoxy value of the system is less than 0.1% to obtain an unsaturated polyol; the mass ratio of the epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide is 10:23.5:0.20;
[0083] 1.2. Mix rosin, 1.0% antioxidant 300 and 1.5% catalyst Z501, heat to 230°C under nitrogen atmosphere, slowly add polyol, add within 30 minutes, heat to 270°C, keep warm for 8 hours to obtain rosin ester; the mass ratio of unsaturated polyol to rosin is 2.39:1;
[0084] Grind the rosin ester into powder, add carboxyl-terminated polydimethylsiloxane, raise the temperature to 260°C, and keep the temperature for 7 hours to obtain a tackifying resin; the mass of the carboxyl-terminated polydimethylsiloxane is 45.8% of the mass of the rosin ester;
[0085] 1.3. Mix the tackifying resin with polyisobutylene and cyclohexane oil, stir and heat to 200°C under the protection of nitrogen atmosphere, add synthetic rubber, stir until the system becomes transparent; cool, add additives to obtain glue solution; the glue solution includes the following mass components: 10 parts of synthetic rubber SIS, 6 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, 10 parts of additives; the additives include 8.9 parts of toluene, 1.0 parts of ethyl acetate and 0.1 parts of leveling agent;
[0086] Step 2: Apply the adhesive on the surface of the MOPP film. The coating amount of the adhesive is 150g / m 2; Ripening, aging process conditions: baking at 130°C for 3 minutes; aging at 35°C for 3 days to form a pressure-sensitive adhesive and obtain a MOPP tape.
[0087] Comparative Example 1: A method for preparing a low-temperature resistant Mopp tape, comprising the following process steps:
[0088] Step 1: Prepare glue solution:
[0089] 1.1. Mix 1,3,5-triglycidyl-S-triazinetrione, ricinoleic acid and tetrabutylammonium bromide, and heat to 120°C under nitrogen atmosphere to react until the epoxy value of the system is less than 0.1% to obtain an unsaturated polyol; the mass ratio of 1,3,5-triglycidyl-S-triazinetrione, ricinoleic acid and tetrabutylammonium bromide is 10:30.2:0.12;
[0090] 1.2. Mix rosin, antioxidant 300 and catalyst Z501, raise the temperature to 220°C under nitrogen atmosphere, slowly add unsaturated polyol, add within 30 minutes, raise the temperature to 260°C, keep the temperature for 6 hours to obtain rosin ester; the mass ratio of unsaturated polyol to rosin is 3.77:1;
[0091] Grind the rosin ester into powder, add stearic acid, heat to 250°C, and keep the temperature for 5 hours to obtain a tackifying resin; the mass of the stearic acid is 40.0% of the mass of the rosin ester;
[0092] 1.3. Mix the tackifying resin with polyisobutylene and cyclohexane oil, stir and heat to 150°C under the protection of nitrogen atmosphere, add synthetic rubber, stir until the system becomes transparent; cool, add additives to obtain glue solution; the glue solution includes the following mass components: 10 parts of synthetic rubber SIS, 4 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, 10 parts of additives; the additives include 8.9 parts of toluene, 1.0 parts of ethyl acetate and 0.1 parts of leveling agent;
[0093] Step 2: Apply the adhesive on the surface of the MOPP film. The coating amount of the adhesive is 100g / m 2 ; Ripening, aging process conditions: baking at 110°C for 2 minutes; aging at 30°C for 2 days to form a pressure-sensitive adhesive and obtain a MOPP tape.
[0094] Comparative Example 2: A method for preparing a low-temperature resistant Mopp tape, comprising the following process steps:
[0095] Step 1: Prepare glue solution:
[0096] 1.1. Grind rosin glycerol ester into powder, add stearic acid, heat to 250℃, keep warm for 5h to obtain tackifying resin; the mass of stearic acid is 1.51 of the mass of rosin glycerol ester;
[0097] 1.2. Mix the tackifying resin with polyisobutylene and cyclohexane oil, stir and heat to 150°C under the protection of nitrogen atmosphere, add synthetic rubber, stir until the system becomes transparent; cool, add additives to obtain glue solution; the glue solution includes the following mass components: 10 parts of synthetic rubber SIS, 4 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, 10 parts of additives; the additives include 8.9 parts of toluene, 1.0 parts of ethyl acetate and 0.1 parts of leveling agent;
[0098] Step 2: Apply the adhesive on the surface of the MOPP film. The coating amount of the adhesive is 100g / m 2 ; Ripening, aging process conditions: baking at 110°C for 2 minutes; aging at 30°C for 2 days to form a pressure-sensitive adhesive and obtain a MOPP tape.
[0099] Comparative Example 3: A method for preparing a low-temperature resistant Mopp tape, comprising the following process steps:
[0100] Step 1: Prepare glue solution:
[0101] The tackifying resin is mixed with polyisobutylene and cyclohexane oil, and the mixture is stirred and heated to 150°C under the protection of nitrogen atmosphere, and synthetic rubber is added and stirred until the system becomes transparent; the mixture is cooled and an auxiliary agent is added to obtain a glue solution; the glue solution includes the following components by mass: 10 parts of synthetic rubber SIS, 4 parts of rosin resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, and 10 parts of auxiliary agents; the auxiliary agents include 8.9 parts of toluene, 1.0 parts of ethyl acetate, and 0.1 parts of a leveling agent;
[0102] Step 2: Apply the adhesive on the surface of the MOPP film. The coating amount of the adhesive is 100g / m 2 ; Ripening, aging process conditions: baking at 110°C for 2 minutes; aging at 30°C for 2 days to form a pressure-sensitive adhesive and obtain a MOPP tape.
[0103] Experiment: Take the MOPP tapes obtained in Examples 1-3 and Comparative Examples 1-3, prepare samples, test their properties respectively and record the test results:
[0104] Peel strength test: GB / T 2792 is used as the reference standard, and an electronic tensile machine is used to test the 180° peel strength of the sample; the experimental temperature is 25±1℃, and the tensile rate is 300mm / min;
[0105] Low temperature resistance test: Place the sample in a -30℃ refrigerator for 1 hour, stick it on a steel plate, place it in the refrigerator again for 24 hours, take it out, and perform a peel strength test within 2 minutes; use GB / T 4851 as a reference document to test its adhesion.
[0106] Room temperature peel strength (N / 2.5mm) Low temperature peel strength (N / cm) Stickiness (h) Example 1 19.0 15.3 >48 Example 2 19.7 16.4 >48 Example 3 19.5 16.0 >48 Comparative Example 1 18.3 12.7 35 Comparative Example 2 17.3 8.6 24 Comparative Example 3 15.5 / /
[0107] According to the data in the above table, we can clearly draw the following conclusions:
[0108] The MOPP tapes obtained in Examples 1-3 are compared with the MOPP tapes obtained in Comparative Examples 1-3. The test results show that:
[0109] Compared with the comparative example, the MOPP tape obtained in Examples 1-3 has higher room temperature peel strength, low temperature peel strength, and adhesion time, and no residual adhesive or adhesive fall-off phenomenon was found in the experiment. This fully demonstrates that the present invention achieves improvement in the adhesive performance, low temperature resistance, and peeling performance of the prepared tape.
[0110] Compared with Example 1, the synthesis process of the unsaturated polyol in Comparative Example 1 and the components used are different; the tackifying resin in Comparative Example 2 is obtained by reacting rosin glycerol ester and stearic acid. The room temperature peel strength, low temperature peel strength and adhesion time data of the MOPP tape obtained in Comparative Examples 1-2 decreased. The tackifying resin in Comparative Example 3 is a commercial product, and the obtained tape has a low room temperature peel strength and falls off in the low temperature test. It can be seen that the preparation process of the tape and the setting of the components used in the present invention can promote the improvement of its bonding performance, low temperature resistance and peeling performance.
[0111] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process method article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process method article or device.
[0112] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. A method for preparing a low-temperature resistant Mopp tape, characterized in that: The process steps include: Step 1, preparing glue solution: mixing tackifying resin with polyisobutylene and cyclohexane oil, stirring and heating to 150-200° C. under nitrogen atmosphere protection, adding synthetic rubber, stirring until the system becomes transparent; cooling, adding additives, and obtaining glue solution; Step 2, coating the adhesive solution on the surface of the MOPP film, ripening it to form a pressure-sensitive adhesive, and obtaining a MOPP tape; The tackifying resin is prepared by the following process: grinding rosin ester into powder, adding long-chain acid, heating to 250-260° C., and keeping the temperature for reaction for 5-7 hours to obtain the tackifying resin; The rosin ester is prepared by the following process: rosin, antioxidant 300 and catalyst Z501 are mixed, the temperature is raised to 220-230° C. under the protection of nitrogen atmosphere, unsaturated polyol is slowly added within 30 minutes, the temperature is raised to 260-270° C., and the temperature is kept for reaction for 6-8 hours to obtain rosin ester; The unsaturated polyol is prepared by the following process: Mix 1,3,5-tris(2-hydroxyethyl)cyanuric acid and a catalyst, add propylene oxide and glycidol under nitrogen atmosphere protection, heat to 130-135°C, react, and obtain a branched polyether; The branched polyether, potassium metal and tetrahydrofuran are mixed, stirred and heated to 50-60°C, and reacted for 8-10 hours; cooled to room temperature, epichlorohydrin is added, and stirred and reacted for 3-4 hours to obtain an epoxy-terminated polyether; Mix epoxy-terminated polyether, ricinoleic acid and tetrabutylammonium bromide, raise the temperature to 120-130° C. under nitrogen atmosphere protection, and react to obtain unsaturated polyol; The adhesive solution comprises the following components by weight: 10 parts of synthetic rubber, 4 to 6 parts of tackifying resin, 7 parts of polyisobutylene, 7 parts of cyclohexane oil, and 10 parts of additives.
2. The method for preparing a low-temperature resistant Mopp tape according to claim 1, characterized in that: The MOPP tape comprises a MOPP film and a pressure-sensitive adhesive arranged on the surface of the MOPP film, wherein the pressure-sensitive adhesive is obtained by coating and aging an adhesive solution.
3. The method for preparing a low-temperature resistant Mopp tape according to claim 1, characterized in that: The synthetic rubber is a mixture of one or more of SEBS, SBS and SIS.
4. The method for preparing a low-temperature resistant Mopp tape according to claim 1, characterized in that: The process conditions for the aging are as follows: baking at a temperature of 110 to 130° C. for 2 to 3 minutes; and aging at a temperature of 30 to 35° C. for 2 to 3 days.
5. The method for preparing a low-temperature resistant Mopp tape according to claim 1, characterized in that: The long-chain acid is one of stearic acid and carboxyl-terminated polydimethylsiloxane.
6. The method for preparing a low-temperature resistant Mopp tape according to claim 1, characterized in that: The mass ratio of 1,3,5-tris(2-hydroxyethyl)cyanuric acid, propylene oxide and glycidol is 10:(0-6.7):(0-8.7); The mass ratio of branched polyether to epichlorohydrin is 10:(6.4-11.5); The mass ratio of epoxy-terminated polyether to ricinoleic acid is 10:(14.9-23.5).
Citation Information
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