Butyl rubber hot melt adhesive with good high temperature resistance, preparation method and automobile hole plugging patch using the same

Through the blending and modification of butyl rubber, ethylene propylene ternary rubber and natural rubber, combined with the addition of bromotriazine, antimony trioxide and polyamide wax, the problem of insufficient high-temperature resistance and flame retardant properties of butyl rubber hot melt adhesive is solved, and stability and safety in high-temperature environments are achieved.

CN115926682BActive Publication Date: 2025-03-18CHANGZHOU AILONGSEN ADHESIVE TAPE CO LTD
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Patent Information

Application Number
CN202310021715.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-01-06
Publication Date
2025-03-18
Estimated Expiration
2043-01-06

AI Technical Summary

Technical Problem

The existing butyl rubber hot melt adhesive has poor high temperature resistance and will flow under high temperature conditions, making it unable to be used in use scenarios with higher ambient temperatures. At the same time, its flame retardant performance is also poor, which poses a safety hazard.

Method used

Through the blending modification of butyl rubber, ethylene propylene ternary rubber and natural rubber, thermodynamic stability and high temperature resistance are improved; bromotriazine and antimony trioxide are added to improve flame retardant performance; polyamide wax is activated at high temperature to form a network structure, which improves anti-sagging and anti-sagging capabilities.

Benefits of technology

It significantly improves the high temperature resistance and flame retardant properties of butyl rubber hot melt adhesive, and does not flow under high temperature environments, ensuring the firmness of the patch seal.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a butyl rubber hot melt adhesive with good high temperature resistance, a preparation method and an automotive plugging patch using the same, wherein the butyl rubber hot melt adhesive comprises the following weight components: 10-18 parts of butyl rubber, 1-3 parts of EPDM rubber, 2-4 parts of natural rubber, 11-17 parts of polyisobutylene, 10-15 parts of plasticizer, 32-50 parts of filler, 6-9 parts of terpene resin, 10-15 parts of bromotriazine, 4-7 parts of antimony trioxide, 1-3 parts of polyamide wax, and 0.5-1.5 parts of antioxidant. The butyl rubber hot melt adhesive of the present invention greatly improves the thermodynamic stability, high temperature resistance, flame retardancy, and anti-sagging performance of the butyl rubber hot melt adhesive at high temperature; the preparation method of the present invention has simple operating steps, high feasibility of implementation, and the production process does not need to add other equipment, which is convenient for directly implementing production in the existing high temperature resistant flame retardant plugging patch production line.
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Description

Technical Field

[0001] The invention relates to the technical field of hot melt adhesives, and in particular to a butyl rubber hot melt adhesive with good high temperature resistance, a preparation method and an automobile hole plugging patch using the same. Background Art

[0002] During the automobile production process, some process holes need to be opened on the surface of the body sheet metal to meet the production and assembly requirements. However, after the automobile is processed, these process holes are not only the entrance of water, dust and noise, but also affect the overall aesthetics of the car body. Therefore, during the assembly process of the car, the process holes on the body sheet metal need to be sealed. For the process holes on the automobile body sheet metal, usually according to the location of the process hole, sealing requirements and other factors, the choice of using a plug cover or a patch is selected. Among them, the patch sealing method is more widely used than the plug cover sealing method because the patch occupies a small space after sealing.

[0003] The high temperature resistant flame retardant patch used to plug the process holes on the automobile body sheet metal consists of three parts: substrate layer, adhesive layer and release paper, wherein the substrate layer usually includes glass fiber cloth and aluminum foil. The plugging patch can be cut into corresponding sizes according to the size of the process hole on the automobile sheet metal and provided to the automobile production line for use. One size of the plugging patch can correspond to process holes of multiple sizes while meeting the space requirements of the application position, so as to reduce the specifications of the plugging patches to be prepared and reduce the cost of warehousing and logistics. Different materials of patch products can also be selected according to the requirements of the use environment. For example, for process holes that have no special requirements for the use temperature, only plugging patches that meet the room temperature requirements are needed.

[0004] Compared with other hot melt adhesives, butyl rubber hot melt adhesive has much higher flexibility, elasticity, low temperature resistance and aging resistance than other hot melt adhesives, so it has been increasingly widely used in packaging, construction, automobile and other industries. For example, automobile sheet metal hole plugging patches using butyl rubber hot melt adhesive as the adhesive layer are also widely used. However, due to the poor high temperature resistance of butyl rubber hot melt adhesive and its tendency to flow under high temperature conditions, it cannot be used in scenarios with high ambient temperatures. Therefore, automobile sheet metal process hole plugging patches using butyl rubber hot melt adhesive as the adhesive layer can only be used in normal temperature scenarios, and due to the poor flame retardant properties of the adhesive layer of the plugging patch, there will also be some hidden dangers to safety in use. Summary of the invention

[0005] The purpose of the present invention is to overcome the defects existing in the prior art, and provide a butyl rubber hot melt adhesive with good high temperature resistance, a preparation method and an automotive plugging patch using the same. The butyl rubber hot melt adhesive with good high temperature resistance of the present invention is modified by blending butyl rubber, EPDM rubber and natural rubber, which greatly improves the thermodynamic stability and high temperature resistance of the butyl rubber hot melt adhesive; by adding bromotriazine and antimony trioxide, the flame retardant performance of the butyl rubber hot melt adhesive is greatly improved; polyamide wax is effectively activated at high temperature, and it forms a strong network structure in the butyl rubber hot melt adhesive system, and its excellent thixotropic properties make the butyl rubber hot melt adhesive have excellent anti-sagging ability and anti-sedimentation ability. The preparation method of a butyl rubber hot melt adhesive with good high temperature resistance of the present invention has simple operation steps, high feasibility of implementation, and no additional equipment is required in the production process, which is convenient for direct production in the existing high temperature resistant flame retardant plugging patch production line. The patch prepared by the butyl rubber hot melt adhesive with good high temperature resistance of the present invention has excellent thermodynamic stability, high temperature resistance and flame retardant performance, and does not flow under high temperature environment, thereby ensuring the sealing firmness of the patch during use.

[0006] One of the purposes of the present invention is to design a butyl rubber hot melt adhesive with good high temperature resistance, comprising the following components by weight: 10 to 18 parts of butyl rubber, 1 to 3 parts of EPDM rubber, 2 to 4 parts of natural rubber, 11 to 17 parts of polyisobutylene, 10 to 15 parts of plasticizer, 32 to 50 parts of filler, 6 to 9 parts of terpene resin, 10 to 15 parts of brominated triazine, 4 to 7 parts of antimony trioxide, 1 to 3 parts of polyamide wax, and 0.5 to 1.5 parts of antioxidant.

[0007] The preferred technical solution is that the viscosity of the polyisobutylene measured at 100° C. is 600-100 CS.

[0008] Another preferred technical solution is that the plasticizer is one or more of paraffin oil, dioctyl phthalate, and diisodecyl phthalate.

[0009] Another preferred technical solution is that the filler is one or more of calcium carbonate, barium sulfate, and silicon micropowder.

[0010] Another preferred technical solution is that the antioxidant model is one or more of antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 164, antioxidant DNP, antioxidant DLTP, antioxidant TNP, antioxidant TPP, antioxidant MB, and antioxidant 264.

[0011] The second object of the present invention is to provide a method for preparing the above-mentioned butyl rubber hot melt adhesive with good high temperature resistance, comprising the following steps:

[0012] S1: Cut butyl rubber, EPDM rubber and natural rubber into blocks with a particle size ranging from 5 cm×2 cm×2 cm to 10 cm×4 cm×4 cm respectively;

[0013] S2: according to the above weight components, the butyl rubber, EPDM rubber, natural rubber, antioxidant and plasticizer cut in step S1 are put into a kneader, heated to 130±10°C, and kneaded at a constant temperature for more than 30 minutes;

[0014] S3: According to the above weight components, polyisobutylene, filler, terpene resin, brominated triazine, antimony trioxide and polyamide wax are added into the above kneading machine, and heated to 130±10°C, kneaded at a constant temperature for more than 30 minutes, and discharged to obtain butyl rubber hot melt adhesive.

[0015] The third purpose of the present invention is to propose an application of the above-mentioned butyl rubber hot melt adhesive with good high temperature resistance, wherein the butyl rubber hot melt adhesive, the substrate layer and the release paper are compositely extruded and formed into a composite film by an extruder, and the butyl rubber hot melt adhesive forms an adhesive layer, wherein the substrate layer and the release paper are respectively located on both sides of the adhesive layer, and then the composite film is die-cut into patches of a certain shape and size by a composite die-cutting machine.

[0016] A preferred technical solution is that the substrate layer is glass fiber cloth or aluminum foil.

[0017] Another preferred technical solution is that the adhesive layer has a thickness of 1.2 to 2 mm.

[0018] (1) The butyl rubber hot melt adhesive with good high temperature resistance of the present invention has excellent air tightness, heat aging resistance and weather aging resistance. The thermodynamic stability and high temperature resistance of the butyl rubber hot melt adhesive are greatly improved by blending and modifying butyl rubber (IIR), ethylene propylene diene monomer rubber (EPDM) and natural rubber (NR). Natural rubber (NR) has high mechanical strength and good comprehensive mechanical properties. The main reason is that it has rubber reinforcement properties. When stretched, the macromolecular chains will be oriented along the stress direction to form crystals, and the amorphous macromolecules in the grains play a reinforcing role. The reason why the strength is also high without expansion is due to the tight agglomeration of tiny particles in its internal structure. EPDM has strong high temperature resistance because its main chain is composed of chemically stable saturated hydrocarbons and only contains unsaturated double bonds in the side chains. Therefore, it has excellent aging resistance such as ozone resistance, high temperature resistance, and weather resistance. Butyl rubber (IIR) / ethylene propylene diene monomer (EPDM) / natural rubber (NR) ternary blending, EPDM and natural rubber as dispersed phase, dispersed in the butyl rubber matrix, has the effect of inducing silver streaks and shear bands: EPDM and natural rubber dispersed in the butyl rubber matrix, induce a large number of silver streaks, and inducing a large number of silver streaks requires a lot of energy (including heat energy). Therefore, the butyl rubber (IIR) / ethylene propylene diene monomer (EPDM) / natural rubber (NR) ternary blending greatly improves the thermodynamic stability and high temperature resistance of butyl rubber. And EPDM and natural rubber dispersed in the butyl rubber matrix, another role is to induce the formation of shear bands, which can make the matrix shear yield and absorb a lot of deformation work. Shear bands not only consume a lot of energy (including heat energy), but also terminate silver streaks so that they do not develop into destructive cracks. Therefore, the formation of shear bands can not only improve the thermodynamic stability and high temperature resistance of butyl rubber, but also improve its mechanical properties.

[0019] (2) A butyl rubber hot melt adhesive with good high temperature resistance of the present invention is flame-retardantly modified by adding bromotriazine and antimony trioxide. Bromotriazine has a low bond energy of C-Br bond and its decomposition temperature is 310°C, which matches the decomposition problem of polymers such as butyl rubber, EPDM rubber, natural rubber, and terpene resin. Bromotriazine can delay or prevent the thermal decomposition of polymers to produce combustible gas. At the decomposition temperature, C-Br bond will generate bromine free radicals, which can capture free radicals that promote the growth of the combustion reaction chain or capture free radicals that maintain the chain reaction, thereby preventing the polymer from continuing to burn. Antimony trioxide and bromotriazine will generate antimony tribromide at high temperature. Antimony trihalide can promote the carbonization reaction of the condensed phase. The carbon layer can cover the surface of the substrate. The activated carbon forms an insulating layer to prevent heat transfer and reduce the generation and escape of gaseous combustible substances into the flame zone, thereby reducing the intensity of combustion.

[0020] (3) The butyl rubber hot melt adhesive with good high temperature resistance of the present invention has polyamide wax with thixotropy. In the process of preparing the butyl rubber hot melt adhesive, the polyamide wax swells to form a paste-like thixotropic agent, and its swollen structure is in a network shape, has very good strength and heat resistance, and has good storage stability. The polyamide wax is effectively activated at high temperature, and forms a strong network structure in the butyl rubber hot melt adhesive system. Its excellent thixotropic property has excellent anti-sagging ability and anti-settling ability, so that the butyl rubber hot melt adhesive has excellent anti-sagging ability in a high temperature environment.

[0021] The advantages and beneficial effects of the present invention are:

[0022] 1. The butyl rubber hot melt adhesive with good high temperature resistance of the present invention is modified by blending butyl rubber, EPDM rubber and natural rubber, so that the thermodynamic stability and high temperature resistance of the butyl rubber hot melt adhesive are greatly improved; the flame retardant performance of the butyl rubber hot melt adhesive is greatly improved by adding bromotriazine and antimony trioxide; the polyamide wax is effectively activated at high temperature, and forms a strong network structure in the butyl rubber hot melt adhesive system, and its excellent thixotropic property makes the butyl rubber hot melt adhesive have excellent anti-sagging ability and anti-settling ability.

[0023] 2. The preparation method of a butyl rubber hot melt adhesive with good high temperature resistance of the present invention has simple operation steps and high implementation feasibility. The production process does not require additional equipment, and is convenient for direct production in the existing high temperature resistant flame retardant plugging patch production line.

[0024] 3. The patch prepared with the butyl rubber hot melt adhesive having good high temperature resistance of the present invention has excellent thermodynamic stability, high temperature resistance, flame retardant properties, and does not flow under high temperature environment, thereby ensuring the firmness of the patch's application and sealing during use. DETAILED DESCRIPTION

[0025] The specific implementation of the present invention is further described below in conjunction with the examples. The following examples are only used to more clearly illustrate the technical solutions of the present invention, and cannot be used to limit the protection scope of the present invention.

[0026] Example 1

[0027] A butyl rubber hot melt adhesive with good high temperature resistance comprises the following components by weight: 10 parts of butyl rubber, 1 part of EPDM rubber, 2 parts of natural rubber, 11 parts of polyisobutylene, 10 parts of plasticizer, 32 parts of filler, 6 parts of terpene resin, 10 parts of brominated triazine, 4 parts of antimony trioxide, 1 part of polyamide wax and 0.5 parts of antioxidant.

[0028] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 600 CS, the plasticizer is paraffin oil, the filler is calcium carbonate, and the antioxidant model is antioxidant 1010.

[0029] The preparation method of the butyl rubber hot melt adhesive with good high temperature resistance comprises the following steps:

[0030] S1: Cut butyl rubber, EPDM rubber and natural rubber into blocks with a particle size ranging from 5 cm×2 cm×2 cm to 10 cm×4 cm×4 cm respectively;

[0031] S2: according to the above weight components, the butyl rubber, EPDM rubber, natural rubber, antioxidant and plasticizer cut in step S1 are put into a kneader, heated to 130±10°C, and kneaded at a constant temperature for more than 30 minutes;

[0032] S3: According to the above weight components, polyisobutylene, filler, terpene resin, brominated triazine, antimony trioxide and polyamide wax are added into the above kneading machine, and heated to 130±10°C, kneaded at a constant temperature for more than 30 minutes, and discharged to obtain butyl rubber hot melt adhesive.

[0033] Example 2

[0034] A butyl rubber hot melt adhesive with good high temperature resistance comprises the following components by weight: 14 parts of butyl rubber, 2 parts of EPDM rubber, 3 parts of natural rubber, 14 parts of polyisobutylene, 12 parts of plasticizer, 40 parts of filler, 8 parts of terpene resin, 13 parts of brominated triazine, 5 parts of antimony trioxide, 2 parts of polyamide wax and 1 part of antioxidant.

[0035] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 800 CS, the plasticizer is dioctyl phthalate, the filler is barium sulfate, and the antioxidant model is antioxidant TNP.

[0036] The preparation method of the above-mentioned butyl rubber hot melt adhesive with good high temperature resistance is the same as that in Example 1.

[0037] Example 3

[0038] A butyl rubber hot melt adhesive with good high temperature resistance comprises the following components by weight: 18 parts of butyl rubber, 3 parts of EPDM rubber, 4 parts of natural rubber, 17 parts of polyisobutylene, 15 parts of plasticizer, 50 parts of filler, 9 parts of terpene resin, 15 parts of brominated triazine, 7 parts of antimony trioxide, 3 parts of polyamide wax and 1.5 parts of antioxidant.

[0039] Preferably, the viscosity of the polyisobutylene measured at 100°C is 1000CS; the plasticizer is paraffin oil, dioctyl phthalate, and diisodecyl phthalate, and the weight ratio of the three is 1:1:1; the filler is barium sulfate and silicon powder, and the weight ratio of the two is 1:1; the antioxidant is antioxidant TPP, antioxidant MB, and antioxidant 264, and the weight ratio of the three is 1:1:1.

[0040] The preparation method of the above-mentioned butyl rubber hot melt adhesive with good high temperature resistance is the same as that in Example 1.

[0041] Comparative Example 1

[0042] A butyl rubber hot melt adhesive comprises the following components by weight: 10 parts of butyl rubber, 11 parts of polyisobutylene, 10 parts of plasticizer, 32 parts of filler, 6 parts of terpene resin, 10 parts of brominated triazine, 4 parts of antimony trioxide, 1 part of polyamide wax and 0.5 parts of antioxidant.

[0043] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 600 CS, the plasticizer is paraffin oil, the filler is calcium carbonate, and the antioxidant model is antioxidant 1010.

[0044] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0045] Comparative Example 2

[0046] A butyl rubber hot melt adhesive comprises the following components by weight: 10 parts of butyl rubber, 1 part of EPDM rubber, 2 parts of natural rubber, 11 parts of polyisobutylene, 10 parts of plasticizer, 32 parts of filler, 6 parts of terpene resin, 1 part of polyamide wax and 0.5 parts of antioxidant.

[0047] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 600 CS, the plasticizer is paraffin oil, the filler is calcium carbonate, and the antioxidant model is antioxidant 1010.

[0048] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0049] Comparative Example 3

[0050] A butyl rubber hot melt adhesive comprises the following components by weight: 10 parts of butyl rubber, 1 part of EPDM rubber, 2 parts of natural rubber, 11 parts of polyisobutylene, 10 parts of plasticizer, 32 parts of filler, 6 parts of terpene resin, 10 parts of bromotriazine, 4 parts of antimony trioxide and 0.5 parts of antioxidant.

[0051] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 600 CS, the plasticizer is paraffin oil, the filler is calcium carbonate, and the antioxidant model is antioxidant 1010.

[0052] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0053] Comparative Example 4

[0054] A butyl rubber hot melt adhesive comprises the following components by weight: 14 parts of butyl rubber, 14 parts of polyisobutylene, 12 parts of plasticizer, 40 parts of filler, 8 parts of terpene resin, 13 parts of bromotriazine, 5 parts of antimony trioxide, 2 parts of polyamide wax and 1 part of antioxidant.

[0055] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 800 CS, the plasticizer is dioctyl phthalate, the filler is barium sulfate, and the antioxidant model is antioxidant TNP.

[0056] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0057] Comparative Example 5

[0058] A butyl rubber hot melt adhesive comprises the following components by weight: 14 parts of butyl rubber, 2 parts of EPDM rubber, 3 parts of natural rubber, 14 parts of polyisobutylene, 12 parts of plasticizer, 40 parts of filler, 8 parts of terpene resin, 2 parts of polyamide wax and 1 part of antioxidant.

[0059] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 800 CS, the plasticizer is dioctyl phthalate, the filler is barium sulfate, and the antioxidant model is antioxidant TNP.

[0060] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0061] Comparative Example 6

[0062] A butyl rubber hot melt adhesive comprises the following components by weight: 14 parts of butyl rubber, 2 parts of EPDM rubber, 3 parts of natural rubber, 14 parts of polyisobutylene, 12 parts of plasticizer, 40 parts of filler, 8 parts of terpene resin, 13 parts of bromotriazine, 5 parts of antimony trioxide and 1 part of antioxidant.

[0063] Preferably, the viscosity of the polyisobutylene measured at 100° C. is 800 CS, the plasticizer is dioctyl phthalate, the filler is barium sulfate, and the antioxidant model is antioxidant TNP.

[0064] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0065] Comparative Example 7

[0066] A butyl rubber hot melt adhesive comprises the following components by weight: 18 parts of butyl rubber, 17 parts of polyisobutylene, 15 parts of plasticizer, 50 parts of filler, 9 parts of terpene resin, 15 parts of brominated triazine, 7 parts of antimony trioxide, 3 parts of polyamide wax and 1.5 parts of antioxidant.

[0067] Preferably, the viscosity of the polyisobutylene measured at 100°C is 1000CS; the plasticizer is paraffin oil, dioctyl phthalate, and diisodecyl phthalate, and the weight ratio of the three is 1:1:1; the filler is barium sulfate and silicon powder, and the weight ratio of the two is 1:1; the antioxidant is antioxidant TPP, antioxidant MB, and antioxidant 264, and the weight ratio of the three is 1:1:1.

[0068] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0069] Comparative Example 8

[0070] A butyl rubber hot melt adhesive comprises the following components by weight: 18 parts of butyl rubber, 3 parts of EPDM rubber, 4 parts of natural rubber, 17 parts of polyisobutylene, 15 parts of plasticizer, 50 parts of filler, 9 parts of terpene resin, 3 parts of polyamide wax and 1.5 parts of antioxidant.

[0071] Preferably, the viscosity of the polyisobutylene measured at 100°C is 1000CS; the plasticizer is paraffin oil, dioctyl phthalate, and diisodecyl phthalate, and the weight ratio of the three is 1:1:1; the filler is barium sulfate and silicon powder, and the weight ratio of the two is 1:1; the antioxidant is antioxidant TPP, antioxidant MB, and antioxidant 264, and the weight ratio of the three is 1:1:1.

[0072] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0073] Comparative Example 9

[0074] A butyl rubber hot melt adhesive comprises the following components by weight: 18 parts of butyl rubber, 3 parts of EPDM rubber, 4 parts of natural rubber, 17 parts of polyisobutylene, 15 parts of plasticizer, 50 parts of filler, 9 parts of terpene resin, 15 parts of bromotriazine, 7 parts of antimony trioxide and 1.5 parts of antioxidant.

[0075] Preferably, the viscosity of the polyisobutylene measured at 100°C is 1000CS; the plasticizer is paraffin oil, dioctyl phthalate, and diisodecyl phthalate, and the weight ratio of the three is 1:1:1; the filler is barium sulfate and silicon powder, and the weight ratio of the two is 1:1; the antioxidant is antioxidant TPP, antioxidant MB, and antioxidant 264, and the weight ratio of the three is 1:1:1.

[0076] The preparation method of the above butyl rubber hot melt adhesive is the same as that in Example 1.

[0077] The butyl rubber hot melt adhesive with good high temperature resistance prepared in Examples 1 to 3 and the butyl rubber hot melt adhesive prepared in Comparative Examples 1 to 9 were respectively extruded with a substrate layer and a release paper to form a composite film by an extruder, and the butyl rubber hot melt adhesive correspondingly formed an adhesive layer with a thickness of 2 mm, wherein the substrate layer and the release paper were respectively located on both sides of the adhesive layer, and then the composite film was die-cut into patches of a certain shape and size by a composite die-cutting machine, and the patches were respectively tested for initial adhesion, heat aging adhesion, flame retardancy, and high-temperature flowability.

[0078] (I) Initial adhesion test

[0079] Sample preparation: Tear off the release paper from a patch of size 200 mm × 20 mm and stick it on a painted board. Use a 4 kg roller to roll 5 times at a speed of 10 m / min and place it at 23 ± 2 ° C and 50 ± 5% RH for 1 hour.

[0080] Fix one end of the paint plate on the upper fixture and one end of the patch on the lower fixture, and perform a 180° peel force test; control the peeling speed of the upper fixture to 300mm / min, remove the initial 25mm length, and take 100mm length as the effective peeling length: each patch sample is tested 3 times in parallel, and the average value is taken. The experimental results are expressed in N / cm.

[0081] (II) Thermal aging adhesion test

[0082] The patch was aged for 1000 h in an environmental chamber at a temperature of 100°C ± 3°C, and then the patch sample was taken out of the environmental chamber and placed at room temperature for 24 h, and a peel strength test was performed according to the above-mentioned (I) initial adhesion test method.

[0083] (III) High temperature flow test

[0084] Take a patch with a size of 100mm×100mm, tear off the release paper from the patch and stick it on a test board of 150mm×150mm, leaving at least 30mm of flow distance at the bottom of the test board. Place the test board vertically in an oven at a baking temperature of 180℃, take it out after baking for 30 minutes, cool it to the test standard conditions and measure it. Measure the position difference of the long end of the patch on the test board before and after baking, and the data is accurate to 0.1mm.

[0085] (IV) Flame retardancy test

[0086] Sample preparation: Take a patch with a size of 60mm×356mm, place it in an environment with a temperature of 23±2℃ and a humidity of 40-50%RH for 24h, and then perform a flame retardancy test according to the method specified in GB 8410-2006 "Combustion Characteristics of Automobile Interior Materials".

[0087] Table 1 Performance test results of the patches corresponding to the butyl rubber hot melt adhesives with good high temperature resistance prepared in Examples 1 to 3 and the butyl rubber hot melt adhesives prepared in Comparative Examples 1 to 9

[0088]

[0089]

[0090] From Table 1 we can see that:

[0091] (1) Compared with the butyl rubber hot melt adhesive with good high temperature resistance in Example 1, the butyl rubber hot melt adhesive in Comparative Example 1 is not blended with EPDM rubber and natural rubber for modification, and its initial bonding strength and heat aging bonding strength are greatly reduced compared with the initial bonding strength and heat aging bonding strength of the butyl rubber hot melt adhesive with good high temperature resistance in Example 1; similarly, the initial bonding strength and heat aging bonding strength of the butyl rubber hot melt adhesive prepared in Comparative Example 4 are greatly reduced compared with the initial bonding strength and heat aging bonding strength of the butyl rubber hot melt adhesive with good high temperature resistance in Example 2; the initial bonding strength and heat aging bonding strength of the butyl rubber hot melt adhesive prepared in Comparative Example 7 are greatly reduced compared with the initial bonding strength and heat aging bonding strength of the butyl rubber hot melt adhesive with good high temperature resistance in Example 3.

[0092] (2) Compared with the butyl rubber hot melt adhesive with good high temperature resistance in Example 1, the butyl rubber hot melt adhesive in Comparative Example 2 does not contain bromotriazine and antimony trioxide, and its flame retardant performance is greatly reduced compared with the flame retardant performance of the butyl rubber hot melt adhesive with good high temperature resistance in Example 1; similarly, the flame retardant performance of the butyl rubber hot melt adhesive prepared in Comparative Example 5 is greatly reduced compared with the flame retardant performance of the butyl rubber hot melt adhesive with good high temperature resistance in Example 2; the flame retardant performance of the butyl rubber hot melt adhesive prepared in Comparative Example 8 is greatly reduced compared with the flame retardant performance of the butyl rubber hot melt adhesive with good high temperature resistance in Example 3.

[0093] (3) The butyl rubber hot melt adhesives with good high temperature resistance in Examples 1 to 3 flow slightly or do not flow at high temperatures; the butyl rubber hot melt adhesive in Comparative Example 3 does not have polyamide wax added compared to the butyl rubber hot melt adhesive with good high temperature resistance in Example 1, and compared with the butyl rubber hot melt adhesive with good high temperature resistance in Example 1, the butyl rubber hot melt adhesive in Comparative Example 3 will flow at high temperatures; similarly, compared with the butyl rubber hot melt adhesive with good high temperature resistance in Example 2, the butyl rubber hot melt adhesive in Comparative Example 6 will flow at high temperatures; compared with the butyl rubber hot melt adhesive with good high temperature resistance in Example 3, the butyl rubber hot melt adhesive in Comparative Example 9 will flow at high temperatures.

[0094] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A butyl rubber hot melt adhesive with good high temperature resistance, characterized in that: It consists of the following components by weight: Butyl rubber 10-18 parts, EPDM rubber 1-3 parts, natural rubber 2-4 parts, polyisobutylene 11-17 parts, Plasticizer 10-15 parts, filler 32-50 parts, terpene resin 6-9 parts, bromotriazine 10-15 parts, trioxide 4-7 parts of antimony, 1-3 parts of polyamide wax, 0.5-1.5 parts of antioxidant; the polyisobutylene is heated at 100°C. The viscosity measured is 600-100CS.

2. The butyl rubber hot melt adhesive with good high temperature resistance as claimed in claim 1, characterized in that: The plasticizer is one or more of paraffin oil, dioctyl phthalate and diisodecyl phthalate.

3. The butyl rubber hot melt adhesive with good high temperature resistance as claimed in claim 1, characterized in that: The filler is one or more of calcium carbonate, barium sulfate and silicon powder.

4. The butyl rubber hot melt adhesive with good high temperature resistance as claimed in claim 1, characterized in that: The antioxidant model is one or more of antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 164, antioxidant DNP, antioxidant DLTP, antioxidant TNP, antioxidant TPP, antioxidant MB, and antioxidant 264.

5. The method for preparing a butyl rubber hot melt adhesive with good high temperature resistance according to any one of claims 1 to 4, characterized in that: The steps are as follows: S1: Cut butyl rubber, EPDM rubber and natural rubber into blocks with a particle size ranging from 5 cm×2 cm×2 cm to 10 cm×4 cm×4 cm respectively; S2: according to the weight composition of claim 1, the butyl rubber, EPDM rubber, natural rubber, antioxidant and plasticizer cut in step S1 are put into a kneader, heated to 130±10°C, and kneaded at a constant temperature for more than 30 minutes; S3: According to the weight components described in claim 1, polyisobutylene, filler, terpene resin, brominated triazine, antimony trioxide and polyamide wax are added into the above kneading machine, heated to 130±10°C, kneaded at a constant temperature for more than 30 minutes, and discharged to obtain butyl rubber hot melt adhesive.

6. The use of the butyl rubber hot melt adhesive with good high temperature resistance as claimed in any one of claims 1 to 4, characterized in that: The butyl rubber hot melt adhesive, the substrate layer and the release paper are compositely extruded into a composite film by an extruder, wherein the butyl rubber hot melt adhesive forms an adhesive layer, wherein the substrate layer and the release paper are respectively located on both sides of the adhesive layer, and then the composite film is die-cut into patches of a certain shape and size by a composite die-cutting machine.

7. The use of the butyl rubber hot melt adhesive with good high temperature resistance as claimed in claim 6, characterized in that: The substrate layer is glass fiber cloth or aluminum foil.

8. The use of the butyl rubber hot melt adhesive with good high temperature resistance as claimed in claim 6, characterized in that: The thickness of the adhesive layer is 1.2-2 mm.

Citation Information

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