High-temperature-resistant hot-melt pressure-sensitive adhesive as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of pressure-sensitive adhesives, and particularly relates to a high-temperature-resistant hot-melt pressure-sensitive adhesive as well as a preparation method and application thereof. The high-temperature-resistant hot-melt pressure-sensitive adhesive is prepared from the following components in parts by weight: 20 to 30 parts of thermoplastic elastomer, 1 to 10 parts of polyvinyl butyral, 10 to 20 parts of terpene resin, 8 to 18 parts of tackifying resin, 10 to 20 parts of plasticizer, 0.1 to 2 parts of antioxidant and 0.1 to 2 parts of light stabilizer. The prepared hot-melt pressure-sensitive adhesive has excellent heat resistance and low-temperature flexibility, and can be used for preparing high-molecular waterproof coiled materials.

Description

Technical Field

[0001] The present invention belongs to the technical field of pressure-sensitive adhesives, and in particular relates to a high-temperature resistant hot-melt pressure-sensitive adhesive and a preparation method and application thereof. Background Art

[0002] Polymer waterproofing membranes are commonly used in building waterproofing projects. Made from synthetic polymers, they exhibit excellent flexibility, weather resistance, tensile strength, and elongation. These membranes are widely used in various applications requiring waterproofing, such as roofs, basements, tunnels, and bridges.

[0003] Hot-melt pressure-sensitive adhesive (HMPSA) is an adhesive that flows upon heating and quickly forms a bond upon cooling. It combines the fast-curing properties of pressure-sensitive adhesives with the ease of handling. This type of adhesive is more environmentally friendly during application and provides immediate initial bond strength. Using HMPSA as the adhesive layer of polymer waterproofing membranes not only improves the overall performance of the membrane but also simplifies the construction process, making waterproofing projects more efficient and reliable.

[0004] Pre-laid waterproofing membranes play a crucial role in building waterproofing projects. To adapt to diverse environmental conditions, these membranes often need to possess both heat resistance and low-temperature flexibility to ensure the integrity and functionality of the waterproofing layer. Buildings can experience high temperatures in the summer, particularly in some regions where rooftops or exposed surfaces can reach extremely high temperatures. Heat-resistant waterproofing membranes can maintain their physical properties, such as shape stability and bond strength, under these conditions, preventing problems such as flow or deformation caused by softening at high temperatures. In winter or in cold regions, temperatures can drop to very low levels. Low-temperature-flexible waterproofing membranes maintain sufficient flexibility and ductility at low temperatures to prevent brittle cracking caused by temperature drops, which is crucial for ensuring the continuity and integrity of the waterproofing layer.

[0005] Therefore, when selecting waterproof membranes, it is very important to consider the balance between heat resistance and low-temperature flexibility. However, the adhesive layer of waterproof membranes in the prior art is difficult to achieve both heat resistance and low-temperature flexibility, often resulting in a loss of one while focusing on the other.

[0006] Chinese patent publication number CN 114806448 B discloses a hot-melt pressure-sensitive adhesive for polymer waterproofing membrane and a preparation method thereof. The pressure-sensitive adhesive prepared by the method has good heat resistance, but its low-temperature flexibility is not ideal.

[0007] Therefore, there is an urgent need for a hot melt pressure sensitive adhesive that is both heat resistant and low temperature flexible. Summary of the Invention

[0008] The purpose of the present invention is to provide a high-temperature resistant hot-melt pressure-sensitive adhesive and a preparation method and application thereof.

[0009] In order to achieve the above object, the present invention provides the following technical solutions:

[0010] The first aspect of the present invention provides a high-temperature resistant hot-melt pressure-sensitive adhesive, comprising the following components in parts by weight: 20-30 parts of a thermoplastic elastomer, 1-10 parts of polyvinyl butyral, 10-20 parts of a terpene resin, 8-18 parts of a tackifying resin, 10-20 parts of a plasticizer, 0.1-2 parts of an antioxidant, and 0.1-2 parts of a light stabilizer.

[0011] Preferably, the composition comprises the following components in parts by weight: 21-25 parts of thermoplastic elastomer, 5-9 parts of polyvinyl butyral, 10-14 parts of terpene resin, 8-14 parts of tackifying resin, 15-19 parts of plasticizer, 0.5-1.5 parts of antioxidant, and 1-2 parts of light stabilizer.

[0012] The present invention improves the peel strength of the hot melt pressure-sensitive adhesive by compounding a specific proportion of thermoplastic elastomer, polyvinyl butyral, and terpene resin, provides strong bonding force, ensures a firm connection between the waterproof membrane and the base surface, effectively prevents moisture penetration, and reduces the occurrence of water leakage.

[0013] Preferably, the thermoplastic elastomer is thermoplastic styrene-butadiene rubber.

[0014] Preferably, the melt index of the thermoplastic styrene-butadiene rubber is 8-24 g / 10 min at 200° C. and 5 kg.

[0015] More preferably, the melt index of the thermoplastic styrene butadiene rubber is 12 g / 10 min at 200° C. and 5 kg. The thermoplastic styrene butadiene rubber can be commercially available or homemade. The commercially available one can be Kraton polymer ( POLYMERS) model D1161P thermoplastic styrene butadiene rubber.

[0016] Preferably, the viscosity of polyvinyl butyral at 20° C. is 14-20 mPa·s, and the content of polyvinyl alcohol is 18-21 wt %. Polyvinyl butyral can be commercially available or homemade. Commercially available products can be obtained from Kuraray International Trading (Shanghai) Co., Ltd., Model B 16H.

[0017] Preferably, the softening point of the terpene resin is 95° C. The terpene resin can be commercially available or homemade, and commercially available products include Terpene Resin TM Series, TM90, from Guangdong Nuochi New Materials Co., Ltd.

[0018] Preferably, the tackifying resin is selected from at least one of C5 petroleum resin, C5 hydrogenated petroleum resin, and rosin resin.

[0019] Preferably, the tackifying resin is C5 hydrogenated petroleum resin.

[0020] Preferably, the plasticizer comprises naphthenic oil, chlorinated paraffin and di(2-ethylhexyl) phthalate in a weight ratio of 1:(1.3-1.5):(0.4-0.7).

[0021] The present invention improves the heat resistance of the hot-melt pressure-sensitive adhesive by adding a plasticizer in a specific ratio. In high-temperature environments, such as in summer or near heat sources (e.g., boiler rooms and around steam pipes), the heat-resistant hot-melt pressure-sensitive adhesive will not soften or flow, thereby maintaining its shape and adhesion, preventing the waterproof layer from failing due to temperature increases.

[0022] Preferably, the plasticizer accounts for 40-45% of the total weight of the thermoplastic elastomer, polyvinyl butyral and terpene resin.

[0023] The present invention improves the low-temperature flexibility of a hot-melt pressure-sensitive adhesive by adjusting the percentage of plasticizer in the total weight of the thermoplastic elastomer, polyvinyl butyral, and terpene resin. In cold weather or low-temperature environments, waterproofing membranes must withstand certain deformations without cracking. A hot-melt pressure-sensitive adhesive with excellent low-temperature flexibility remains pliable even in these conditions, allowing the membrane to contract or expand with the substrate without compromising its integrity, ensuring uncompromising waterproofing effectiveness.

[0024] Preferably, the composition comprises the following components in parts by weight: 23 parts of thermoplastic elastomer, 6 parts of polyvinyl butyral, 12 parts of terpene resin, 10 parts of tackifying resin, 17 parts of plasticizer, 1 part of antioxidant, and 1.5 parts of light stabilizer.

[0025] Preferably, the antioxidant is selected from at least one of antioxidant 1010, antioxidant 1076, and antioxidant 1726.

[0026] Preferably, the light stabilizer is a hindered amine light stabilizer.

[0027] Preferably, the hindered amine light stabilizer is bis(1,2,2,6,6-pentamethyl-4-piperidinyl) sebacate.

[0028] The second aspect of the present invention provides a method for preparing a high-temperature resistant hot-melt pressure-sensitive adhesive, comprising the following steps: mixing a thermoplastic elastomer, polyvinyl butyral, a terpene resin, a tackifying resin, a plasticizer, an antioxidant and a light stabilizer, heating to 180-200°C, evacuating to -0.02MPa, and stirring until uniform to obtain a high-temperature resistant hot-melt pressure-sensitive adhesive.

[0029] The third aspect of the present invention provides the use of a high temperature resistant hot melt pressure sensitive adhesive in the preparation of a polymer waterproof membrane.

[0030] Compared with the prior art, the advantages and beneficial effects of the present invention are:

[0031] 1. The present invention improves the peel strength of the hot melt pressure-sensitive adhesive by compounding thermoplastic elastomer, polyvinyl butyral and terpene resin in a specific proportion, provides strong bonding force, ensures a firm connection between the waterproof membrane and the base surface, effectively prevents moisture penetration and reduces the occurrence of water leakage.

[0032] 2. By adding a plasticizer in a specific ratio, the present invention improves the heat resistance of the hot-melt pressure-sensitive adhesive. In high-temperature environments, such as in summer or near heat sources (e.g., boiler rooms and around steam pipes), the heat-resistant hot-melt pressure-sensitive adhesive will not soften or flow, thereby maintaining its shape and adhesion, preventing the waterproof layer from failing due to temperature increases.

[0033] 3. The present invention improves the low-temperature flexibility of the hot-melt pressure-sensitive adhesive by adjusting the percentage of plasticizer in the total weight of the thermoplastic elastomer, polyvinyl butyral, and terpene resin. In cold weather or low-temperature environments, waterproofing membranes must withstand certain deformations without cracking. A hot-melt pressure-sensitive adhesive with excellent low-temperature flexibility remains pliable under these conditions, allowing the membrane to contract or expand with the substrate without compromising its integrity, ensuring uncompromising waterproofing effectiveness.

[0034] In summary, the hot-melt pressure-sensitive adhesive of the present invention simultaneously exhibits excellent peel strength, heat resistance, and low-temperature flexibility. This novel hot-melt pressure-sensitive adhesive possesses multiple superior properties, making it suitable not only for traditional building waterproofing projects but also for use in more demanding environments, such as those in extreme climates and industrial facilities, where higher demands are placed on waterproof materials. This further broadens the application areas of polymer waterproof membranes. In complex and diverse practical application scenarios, whether facing sudden temperature changes or long-term exposure to harsh environments, the hot-melt pressure-sensitive adhesive of the present invention can maintain stable performance, thereby enhancing the reliability and durability of the entire waterproofing system and extending the service life of the waterproofing project.

[0035] In summary, this hot-melt pressure-sensitive adhesive, which has peel strength, heat resistance and low-temperature flexibility, greatly improves the quality and applicability of polymer waterproof membranes, provides a new solution to the problems existing in traditional waterproof materials, and helps promote the development and progress of waterproof technology. DETAILED DESCRIPTION

[0036] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0037] The raw materials used in the following examples of the present invention are all commercially available commodities:

[0038] The melt index of thermoplastic styrene butadiene rubber is 12g / 10min at 200℃ and 5kg. POLYMERS) model D1161P.

[0039] The viscosity of polyvinyl butyral at 20°C is 14-20 mPa·s, and the content of polyvinyl alcohol is 18-21 wt%. Kuraray International Trading (Shanghai) Co., Ltd., Model B 16H.

[0040] The softening point of terpene resin is 95°C. Guangdong Nuochi New Materials Co., Ltd., Terpene Resin TM Series, TM90.

[0041] The tackifying resin is C5 hydrogenated petroleum resin, Puyang Hengtai Petrochemical Co., Ltd., H5-1100.

[0042] Bis(1,2,2,6,6-pentamethyl-4-piperidinyl)sebacate, Cas:41556-26-7.

[0043] Antioxidant 1010, Shanghai Better Chemical Co., Ltd.

[0044] Example 1

[0045] This embodiment provides a high-temperature resistant hot-melt pressure-sensitive adhesive, comprising the following components in parts by weight: 23 parts of thermoplastic elastomer, 6 parts of polyvinyl butyral, 12 parts of terpene resin, 10 parts of tackifying resin, 17 parts of plasticizer, 1 part of antioxidant, and 1.5 parts of light stabilizer.

[0046] The plasticizer includes naphthenic oil, chlorinated paraffin and di(2-ethylhexyl) phthalate in a weight ratio of 1:1.4:0.6. The antioxidant is antioxidant 1010. The light stabilizer is bis(1,2,2,6,6-pentamethyl-4-piperidinyl) sebacate.

[0047] The preparation method of the high-temperature resistant hot-melt pressure-sensitive adhesive comprises the following steps: mixing a thermoplastic elastomer, polyvinyl butyral, a terpene resin, a tackifying resin, a plasticizer, an antioxidant and a light stabilizer, heating to 190° C., evacuating to -0.02 MPa, and stirring until uniform to obtain the high-temperature resistant hot-melt pressure-sensitive adhesive.

[0048] Example 2

[0049] This embodiment provides a high-temperature resistant hot-melt pressure-sensitive adhesive, comprising the following components in parts by weight: 21 parts of thermoplastic elastomer, 9 parts of polyvinyl butyral, 10 parts of terpene resin, 8 parts of tackifying resin, 16 parts of plasticizer, 1.5 parts of antioxidant, and 1 part of light stabilizer.

[0050] The plasticizer includes naphthenic oil, chlorinated paraffin, and di(2-ethylhexyl) phthalate in a weight ratio of 1:1.3:0.7. The antioxidants include antioxidant 1010, antioxidant 1076, and antioxidant 1726. The light stabilizer is bis(1,2,2,6,6-pentamethyl-4-piperidinyl) sebacate.

[0051] The preparation method of the high-temperature resistant hot-melt pressure-sensitive adhesive comprises the following steps: mixing a thermoplastic elastomer, polyvinyl butyral, a terpene resin, a tackifying resin, a plasticizer, an antioxidant and a light stabilizer, heating to 200° C., evacuating to -0.02 MPa, and stirring until uniform to obtain the high-temperature resistant hot-melt pressure-sensitive adhesive.

[0052] Example 3

[0053] This embodiment provides a high-temperature resistant hot-melt pressure-sensitive adhesive, comprising the following components in parts by weight: 25 parts of thermoplastic elastomer, 5 parts of polyvinyl butyral, 14 parts of terpene resin, 14 parts of tackifying resin, 19 parts of plasticizer, 0.5 parts of antioxidant, and 2 parts of light stabilizer.

[0054] The plasticizer includes naphthenic oil, chlorinated paraffin, and di(2-ethylhexyl) phthalate in a weight ratio of 1:1.5:0.4. The antioxidants include antioxidant 1010, antioxidant 1076, and antioxidant 1726. The light stabilizer is bis(1,2,2,6,6-pentamethyl-4-piperidinyl) sebacate.

[0055] The preparation method of the high-temperature resistant hot-melt pressure-sensitive adhesive comprises the following steps: mixing a thermoplastic elastomer, polyvinyl butyral, a terpene resin, a tackifying resin, a plasticizer, an antioxidant and a light stabilizer, heating to 180° C., evacuating to -0.02 MPa, and stirring until uniform to obtain the high-temperature resistant hot-melt pressure-sensitive adhesive.

[0056] Example 4

[0057] The difference between this embodiment and embodiment 1 is that the amount of plasticizer used is different. The details are as follows:

[0058] A high-temperature resistant hot-melt pressure-sensitive adhesive comprises the following components in parts by weight: 23 parts of a thermoplastic elastomer, 6 parts of polyvinyl butyral, 12 parts of a terpene resin, 10 parts of a tackifying resin, 10 parts of a plasticizer, 1 part of an antioxidant, and 1.5 parts of a light stabilizer.

[0059] Example 5

[0060] The difference between this embodiment and embodiment 1 is that the amount of plasticizer used is different. The details are as follows:

[0061] A high-temperature resistant hot-melt pressure-sensitive adhesive comprises the following components in parts by weight: 23 parts of a thermoplastic elastomer, 6 parts of polyvinyl butyral, 12 parts of a terpene resin, 10 parts of a tackifying resin, 19 parts of a plasticizer, 1 part of an antioxidant, and 1.5 parts of a light stabilizer.

[0062] Comparative Example 1

[0063] The difference between this comparative example and Example 1 is that the total weight of the thermoplastic elastomer, polyvinyl butyral, and terpene resin remains unchanged, but the proportions are changed. The details are as follows:

[0064] A high-temperature resistant hot-melt pressure-sensitive adhesive comprises the following components in parts by weight: 18 parts of a thermoplastic elastomer, 17 parts of polyvinyl butyral, 6 parts of a terpene resin, 10 parts of a tackifying resin, 17 parts of a plasticizer, 1 part of an antioxidant, and 1.5 parts of a light stabilizer.

[0065] Comparative Example 2

[0066] The difference between this comparative example and Example 1 is that the plasticizer comprises naphthenic oil, chlorinated paraffin and di(2-ethylhexyl) phthalate in a weight ratio of 0.3:1:1.7.

[0067] Comparative Example 3

[0068] The difference between this comparative example and Example 1 is that the plasticizer comprises naphthenic oil and chlorinated paraffin in a weight ratio of 3:1.

[0069] Comparative Example 4

[0070] The difference between this comparative example and Example 1 is that the plasticizer is di(2-ethylhexyl) phthalate.

[0071] Comparative Example 5

[0072] The difference between this comparative example and Example 1 is that the melt index of the thermoplastic styrene-butadiene rubber is 3 g / 10 min at 200° C. and 5 kg. POLYMERS), model D1111K.

[0073] Comparative Example 6

[0074] The difference between this comparative example and Example 1 is that the terpene resin has a softening point of 115° C. Guangdong Nuochi New Materials Co., Ltd., terpene resin TM series, TM115.

[0075] Comparative Example 7

[0076] The difference between this comparative example and Example 1 is that the viscosity of polyvinyl butyral at 20° C. is 9-13 mPa·s, and the content of polyvinyl alcohol is 14-18 wt %. Kuraray International Trading (Shanghai) Co., Ltd., model Mowital°B 14S.

[0077] Comparative Example 8

[0078] This comparative example is the hot melt pressure-sensitive adhesive of Example 1 in the Chinese patent publication number CN 114806448 B, "A hot melt pressure-sensitive adhesive for polymer waterproof membrane and its preparation method."

[0079] Performance Testing

[0080] The hot melt pressure-sensitive adhesives of Examples 1-5 and Comparative Examples 1-7 were applied to HDPE polymer sheets to obtain pre-laid waterproof membranes. The peel strength, heat resistance, and low-temperature flexibility after immersion in post-cast concrete were tested with reference to GB / T 23457-2017.

[0081] The results are shown in Table 1.

[0082] Table 1 Pre-laid waterproof membrane performance test results

[0083]

[0084]

[0085] As shown in Table 1, the hot-melt pressure-sensitive adhesives of Examples 1-5 exhibit excellent peel strength, and the hot-melt pressure-sensitive adhesives of Examples 1-3 exhibit both heat resistance and low-temperature flexibility, outperforming the prior art product of Comparative Example 8. The results indicate that, in Example 4, the heat resistance of the pressure-sensitive adhesive decreased due to a low level of plasticizer addition, while in Example 5, the low-temperature flexibility of the pressure-sensitive adhesive decreased due to a high level of plasticizer addition.

[0086] In Comparative Example 1, the ratio of the thermoplastic elastomer, polyvinyl butyral, and terpene resin was changed, and the peel strength of the hot melt pressure-sensitive adhesive decreased.

[0087] In Comparative Examples 2-4, the composition of the plasticizer was changed, and the heat resistance and low-temperature flexibility of the pressure-sensitive adhesive decreased to varying degrees.

[0088] In Comparative Example 5, the parameters of the thermoplastic elastomer were changed, the peel strength and the low-temperature flexibility were deteriorated.

[0089] In Comparative Example 6, the parameters of the terpene resin were changed, and the low-temperature flexibility of the hot-melt pressure-sensitive adhesive decreased.

[0090] In Comparative Example 7, the parameters of polyvinyl butyral changed, the peel strength decreased, and both the heat resistance and low-temperature flexibility decreased.

[0091] The hot-melt pressure-sensitive adhesive of the present invention exhibits excellent peel strength, heat resistance, and low-temperature flexibility. These multiple advantages make it suitable not only for traditional building waterproofing projects but also for use in more demanding environments, such as those in extreme climates and industrial facilities, where higher demands are placed on waterproof materials. This further broadens the application areas of polymer waterproof membranes. In complex and diverse practical application scenarios, whether facing sudden temperature fluctuations or long-term exposure to harsh environments, the hot-melt pressure-sensitive adhesive of the present invention maintains stable performance, thereby enhancing the reliability and durability of the entire waterproofing system and extending the service life of the waterproofing project.

[0092] In summary, this hot-melt pressure-sensitive adhesive, which has peel strength, heat resistance and low-temperature flexibility, greatly improves the quality and applicability of polymer waterproof membranes, provides a new solution to the problems existing in traditional waterproof materials, and helps promote the development and progress of waterproof technology.

[0093] The above is 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 principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A high temperature resistant hot melt pressure sensitive adhesive, characterized in that: The invention comprises the following components in parts by weight: 20-30 parts of thermoplastic elastomer, 1-10 parts of polyvinyl butyral, 10-20 parts of terpene resin, 8-18 parts of tackifying resin, 10-20 parts of plasticizer, 0.1-2 parts of antioxidant and 0.1-2 parts of light stabilizer.

2. The high temperature resistant hot melt pressure sensitive adhesive according to claim 1, characterized in that: The invention comprises the following components in parts by weight: 21-25 parts of thermoplastic elastomer, 5-9 parts of polyvinyl butyral, 10-14 parts of terpene resin, 8-14 parts of tackifying resin, 15-19 parts of plasticizer, 0.5-1.5 parts of antioxidant and 1-2 parts of light stabilizer.

3. The high temperature resistant hot melt pressure sensitive adhesive according to claim 2, characterized in that: The thermoplastic elastomer is thermoplastic styrene-butadiene rubber, and the melt index of the thermoplastic styrene-butadiene rubber is 8-24 g / 10 min under the conditions of 200° C. and 5 kg.

4. The high temperature resistant hot melt pressure sensitive adhesive according to claim 1, characterized in that: The viscosity of polyvinyl butyral at 20° C. is 14-20 mPa·s, and the content of polyvinyl alcohol is 18-21 wt %.

5. The high temperature resistant hot melt pressure sensitive adhesive according to claim 1, characterized in that: The softening point of terpene resin is 95°C.

6. The high temperature resistant hot melt pressure sensitive adhesive according to claim 1, characterized in that: The tackifying resin is selected from at least one of C5 petroleum resin, C5 hydrogenated petroleum resin and rosin resin.

7. The high temperature resistant hot melt pressure sensitive adhesive according to claim 1, characterized in that: The plasticizer comprises naphthenic oil, chlorinated paraffin and di(2-ethylhexyl) phthalate in a weight ratio of 1:(1.3-1.5):(0.4-0.7).

8. The high temperature resistant hot melt pressure sensitive adhesive according to claim 7, characterized in that: The plasticizer accounts for 40-45% of the total weight of the thermoplastic elastomer, polyvinyl butyral and terpene resin.

9. A method for preparing the high temperature resistant hot melt pressure sensitive adhesive according to any one of claims 1 to 8, characterized in that: The following steps are involved: Thermoplastic elastomer, polyvinyl butyral, terpene resin, tackifying resin, plasticizer, antioxidant and light stabilizer are mixed, heated to melt, vacuumed and stirred to be uniform to prepare a high temperature resistant hot melt pressure sensitive adhesive.

10. Use of the high temperature resistant hot melt pressure sensitive adhesive according to any one of claims 1 to 8 in the preparation of polymer waterproof membrane.

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