A high-reliability tireless self-adhesive waterproof membrane and its production process

Abstract

The present invention provides a highly reliable, tireless, self-adhesive waterproofing membrane and its production process. The membrane comprises a composite membrane formed by bonding a polytetrafluoroethylene membrane and a polyethylene membrane, and a self-adhesive material comprising the following components: aromatic oil, bio-asphalt, polyisobutylene, DCP, SBS, C5 hydrogenated petroleum resin, SBR, talc, PPD, nano-zirconium powder, and eucommia gum. The tireless waterproofing membrane produced by this invention offers a long service life, excellent durability, and high reliability, and can be applied under low-temperature conditions of (-5-10)°C.

Description

Technical Field

[0001] The present invention relates to the field of waterproof rolls, and in particular to a high-reliability tireless self-adhesive waterproof roll and a production process thereof. Background Art

[0002] Self-adhesive waterproofing membrane is made from a self-adhesive rubber asphalt base, made from synthetic rubbers like SBS, tackifiers, and high-quality road petroleum asphalt. It features a tough, high-density polyethylene film or aluminum foil as the top surface and a removable silicone-coated release film or paper as the bottom surface. This waterproofing membrane is a promising new waterproofing material, characterized by low-temperature flexibility, self-healing properties, and excellent adhesion. It can be applied at room temperature, is fast, and meets environmental standards.

[0003] However, the reliability level of existing asphalt-based tireless self-adhesive waterproof membranes is low (reaching levels 10 and 15), and their durability and weather resistance are poor; the polymer membrane base used in existing tireless self-adhesive waterproof membranes is PET and PE, which have poor durability, limiting the reliability level of the waterproof membranes; existing self-adhesive waterproof membranes cannot be constructed under low temperature conditions, and auxiliary heating is required during winter construction to complete the construction, which consumes manpower and time.

[0004] In the existing technology, a polytetrafluoroethylene composite isolation material and preparation method and a self-adhesive asphalt waterproof membrane with patent number CN202011322447.2, and a self-adhesive asphalt and heat-insulating tireless waterproof membrane and preparation method with patent number CN201811397676.3 have certain technical advantages over traditional tireless self-adhesive waterproof membranes, but they still cannot solve the problems of the existing technology such as inability to construct at low temperatures and poor durability.

[0005] It can be seen that the existing technology has the following technical problems: the service life of tireless waterproof membrane is short, the durability of membrane base and self-adhesive material is poor; it cannot be constructed under low temperature conditions of -5°C. Summary of the Invention

[0006] In response to the above technical problems, the present invention provides a high-reliability tireless self-adhesive waterproof membrane and its production process, and aims to achieve the following invention objectives: the prepared tireless waterproof membrane has a long service life, good durability and high reliability; and can be constructed under low temperature conditions of (-5~-10)℃.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions:

[0008] The highly reliable, tireless, self-adhesive waterproof membrane comprises a composite membrane, a self-adhesive material, and a barrier membrane from top to bottom. The composite membrane is formed by dry or wet bonding of a polytetrafluoroethylene (PTFE) membrane and a polyethylene (PE) membrane. The thickness of the PTFE membrane is 0.065-0.075 mm, and the thickness of the polyethylene membrane is 0.035-0.045 mm.

[0009] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane comprises the following components, calculated by weight: 40-50 parts of aromatic oil, 10-15 parts of bio-asphalt, 8-12 parts of polyisobutylene, 0.05-0.1 parts of DCP, 4-6 parts of SBS, 2-4 parts of C5 hydrogenated petroleum resin, 3-5 parts of SBR, 5-10 parts of nano zirconium powder, 3-5 parts of eucommia gum, 20-25 parts of talc, and 1-2 parts of PPD.

[0010] The aromatic oil: aromatic content is more than 90%;

[0011] The bio-asphalt has the following characteristics: bio-oil ratio <10%; needle penetration (25°C, 5s, 100g) 70-100; softening point ≥40°C; elongation at 15°C ≥30cm; and flash point ≥200°C.

[0012] The SBS is linear SBS with a molecular weight of 100,000-120,000;

[0013] The SBR is powder or sheet styrene butadiene rubber with a content of more than 80%;

[0014] The talcum powder is 600 mesh;

[0015] The nano zirconium powder has an average particle size of 20-50 nm and a density of 6.0-6.5 g / cm 3 ;

[0016] The Eucommia gum has a density of 0.95-0.98 g / cm 3 .

[0017] A method for preparing a high-reliability tireless self-adhesive waterproof membrane, the preparation method comprises the following steps:

[0018] Step 1: Prepare self-adhesive material

[0019] (1) Weigh the raw materials according to the formula of the self-adhesive material and set aside.

[0020] (2) Add aromatic oil, bio-asphalt, and polyisobutylene into a stirring tank, start stirring at a rate of 20-25 Hz, start heating, heat to 130-140 ° C, and stir for 20-30 minutes.

[0021] (3) Add DCP to the mixing tank and measure the viscosity of the asphalt material every 10 minutes using a handheld viscometer. If the viscosity does not increase for three consecutive times, proceed to the next step.

[0022] (4) Add SBR and Eucommia gum to the mixing tank, control the temperature at 130-140℃, adjust the stirring rate to 40-45Hz, and the stirring time to 50-60min. After completion, grind it in a colloid mill.

[0023] (5) Add SBS and C5 hydrogenated resin to the stirring tank, heat it to 150-160℃, keep the stirring rate at 40-45Hz, and stir for 90-100min. After completion, grind it in a colloid mill.

[0024] (6) Add nano zirconium powder, PPD, and talc powder to the stirring tank, control the temperature at 130-140 °C, adjust the stirring rate to 35-40 Hz, and discharge the material after stirring for 50-60 min to obtain a self-adhesive material.

[0025] Step 2: Preparation of composite membrane

[0026] The polytetrafluoroethylene film and the polyethylene film are bonded together by a traditional dry method to form a composite film.

[0027] The thickness of the polytetrafluoroethylene film is 0.065-0.075 mm, and the thickness of the polyethylene film is 0.035-0.045 mm.

[0028] Step 3: Coating

[0029] The prepared self-adhesive material is applied to the surface of the polyethylene film side of the composite film with a coating thickness of 1.5-2.0 mm and a coating temperature of 130-140° C. After coating, the surface of the self-adhesive material is covered with an isolation film.

[0030] Step 4: The coated coiled material is cooled, shaped, measured, rolled, and packaged to obtain a highly reliable tireless self-adhesive waterproof coiled material.

[0031] The present invention improves the reliability level of tireless self-adhesive roll materials to a level greater than 25 through the use of a specific composite film and a self-adhesive material; the specific self-adhesive material combination of the present invention has excellent initial adhesion, stability, and viscosity under low temperature conditions; the excellent anti-aging performance of bio-asphalt and excellent compatibility with other materials are not possessed by traditional asphalt; the formula of the present invention using polyisobutylene as the softening system allows the roll material to have excellent stability while maintaining good low-temperature flexibility, and the softener is not easy to volatilize in the roll material; the specific combination of nano-zirconium powder and eucommia gum of the present invention is added to the formula system, which greatly improves the corrosion resistance and anti-aging performance of the waterproof roll material; the production process of the roll material of the present invention uses a lower degree of cross-linking, making the formula system more stable and easy to process, safe and efficient.

[0032] The present invention has the following beneficial effects:

[0033] (1) The tireless waterproof membrane prepared by the present invention has a service life of more than 25 years, good durability, and a reliability of up to 25 levels; it can be constructed under low temperature conditions of (-5~-10)°C;

[0034] (2) The asphalt elongation at break of the tireless self-adhesive waterproof membrane prepared by the present invention reaches more than 750%, and can still reach more than 650% after heat treatment (70℃×7d).

[0035] (3) After hot air aging (80°C×28d), the tireless self-adhesive waterproof membrane prepared by the present invention has low-temperature flexibility of -30~-33°C without cracks, and the peel strength between membranes is 1.7~2.0N / mm, and the peel strength between membranes and aluminum plates is 1.8~2.0N / mm.

[0036] (4) The tireless self-adhesive waterproof membrane prepared by the present invention has a water resistance (23°C×40d) of 0.1-0.3%, and a water resistance (60°C×14d) of 0.7-0.1%. DETAILED DESCRIPTION

[0037] Example 1 A high-reliability tireless self-adhesive waterproof membrane and its production process

[0038] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane, comprising the following components in parts by weight:

[0039] Aromatic oil 40 parts, bio-asphalt 15 parts, polyisobutylene 12 parts, DCP 0.05 parts, SBS 4 parts, C5 hydrogenated petroleum resin 4 parts, SBR 5 parts, nano zirconium powder 5 parts, eucommia gum 3 parts, talc 20 parts, PPD 2 parts.

[0040] The aromatic oil has an aromatic content of more than 90%;

[0041] The bio-asphalt has a bio-oil blending ratio of 7%, a needle penetration (25°C, 5s, 100g) of 70, a softening point of 42°C, and an elongation of 30cm at 15°C.

[0042] The SBS is linear SBS with a molecular weight of 100,000;

[0043] The SBR: styrene-butadiene rubber content is 80%;

[0044] The talcum powder is 600 mesh;

[0045] The nano zirconium powder has an average particle size of 20 nm and a density of 6.5 g / cm 3 ;

[0046] The eucommia gum: density 0.98g / cm 3 .

[0047] A method for preparing a high-reliability tireless self-adhesive waterproof membrane, the preparation method comprises the following steps:

[0048] Step 1: Prepare self-adhesive material

[0049] (1) Weigh the raw materials according to the formula of the self-adhesive material and set aside.

[0050] (2) Add aromatic oil, bio-asphalt, and polyisobutylene into a stirring tank, start stirring at a stirring rate of 22 Hz, start heating, heat to 135 °C, and stir for 26 min.

[0051] (3) Add DCP to the mixing tank and measure the viscosity of the asphalt material every 10 minutes using a handheld viscometer. If the viscosity does not increase for three consecutive times, proceed to the next step.

[0052] (4) Add SBR and Eucommia gum to the mixing tank, control the temperature at 135℃, adjust the stirring rate to 43Hz, and the stirring time to 55min. After completion, grind it once in a colloid mill.

[0053] (5) Add SBS and C5 hydrogenated resin to the stirring tank, raise the temperature to 155 ° C, maintain the stirring rate at 42 Hz, and stir for 95 minutes. After completion, grind it once in a colloid mill.

[0054] (6) Add nano zirconium powder, PPD, and talc powder to the stirring tank, control the temperature at 135 °C, adjust the stirring rate to 37 Hz, and discharge the material after stirring for 55 min to obtain a self-adhesive material.

[0055] Step 2: Preparation of composite membrane

[0056] The polytetrafluoroethylene film and the polyethylene film are bonded together by a traditional dry method to form a composite film.

[0057] The thickness of the polytetrafluoroethylene film is 0.07 mm, and the thickness of the polyethylene film is 0.04 mm.

[0058] Step 3: Coating

[0059] The prepared self-adhesive material is applied to the surface of the polyethylene film side of the composite film with a coating thickness of 1.5 mm and a coating temperature of 135° C. After coating, the surface of the self-adhesive material is covered with an isolation film.

[0060] Step 4: The coated coiled material is cooled, shaped, measured, rolled, and packaged to obtain a highly reliable tireless self-adhesive waterproof coiled material.

[0061] Example 2 A high-reliability tireless self-adhesive waterproof membrane and its production process

[0062] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane, comprising the following components in parts by weight:

[0063] 45 parts of aromatic oil, 12.5 parts of bio-asphalt, 10 parts of polyisobutylene, 0.05 parts of DCP, 5 parts of SBS, 3 parts of C5 hydrogenated petroleum resin, 4 parts of SBR, 5 parts of nano zirconium powder, 3 parts of eucommia gum, 23 parts of talc, and 1.5 parts of PPD.

[0064] The aromatic oil has an aromatic content of more than 90%;

[0065] The bio-asphalt has a bio-oil blending ratio of 8.7%, a needle penetration (25°C, 5s, 100g) of 85, a softening point of 45°C, and an elongation of 31 cm at 15°C.

[0066] The SBS is linear SBS with a molecular weight of 120,000;

[0067] The SBR: styrene-butadiene rubber content is 80%;

[0068] The talcum powder is 600 mesh;

[0069] The nano zirconium powder has an average particle size of 30 nm and a density of 6.3 g / cm 3 ;

[0070] The eucommia gum: density 0.98g / cm 3 .

[0071] A method for preparing a high-reliability tireless self-adhesive waterproof membrane, the preparation method comprises the following steps:

[0072] Step 1: Prepare self-adhesive material

[0073] (1) Weigh the raw materials according to the formula of the self-adhesive material and set aside.

[0074] (2) Add aromatic oil, bio-asphalt, and polyisobutylene into a stirring tank, start stirring at a stirring rate of 25 Hz, start heating, heat to 130 °C, and stir for 30 min.

[0075] (3) Add DCP to the mixing tank and measure the viscosity of the asphalt material every 10 minutes using a handheld viscometer. If the viscosity does not increase for three consecutive times, proceed to the next step.

[0076] (4) Add SBR and Eucommia gum to the mixing tank, control the temperature at 140℃, adjust the stirring rate to 40Hz, and stir for 60min. After completion, grind it once in a colloid mill.

[0077] (5) Add SBS and C5 hydrogenated resin to the stirring tank, raise the temperature to 160℃, maintain the stirring rate at 40Hz, and stir for 90min. After completion, grind it once in a colloid mill.

[0078] (6) Add nano zirconium powder, PPD, and talc powder to the stirring tank, control the temperature at 140 °C, adjust the stirring rate to 35 Hz, and discharge the material after stirring for 50 minutes to obtain a self-adhesive material.

[0079] Step 2: Preparation of composite membrane

[0080] The polytetrafluoroethylene film and the polyethylene film are bonded together by a traditional dry method to form a composite film.

[0081] The thickness of the polytetrafluoroethylene film is 0.07 mm, and the thickness of the polyethylene film is 0.04 mm.

[0082] Step 3: Coating

[0083] The prepared self-adhesive material is applied to the surface of the polyethylene film side of the composite film with a coating thickness of 1.5 mm and a coating temperature of 130° C. After coating, the surface of the self-adhesive material is covered with an isolation film.

[0084] Step 4: The coated coiled material is cooled, shaped, measured, rolled, and packaged to obtain a highly reliable tireless self-adhesive waterproof coiled material.

[0085] Example 3 A high-reliability tireless self-adhesive waterproof membrane and its production process

[0086] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane, comprising the following components in parts by weight:

[0087] 50 parts of aromatic oil, 10 parts of bio-asphalt, 8 parts of polyisobutylene, 0.1 parts of DCP, 6 parts of SBS, 2 parts of C5 hydrogenated petroleum resin, 3 parts of SBR, 5 parts of nano zirconium powder, 3 parts of eucommia gum, 25 parts of talc, and 1 part of PPD.

[0088] The aromatic oil has an aromatic content of more than 90%;

[0089] The bio-asphalt has a bio-oil blending ratio of 9%, a needle penetration (25°C, 5s, 100g) of 89, a softening point of 43°C, and an elongation of 31.5 cm at 15°C.

[0090] The SBS is linear SBS with a molecular weight of 115,000;

[0091] The SBR: styrene-butadiene rubber content is 85%;

[0092] The talcum powder is 600 mesh;

[0093] The nano zirconium powder has an average particle size of 38 nm and a density of 6.1 g / cm 3 ;

[0094] The Eucommia gum: density 0.95g / cm 3 .

[0095] A method for preparing a high-reliability tireless self-adhesive waterproof membrane, the preparation method comprises the following steps:

[0096] Step 1: Prepare self-adhesive material

[0097] (1) Weigh the raw materials according to the formula of the self-adhesive material and set aside.

[0098] (2) Add aromatic oil, bio-asphalt, and polyisobutylene into a stirring tank, start stirring at a stirring rate of 20 Hz, start heating, heat to 140 °C, and stir for 20 min.

[0099] (3) Add DCP to the mixing tank and measure the viscosity of the asphalt material every 10 minutes using a handheld viscometer. If the viscosity does not increase for three consecutive times, proceed to the next step.

[0100] (4) Add SBR and Eucommia gum to the mixing tank, control the temperature at 130℃, adjust the stirring rate to 45Hz, and stir for 50min. After completion, grind it in a colloid mill.

[0101] (5) Add SBS and C5 hydrogenated resin to the stirring tank, heat to 150℃, maintain the stirring rate at 45Hz, and stir for 100min. After completion, grind it once in a colloid mill.

[0102] (6) Add nano zirconium powder, PPD, and talc powder to the stirring tank, control the temperature at 130 °C, adjust the stirring rate to 40 Hz, and discharge the material after stirring for 60 min to obtain a self-adhesive material.

[0103] Step 2: Preparation of composite membrane

[0104] The polytetrafluoroethylene film and the polyethylene film are bonded together by a traditional dry method to form a composite film.

[0105] The thickness of the polytetrafluoroethylene film is 0.07 mm, and the thickness of the polyethylene film is 0.04 mm.

[0106] Step 3: Coating

[0107] The prepared self-adhesive material is coated on the surface of the polyethylene film side of the composite film with a coating thickness of 1.5 mm and a coating temperature of 140° C. After coating, the surface of the self-adhesive material is covered with an isolation film.

[0108] Step 4: The coated coiled material is cooled, shaped, measured, rolled, and packaged to obtain a highly reliable tireless self-adhesive waterproof coiled material.

[0109] Example 4 A high-reliability tireless self-adhesive waterproof membrane and its production process

[0110] Same as Example 1, only the composition ratio of the self-adhesive material is changed to the following:

[0111] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane, comprising the following components in parts by weight:

[0112] 40 parts of aromatic oil, 15 parts of bio-asphalt, 12 parts of polyisobutylene, 0.05 parts of DCP, 4 parts of SBS, 4 parts of C5 hydrogenated petroleum resin, 5 parts of SBR, 10 parts of nano zirconium powder, 5 parts of eucommia gum, 20 parts of talc, and 2 parts of PPD.

[0113] Produced according to the preparation method described in Example 1.

[0114] Example 5 A high-reliability tireless self-adhesive waterproof membrane and its production process

[0115] Same as Example 2, only the composition ratio of the self-adhesive material is changed to the following:

[0116] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane, comprising the following components in parts by weight:

[0117] 45 parts of aromatic oil, 12.5 parts of bio-asphalt, 10 parts of polyisobutylene, 0.05 parts of DCP, 5 parts of SBS, 3 parts of C5 hydrogenated petroleum resin, 4 parts of SBR, 10 parts of nano zirconium powder, 5 parts of eucommia gum, 23 parts of talc, and 1.5 parts of PPD.

[0118] Produced according to the preparation method described in Example 2.

[0119] Example 6 A high-reliability tireless self-adhesive waterproof membrane and its production process

[0120] Same as Example 3, only the composition ratio of the self-adhesive material is changed to the following:

[0121] A self-adhesive material for a high-reliability tireless self-adhesive waterproof membrane, comprising the following components in parts by weight:

[0122] 50 parts of aromatic oil, 10 parts of bio-asphalt, 8 parts of polyisobutylene, 0.1 parts of DCP, 6 parts of SBS, 2 parts of C5 hydrogenated petroleum resin, 3 parts of SBR, 10 parts of nano zirconium powder, 5 parts of eucommia gum, 25 parts of talc, and 1 part of PPD.

[0123] Produced according to the preparation method described in Example 3.

[0124] The tireless self-adhesive waterproof membranes prepared in Examples 1-6 were tested for their technical parameters according to the test methods of GB23441-2009 "Self-adhesive polymer modified asphalt waterproof membrane" (the "elongation at break of asphalt" refers to this standard) and CTS 07013-2020 "Technical Specification for Reliability Grade Certification of Building Waterproof Membrane" (the "heat aging and water resistance" refers to this standard). The specific test results are shown in Table 1:

[0125] Table 1

[0126]

[0127] As can be seen from Table 1, the asphalt elongation at break of the tireless self-adhesive waterproof membrane prepared by the present invention is 764-805%, and the elongation at break of the asphalt after heat treatment at 70°C × 7d is 673-703%; after aging in hot air at 80°C for 28d, the low-temperature flexibility reaches -30~-33°C without cracks, the peel strength between the membranes is 1.78~1.97N / mm, and the peel strength between the membrane and the aluminum plate is 1.83~1.93N / mm; the water resistance (23°C × 40d) is 0.15-0.25%, and the water resistance (60°C × 14d) is 0.73-0.96%.

[0128] The reliability of waterproof membranes is characterized by two aspects: aging resistance and water resistance. The table above shows that the hot air aging (80°C x 28 days) and water resistance (23°C x 40 days) of this patented product both meet the requirements of Reliability Level 25, with ample margin.

[0129] Asphalt elongation at break reflects the overall stability of the asphalt material and demonstrates the excellent stability of the formulation under thermal aging conditions. Peel strength reflects the waterproof membrane's construction performance. Its ability to maintain excellent adhesion under aging conditions demonstrates both the membrane's storage durability and its robustness and reliability after bonding.

[0130] Unless otherwise specified, all ratios and percentages described in the present invention are by mass.

[0131] The above-described embodiments merely illustrate preferred implementations of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications or variations that can be made by those skilled in the art without inventive effort are still within the scope of protection of the present invention.

Claims

1. A high-reliability tireless self-adhesive waterproof membrane, characterized by: It includes a composite film and a self-adhesive material; the composite film is formed by bonding a polytetrafluoroethylene film and a polyethylene film; the self-adhesive material includes the following components: aromatic oil, bio-asphalt, polyisobutylene, DCP, SBS, C5 hydrogenated petroleum resin, SBR, talc, PPD, nano zirconium powder and eucommia gum; the nano zirconium powder has an average particle size of 20-50nm; The self-adhesive material comprises the following components, in parts by weight: 40-50 parts of aromatic oil, 10-15 parts of bio-asphalt, 8-12 parts of polyisobutylene, 0.05-0.1 parts of DCP, 4-6 parts of SBS, 2-4 parts of C5 hydrogenated petroleum resin, 3-5 parts of SBR, 5-10 parts of nano zirconium powder, 3-5 parts of eucommia gum, 20-25 parts of talc, and 1-2 parts of PPD.

2. The high-reliability tireless self-adhesive waterproof membrane according to claim 1, characterized in that: The aromatic oil has an aromatic content of more than 90%; the bio-asphalt has a bio-oil blending ratio of less than 10%.

3. The high-reliability tireless self-adhesive waterproof membrane according to claim 1, characterized in that: The SBS is linear SBS with a molecular weight of 100,000 to 120,000.

4. The method for preparing a high-reliability tireless self-adhesive waterproof membrane according to claim 1, characterized in that: The method comprises the steps of preparing a self-adhesive material, preparing a composite film and coating. The composite film preparation comprises bonding a polytetrafluoroethylene film and a polyethylene film to form a composite film. The thickness of the polytetrafluoroethylene film is 0.065-0.075 mm, and the thickness of the polyethylene film is 0.035-0.045 mm.

5. The method for preparing a high-reliability tireless self-adhesive waterproof membrane according to claim 4, characterized in that: The preparation of the self-adhesive material comprises the following steps: adding aromatic oil, bio-asphalt, and polyisobutylene into a stirring tank, starting stirring and heating for 20-30 minutes; adding DCP; stirring at a rate of 20-25 Hz, and heating to 130-140° C.

6. The method for preparing a high-reliability tireless self-adhesive waterproof membrane according to claim 4, characterized in that: The preparation of the self-adhesive material further comprises the following steps: adding SBR and eucommia gum into a stirring tank, adjusting the stirring rate to 40-45 Hz, stirring for 50-60 minutes, and passing through a colloid mill.

7. The method for preparing a high-reliability tireless self-adhesive waterproof membrane according to claim 4, characterized in that: The preparation of the self-adhesive material further comprises the following steps: adding SBS and C5 hydrogenated petroleum resin into a stirring tank, heating to 150-160° C., stirring for 90-100 minutes, and passing through a colloid mill; adding nano zirconium powder, PPD, and talc powder, controlling the temperature at 130-140° C., adjusting the stirring rate to 35-40 Hz, and stirring for 50-60 minutes.

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