CN107936863B - Preparation method of multilayer composite waterproof roll - Google Patents

Preparation method of multilayer composite waterproof roll Download PDF

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Publication number
CN107936863B
CN107936863B CN201711240988.9A CN201711240988A CN107936863B CN 107936863 B CN107936863 B CN 107936863B CN 201711240988 A CN201711240988 A CN 201711240988A CN 107936863 B CN107936863 B CN 107936863B
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mass
parts
waterproof roll
acrylic resin
organic silicon
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CN107936863A (en
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王小武
李培任
杨才权
周虎
熊一帜
蹇建
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Hunan Shenyu New Material Co ltd
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Hunan Shenyu New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2433/00Presence of (meth)acrylic polymer
    • C09J2433/006Presence of (meth)acrylic polymer in the substrate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2463/00Presence of epoxy resin
    • C09J2463/006Presence of epoxy resin in the substrate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2479/00Presence of polyamine or polyimide
    • C09J2479/08Presence of polyamine or polyimide polyimide
    • C09J2479/086Presence of polyamine or polyimide polyimide in the substrate

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Laminated Bodies (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a preparation method of a multilayer composite waterproof roll. The invention mainly comprises the steps of mixing butyl acrylate, methyl methacrylate, styrene, acrylic acid, hydroxyethyl acrylate, an emulsifier and a solvent, and stirring for reaction to obtain an acrylic resin glue solution; coating the acrylic resin glue solution on the upper side surface of the polyimide film by a roller, and drying at constant temperature to form an acrylic resin layer; stirring and mixing epoxy resin, a polyamide curing agent, a polyether amine curing agent, a light shielding agent, a plasticizer and a diluent for 20 minutes, coating the mixture on the upper side surface of an acrylic resin layer, and curing to form an epoxy resin layer; and coating the organic silicon adhesive glue on the lower side surface of the polyimide film layer, and drying to form the organic silicon adhesive bonding layer. The invention adopts a multilayer composite structure, has good waterproof performance, mechanical performance and chemical stability, prolongs the service life and avoids environmental pollution in the construction process.

Description

Preparation method of multilayer composite waterproof roll
Technical Field
The invention belongs to the field of polymer synthesis and processing, and particularly relates to a preparation method of a multilayer composite waterproof roll.
Background
With the rapid development of urban construction and infrastructure construction in China, the waterproof roll is gradually applied to the fields of buildings, bridges and tunnels, traffic transportation and the like. The waterproof coiled material product mainly comprises an asphalt type waterproof coiled material and a high polymer type waterproof coiled material. However, the asphalt type waterproof roll requires a hot melting method during construction, which causes asphalt contamination and also damages the health of the constructors. In recent years, most cities have banned the use of this process for the production of waterproofing rolls.
The high-molecular waterproof coiled material is mainly prepared by using synthetic resin, synthetic rubber or a mixture of the synthetic resin and the synthetic rubber as a matrix, adding chemical auxiliaries and fillers, and carrying out calendering, extrusion, banburying and other methods. The high-molecular waterproof coiled material has the advantages of high tensile strength, high tear strength, good heat resistance, good homogeneity, good low-temperature flexibility and the like. And by adding the chemical additives and the fillers, the aging resistance and the oxidation resistance of the high-molecular waterproof roll can be improved. Therefore, the polymer waterproof roll becomes the main force of the future waterproof roll.
Disclosure of Invention
The invention aims to provide a preparation method of a multilayer composite waterproof roll, which comprises the following steps:
(1) mixing 65-80 parts by mass of Butyl Acrylate (BA), 15-30 parts by mass of Methyl Methacrylate (MMA), 5-20 parts by mass of styrene (PS), 2-4 parts by mass of Acrylic Acid (AA), 2-4 parts by mass of hydroxyethyl acrylate (HEA), 2-5 parts by mass of an emulsifier and 40 parts by mass of a solvent, and stirring and reacting at 80 ℃ for 6 hours to prepare an acrylic resin glue solution;
(2) coating the acrylic resin glue solution prepared in the step (1) on the upper side surface of a polyimide film in a rolling way, drying at the constant temperature of 50-60 ℃, and drying the acrylic resin glue solution to form an acrylic resin layer;
(3) stirring and mixing 100 parts by mass of epoxy resin (E-44), 20-30 parts by mass of polyamide curing agent (650), 20-30 parts by mass of polyetheramine curing agent (D400), 1.5-4.5 parts by mass of light shielding agent, 1.5-7.5 parts by mass of plasticizer and 15-45 parts by mass of diluent for 20 minutes, coating the mixture on the upper side surface of the acrylic resin layer in the step (2), and curing at 50-60 ℃ to form an epoxy resin layer;
(4) coating the organic silicon self-adhesive glue on the lower side surface of the polyimide film layer, and drying to form an organic silicon self-adhesive bonding layer;
(5) the multilayer composite waterproof roll is formed by the epoxy resin layer, the acrylic resin layer, the polyimide film layer and the organic silicon adhesive bonding layer.
Specifically, in the step (1), the solvent is ethyl acetate, and the stirring speed in the reaction process is 120 r/min.
Specifically, in the step (2), the polyimide film is prepared by a casting method, and the shore hardness is 70 degrees.
Specifically, in the step (3), the light shielding agent is carbon black with the particle size of 325 meshes, the plasticizer is epoxidized vegetable oil, and the diluent is phenyl glycidyl ether.
Specifically, in the step (4), the organic silicon self-adhesive glue is a solvent type glue, the main component is organic silicon self-adhesive resin, the solid content of the organic silicon self-adhesive glue is 35%, and the viscosity of the organic silicon self-adhesive resin is 1-2 Pa ∙ seconds.
Specifically, in the step (5), the thickness of the epoxy resin layer is 0.30-0.50 mm, the thickness of the acrylic resin layer is 0.35-0.50 mm, the thickness of the polyimide film layer is 0.70-0.90 mm, and the thickness of the organic silicon non-setting adhesive bonding layer is 0.10-0.12 mm; the total thickness of the waterproof roll is 1.45-2.02 mm, and the width of the waterproof roll is controlled to be 1.00 m.
Compared with the traditional polymer waterproof coiled material, the invention has the following advantages:
(1) the invention adopts a multilayer composite structure, takes the polyimide film layer as a main waterproof layer, and the polyimide has good mechanical property and chemical stability, thereby not only ensuring the good performance of the invention, but also ensuring the service life of the invention.
(2) The surface of the waterproof coiled material is coated with the epoxy resin layer, and the epoxy resin can play a good role in protecting the waterproof coiled material. Meanwhile, the invention adopts a cold processing technology in the construction process, and can avoid environmental pollution brought by the asphalt refining process.
Detailed Description
The present invention will be described in further detail by the following specific examples, wherein the raw materials are all industrial products, and the equipment is common industrial production equipment.
Example 1:
adding 65kg of Butyl Acrylate (BA), 30kg of Methyl Methacrylate (MMA), 15kg of styrene (PS), 2kg of Acrylic Acid (AA), 2kg of hydroxyethyl acrylate (HEA), 2kg of emulsifier and 40kg of ethyl acetate into a reaction kettle for mixing, and stirring and reacting at 80 ℃ for 6 hours to obtain an acrylic resin glue solution; coating an acrylic resin glue solution on the upper side of a polyimide film layer (prepared by a casting method) with the thickness of 0.70mm by a roller, and drying at 50 ℃ to prepare an acrylic resin layer with the thickness of 0.35 mm; mixing 100kg of epoxy resin (E-44), 20kg of polyamide curing agent (650), 20kg of polyetheramine curing agent (D400), 1.5kg of carbon black with the granularity of 325 meshes, 1.5kg of epoxidized vegetable oil and 15kg of phenyl glycidyl ether, stirring for 20 minutes, coating the mixture on the upper side surface and the side surface of an acrylic resin layer, and curing at 50 ℃ to form an epoxy resin layer with the thickness of 0.30 mm; and coating the organic silicon adhesive glue on the lower side surface of the polyimide film layer, and drying to form an organic silicon adhesive bonding layer with the thickness of 0.10mm, thereby preparing the multilayer composite waterproof roll.
In the embodiment, the stirring speed is 120r/min in the preparation process of the acrylic resin glue solution; the Shore hardness of the polyimide film layer is 70 degrees; the organic silicon self-adhesive glue is a solvent type glue, the main component is organic silicon self-adhesive resin, the solid content is 35%, and the viscosity is 1-2 Pa ∙ seconds; the total thickness of the waterproof roll is 1.45mm, and the width is controlled to be 1.00 m.
Example 2:
putting 75kg of Butyl Acrylate (BA), 15kg of Methyl Methacrylate (MMA), 20kg of styrene (PS), 3kg of Acrylic Acid (AA), 3kg of hydroxyethyl acrylate (HEA), 3kg of emulsifier and 40kg of ethyl acetate into a reaction kettle for mixing, and stirring and reacting at 80 ℃ for 6 hours to obtain an acrylic glue solution; coating the acrylic acid glue solution on the upper side of a polyimide film layer (prepared by a casting method) with the thickness of 0.80mm in a roller manner, and drying at 50 ℃ to prepare an acrylic acid resin layer with the thickness of 0.40 mm; mixing and stirring 100kg of epoxy resin (E-44), 23kg of polyamide curing agent (650), 25kg of polyetheramine curing agent (D400), 2.5kg of carbon black with the granularity of 325 meshes, 3.5kg of epoxidized vegetable oil and 25kg of phenyl glycidyl ether for 20 minutes, coating the mixture on the upper side surface and the side surface of an acrylic resin layer, and curing at 50 ℃ to form an epoxy resin layer with the thickness of 0.37 mm; and coating the organic silicon adhesive glue on the lower side surface of the polyimide film layer, and drying to form an organic silicon adhesive bonding layer with the thickness of 0.11mm, thereby preparing the multilayer composite waterproof roll.
In the embodiment, the stirring speed is 120r/min in the preparation process of the acrylic resin glue solution; the Shore hardness of the polyimide film layer is 70 degrees; the organic silicon self-adhesive glue is a solvent type glue, the main component is organic silicon self-adhesive resin, the solid content is 35%, and the viscosity is 1-2 Pa ∙ seconds; the total thickness of the waterproof roll is 1.68mm, and the width is controlled to be 1.00 m.
Example 3:
putting 65kg of Butyl Acrylate (BA), 25kg of Methyl Methacrylate (MMA), 10kg of styrene (PS), 3kg of Acrylic Acid (AA), 3kg of hydroxyethyl acrylate (HEA), 4kg of emulsifier and 40kg of ethyl acetate into a reaction kettle for mixing, and stirring and reacting at 80 ℃ for 6 hours to obtain an acrylic glue solution; coating the acrylic acid glue solution on the upper side of a polyimide film layer (prepared by a casting method) with the thickness of 0.80mm in a roller manner, and drying at the temperature of 60 ℃ to prepare an acrylic acid resin layer with the thickness of 0.45 mm; mixing and stirring 100kg of epoxy resin (E-44), 27kg of polyamide curing agent (650), 27kg of polyetheramine curing agent (D400), 3.5kg of carbon black with the granularity of 325 meshes, 5.5kg of epoxidized vegetable oil and 35kg of phenyl glycidyl ether for 20 minutes, coating the mixture on the upper side surface and the side surface of an acrylic resin layer, and curing at the temperature of 60 ℃ to form an epoxy resin layer with the thickness of 0.43 mm; and coating the organic silicon adhesive glue on the lower side surface of the polyimide film layer, and drying to form an organic silicon adhesive bonding layer with the thickness of 0.11mm, thereby preparing the multilayer composite waterproof roll.
In the embodiment, the stirring speed is 120r/min in the preparation process of the acrylic resin glue solution; the Shore hardness of the polyimide film layer is 70 degrees; the organic silicon self-adhesive glue is a solvent type glue, the main component is organic silicon self-adhesive resin, the solid content is 35%, and the viscosity is 1-2 Pa ∙ seconds; the total thickness of the waterproof roll is 1.79mm, and the width is controlled to be 1.00 m.
Example 4:
putting 80kg of Butyl Acrylate (BA), 15kg of Methyl Methacrylate (MMA), 5kg of styrene (PS), 4kg of Acrylic Acid (AA), 4kg of hydroxyethyl acrylate (HEA), 5kg of emulsifier and 40kg of ethyl acetate into a reaction kettle for mixing, and stirring and reacting at 80 ℃ for 6 hours to obtain an acrylic glue solution; coating the acrylic acid glue solution on the upper side of a polyimide film layer (prepared by a casting method) with the thickness of 0.90mm in a roller manner, and drying at the temperature of 60 ℃ to prepare an acrylic acid resin layer with the thickness of 0.50 mm; 100kg of epoxy resin (E-44), 30kg of polyamide curing agent (650), 30kg of polyetheramine curing agent (D400), 4.5kg of carbon black with the granularity of 325 meshes, 7.5kg of epoxidized vegetable oil and 45kg of phenyl glycidyl ether are mixed for 20 minutes by stirring, coated on the upper side surface and the lower side surface of an acrylic resin layer and cured at the temperature of 60 ℃ to form an epoxy resin layer with the thickness of 0.50 mm; and coating the organic silicon adhesive glue on the lower side surface of the polyimide film layer, and drying to form an organic silicon adhesive bonding layer with the thickness of 0.12mm, thereby preparing the multilayer composite waterproof roll.
In the embodiment, the stirring speed is 120r/min in the preparation process of the acrylic resin glue solution; the Shore hardness of the polyimide film layer is 70 degrees; the organic silicon self-adhesive glue is a solvent type glue, the main component is organic silicon self-adhesive resin, the solid content is 35%, and the viscosity is 1-2 Pa ∙ seconds; the total thickness of the waterproof roll is 2.02mm, and the width is controlled to be 1.00 m.

Claims (6)

1. A preparation method of a multilayer composite waterproof roll is characterized by comprising the following steps:
(1) mixing 65-80 parts by mass of Butyl Acrylate (BA), 15-30 parts by mass of Methyl Methacrylate (MMA), 5-20 parts by mass of styrene, 2-4 parts by mass of Acrylic Acid (AA), 2-4 parts by mass of hydroxyethyl acrylate (HEA), 2-5 parts by mass of an emulsifier and 40 parts by mass of a solvent, and stirring and reacting at 80 ℃ for 6 hours to prepare an acrylic resin glue solution;
(2) coating the acrylic resin glue solution prepared in the step (1) on the upper side surface of a polyimide film in a rolling way, drying at the constant temperature of 50-60 ℃, and drying the acrylic resin glue solution to form an acrylic resin layer;
(3) stirring and mixing 100 parts by mass of epoxy resin, 20-30 parts by mass of polyamide curing agent, 20-30 parts by mass of polyetheramine curing agent, 1.5-4.5 parts by mass of light shielding agent, 1.5-7.5 parts by mass of plasticizer and 15-45 parts by mass of diluent for 20 minutes, coating the mixture on the upper side surface of the acrylic resin layer in the step (2), and curing the mixture at 50-60 ℃ to form an epoxy resin layer;
(4) coating the organic silicon self-adhesive glue on the lower side surface of the polyimide film layer, and drying to form an organic silicon self-adhesive bonding layer;
(5) the multilayer composite waterproof roll is formed by the epoxy resin layer, the acrylic resin layer, the polyimide film layer and the organic silicon adhesive bonding layer.
2. The preparation method of the multilayer composite waterproof roll material according to claim 1, characterized in that: in the step (1), the solvent is ethyl acetate, and the stirring speed in the reaction process is 120 r/min.
3. The preparation method of the multilayer composite waterproof roll material according to claim 1, characterized in that: in the step (2), the polyimide film is prepared by a casting method, and the Shore hardness is 70 degrees.
4. The preparation method of the multilayer composite waterproof roll material according to claim 1, characterized in that: in the step (3), the light shielding agent is carbon black with the particle size of 325 meshes, the plasticizer is epoxidized vegetable oil, and the diluent is phenyl glycidyl ether.
5. The preparation method of the multilayer composite waterproof roll material according to claim 1, characterized in that: in the step (4), the organic silicon self-adhesive glue is a solvent type glue, the main component is organic silicon self-adhesive resin, the solid content is 35%, and the viscosity is 1-2 Pa ∙ seconds.
6. The preparation method of the multilayer composite waterproof roll material according to claim 1, characterized in that: in the step (5), the thickness of the epoxy resin layer is 0.30-0.50 mm, the thickness of the acrylic resin layer is 0.35-0.50 mm, the thickness of the polyimide film layer is 0.70-0.90 mm, and the thickness of the organic silicon non-setting adhesive bonding layer is 0.10-0.12 mm; the total thickness of the waterproof roll is 1.45-2.02 mm, and the width of the waterproof roll is controlled to be 1.00 m.
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Denomination of invention: A preparation method for multi-layer composite waterproof membrane

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