CN115477815A - Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof - Google Patents

Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof Download PDF

Info

Publication number
CN115477815A
CN115477815A CN202211208309.0A CN202211208309A CN115477815A CN 115477815 A CN115477815 A CN 115477815A CN 202211208309 A CN202211208309 A CN 202211208309A CN 115477815 A CN115477815 A CN 115477815A
Authority
CN
China
Prior art keywords
parts
waterproof roll
roll material
diene monomer
propylene diene
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202211208309.0A
Other languages
Chinese (zh)
Inventor
史猛
顾伟
卫如意
陆燕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cgn Delta Jiangsu Plastics Co ltd
Original Assignee
Cgn Delta Jiangsu Plastics Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cgn Delta Jiangsu Plastics Co ltd filed Critical Cgn Delta Jiangsu Plastics Co ltd
Priority to CN202211208309.0A priority Critical patent/CN115477815A/en
Publication of CN115477815A publication Critical patent/CN115477815A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of heat-weldable high resilience dynamic vulcanization ethylene propylene diene monomer waterproof roll material and its preparation method, the material formulation includes: 15-40 parts of polypropylene resin, 10-40 parts of polyolefin elastomer, 30-60 parts of ethylene propylene diene monomer, 5-25 parts of rubber oil, 5-30 parts of filler, 0.5-5 parts of lubricant, 0.1-1 part of crosslinking agent, 0.4-4 parts of auxiliary crosslinking agent and 0.1-3 parts of antioxidant. The preparation method comprises the following steps: 1. preparing an uncrosslinked thermoplastic elastomer intermediate; 2. preparing the dynamic vulcanization thermoplastic elastomer waterproof roll material. The added polyolefin elastomer fundamentally solves the problem that the dynamic vulcanized thermoplastic elastomer waterproof coiled material is difficult to weld under the condition of ensuring high tensile strength and water impermeability of the existing dynamic vulcanized thermoplastic waterproof material, greatly improves the bonding force of the material, increases the flexibility, avoids the weakness of low temperature brittleness, and can be applied to a wider application market.

Description

Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a thermally weldable high-resilience dynamically vulcanized ethylene propylene diene monomer waterproof roll material and a preparation method thereof.
Background
In order to protect facilities such as buildings, bridges, tunnels and the like, waterproof materials are required to block moisture, rainwater and corrosive gases. The high-molecular waterproof coiled material is convenient to process, convenient to construct, light in weight and excellent in waterproof air permeability, so that the high-molecular waterproof coiled material is widely applied to facilities such as civil buildings, airports, bridges and the like.
At present, waterproof coatings, asphalt-based waterproof rolls and high polymer-based waterproof rolls (including ethylene propylene diene monomer waterproof rolls, polyvinyl chloride waterproof rolls, chlorinated polyethylene waterproof rolls and the like) are mainly used, but certain problems exist, such as flammability and explosiveness of organic solvent type waterproof coatings, environmental pollution, poor low-temperature flexibility of asphalt-based waterproof rolls, poor heat resistance and poor light resistance of polyvinyl chloride waterproof rolls and the like. Ethylene Propylene Diene Monomer (EPDM) vulcanized coiled material belongs to a nonpolar difficult-to-bond material, and the bonding problem is always limited to the popularization and application of the material. In recent years, butyl rubber adhesive tapes matched with the butyl rubber adhesive tapes are developed in China, the problems are solved, and the application development of Ethylene Propylene Diene Monomer (EPDM) vulcanized coiled materials is influenced even if the price of the butyl rubber adhesive tapes is relatively high. The polyvinyl chloride (PVC) waterproof coiled material is relatively low in price, can be subjected to body welding construction, does not have the bonding problem, but also has the fatal defect, namely the technical problem that a plasticizer is easy to migrate and seep.
In addition, the current high-molecular waterproof coiled material cannot integrate bonding, aging and high elasticity, has the disadvantage of being fragile at low temperature, and cannot be applied to northern regions with severe cold climate. The polyvinyl chloride (PVC) waterproof coiled material can be welded, but has serious degradation, environmental pollution, brittleness and cracking at low temperature, and the Ethylene Propylene Diene Monomer (EPDM) vulcanized coiled material has excellent weather resistance but has fatal welding problem.
Therefore, how to solve the above-mentioned deficiencies of the prior art is a problem to be solved by the present invention.
Disclosure of Invention
The invention aims to provide a thermally weldable high-resilience dynamically vulcanized ethylene propylene diene monomer waterproof roll material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a thermally weldable high-resilience dynamically vulcanized ethylene propylene diene monomer waterproof roll material comprises the following components in parts by weight:
15-40 parts of polypropylene resin;
10-40 parts of polyolefin elastomer;
30-60 parts of ethylene propylene diene monomer;
5-25 parts of rubber oil;
5-30 parts of a filler;
0.5-5 parts of a lubricant;
0.1-1 part of cross-linking agent;
0.4-4 parts of assistant crosslinking agent;
0.1-3 parts of an antioxidant;
the polyolefin elastomer is a copolymer of ethylene and octene, the melting temperature of the polyolefin elastomer is 50-120 ℃, the melt index is 5.0-30.0 g/10min, and the content of octene is 10-40%;
the rubber is ethylene propylene diene monomer, and the constituent monomers comprise ethylene, propylene and a crosslinking monomer;
the auxiliary crosslinking agent is one or a combination of more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, glycol triacrylate, glycol diacrylate, glycol dimethacrylate, zinc diacrylate, zinc dimethacrylate, triallyl cyanurate, triallyl isocyanurate, N-N-bismaleimide and 1, 2-polybutadiene, and the ratio of the auxiliary crosslinking agent to the crosslinking agent is 4:1.
1. the thermoplastic waterproof material prepared by combining the specific formula with the dynamic vulcanization processing technology has the advantages that the components in the formula cooperate to ensure that the elastomer has the excellent performances of the components, the polyolefin elastomer POE has large welding adhesion, excellent flexibility, the elasticity of ethylene propylene diene monomer, the strength of thermoplastic resin, a better thermal welding range, excellent waterproof performance, firm bonding, excellent elasticity and toughness at low temperature, high dimensional stability, convenience in construction and effective prolonging of the service life.
2. In the further technical scheme, the polypropylene is a copolymer of ethylene and propylene, the melt index of the polypropylene is 1.0-20.0 g/10min, and the melting temperature is 150-170 ℃.
3. In a further technical scheme, the polyolefin elastomer can be selected from one or a combination of more of POE8150, POE8003 and POE8042 in the Dow chemical industry and POE6102 in the Exon America.
4. In a further technical scheme, the rubber can be any one of EPT 3092PM of the triple well chemical, EPDM J-3080P of the Jilin chemical, EPDM 7001, EPDMM5604 and EPDM 8800 of the American Exxon, EPDM S505 and EPDM S5206F of the Korean SK.
5. In a further technical scheme, the filler is one of talcum powder, titanium dioxide, superfine calcium carbonate or kaolin.
6. The rubber oil is one or a combination of several of white oil, paraffin oil and naphthenic oil, and the kinematic viscosity of the rubber oil is 40-400 mm at 40 DEG C 2 The kinematic viscosity is between 10 and 50mm at 100 DEG C 2 Between/s, the evaporation loss is not more than 0.6%. The lubricant is one or a combination of more of silicone, silicone oil, erucamide, stearate, PE wax and paraffin.
7. In a further technical scheme, the cross-linking agent is organic peroxide, and the organic peroxide is one of 2, 5-bis (tert-butylperoxy) -2, 5-dimethyl-3-hexyne, 2, 5-bis (tert-butylperoxy) -2, 5-dimethylhexane, dicumyl peroxide, tert-butylperoxyisopropyl carbonate, tert-butylcumyl peroxide and di- (tert-butylperoxyisopropyl) benzene.
8. According to a further technical scheme, the antioxidant is any one of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, N ' -bis- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, 2' -methylenebis (4-methyl-6-tert-butylphenol), 4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine and N-hexadecyl 3, 5-di-tert-butyl-4-hydroxybenzoic acid.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a heat-weldable high-resilience dynamically vulcanized thermoplastic elastomer waterproof roll material comprises the following steps:
step one, preparation of an intermediate: mixing polypropylene resin, polyolefin elastomer, ethylene propylene diene monomer, filler, rubber oil, lubricant and antioxidant in parts by weight, putting the mixture into an internal mixer, mixing the mixture at the mixing temperature of 170-190 ℃ for 10-30 min, uniformly blending the rubber and the thermoplastic resin, and then feeding the mixture into a single screw at the same set temperature as the mixing temperature for granulation to obtain an uncrosslinked thermoplastic elastomer intermediate;
step two, crosslinking reaction: the thermoplastic elastomer intermediate, the auxiliary crosslinking agent and the crosslinking agent are prepared according to the parts by weight, and are extruded and granulated on a double-screw extruder by adopting a dynamic vulcanization process, wherein the vulcanization temperature is 160-200 ℃, the rotating speed is 200-500 r/min, and the thermoplastic elastomer intermediate, the auxiliary crosslinking agent and the crosslinking agent are subjected to crosslinking reaction, so that the dynamic vulcanized thermoplastic elastomer waterproof roll material is obtained.
1. In the technical scheme, the dynamic vulcanization process is a process of crosslinking, shearing and crushing the elastomer in a double-screw extruder, is a dynamic process, can ensure that the material can be fully crosslinked and uniformly dispersed in a proper time through a special screw structure of the double-screw extruder, and has a conventional processing technology, which can be known by a person skilled in the art.
2. By adopting the technical scheme, the intermediate is prepared firstly and then is crosslinked, unvulcanized raw rubber in the intermediate and unvulcanized thermoplastic resin are melted and blended in a high-temperature and high-shear double screw (the parameters of the adopted double screw extruder are that the length-diameter ratio is 38-58, the rotating speed is 200-500 r/min, and the temperature of each area of the screw can be stably kept between 120-200 ℃), and meanwhile, under the action of a crosslinking agent, the rubber is completely subjected to crosslinking reaction and is crushed into micron-sized vulcanized rubber particles which are uniformly dispersed in a resin phase, so that the structure is very stable, the performance of the elastomer is greatly improved, and the hot-weldable high-resilience dynamic vulcanized thermoplastic elastomer waterproof roll material is obtained. The prepared high-resilience dynamic vulcanization thermoplastic elastomer waterproof roll material capable of being thermally welded has the excellent performances of all components, has excellent weldability, excellent low-temperature flexibility, very high elasticity and tensile strength, is firmly bonded with a TPV (thermoplastic vulcanized rubber) waterproof roll material, can stand wind, blow and rain, has sufficient guarantee with the airtightness of an inner wall, can effectively isolate contact of rainwater gas and the inner wall, has good low-temperature flexibility, can be constructed and applied in regions with lower temperature, enlarges the application region range of the product, can utilize white reflected sunlight of the roll material when being used as a roofing material, reduces the absorption of ultraviolet rays, prolongs the service life, and has positive significance for solving the problems of most of the existing waterproof materials.
3. According to a further technical scheme, the thermoplastic elastomer intermediate comprises polypropylene, a polyolefin elastomer, ethylene propylene diene monomer, a filler, rubber oil, an antioxidant and a lubricant; the weight percentage of the ethylene propylene diene monomer in the matrix is 30-60%, the weight percentage of the polypropylene resin is 15-40%, the weight percentage of the polyolefin elastomer is 10-40%, the weight percentage of the filler is 5-30%, the weight percentage of the rubber oil is 5-25%, the weight percentage of the antioxidant is 0.1-3%, and the weight percentage of the lubricant is 0.5-5%.
4. The further technical scheme is that the Mooney viscosity ML (1 + 4) of the rubber is between 40 and 70 ℃ at 125 ℃, the ethylene content is between 50 and 70 percent, the crosslinking monomer content is between 2 and 5 percent, and the crosslinking monomer is ethylidene norbornene.
The working principle and the advantages of the invention are as follows:
1. the TPV thermoplastic elastomer is prepared by taking polypropylene and ethylene propylene diene monomer as base materials and adopting dynamic vulcanization, has high strength and excellent elasticity, can effectively solve the problems of low elongation, easy leakage, poor aging performance and the like of the traditional waterproof roll, and meanwhile, the waterproof roll material can be recycled and is an environment-friendly material.
2. The ethylene-octene copolymer POE added in the invention fundamentally solves the problem that the dynamic vulcanization thermoplastic elastomer waterproof coiled material is difficult to weld, greatly improves the bonding force of the material and enhances the use safety; in addition, the elastic material contained in the material component endows the waterproof roll material product with excellent elasticity and toughness and can resist severe cold weather.
3. The waterproof thermoplastic dynamic vulcanized elastomer prepared by the invention has the advantages of good wear resistance, strong ultraviolet resistance, smooth surface, high reflectivity and pollution resistance, can replace the application of the traditional waterproof material in various fields, and can generate great promotion effect on the development of the fields of environmental protection, building energy conservation and the like.
4. The invention adds proper amount of assistant cross-linking agent, matches with cross-linking agent, makes the ethylene propylene diene monomer fully cross-linked, improves the cross-linking degree, avoids the degradation of polypropylene resin, fully improves the elastic recovery rate of thermoplastic elastomer waterproof material, and can be used in roofs, underground and bridges with complex structures.
Detailed Description
The invention is further described below with reference to examples:
the embodiment is as follows: the present disclosure will be described in detail below, and it is to be understood that variations and modifications can be made by the techniques taught in the present disclosure without departing from the spirit and scope of the present disclosure by those skilled in the art after understanding the present disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. The singular forms "a", "an", "the" and "the", as used herein, also include the plural forms. As used herein, the terms "comprising," "including," "having," and the like are open-ended terms that mean including but not limited to.
As used herein, the term (terms), unless otherwise indicated, shall generally have the ordinary meaning as commonly understood by one of ordinary skill in the art, in this written description and in the claims. Certain words used to describe the disclosure are discussed below or elsewhere in this specification to provide additional guidance to those skilled in the art in describing the disclosure.
The invention discloses a preparation method of a hot-weldable high-resilience dynamically vulcanized ethylene propylene diene monomer waterproof roll material, which specifically comprises the following steps:
(1) The preparation method comprises the steps of mixing polypropylene resin, polyolefin elastomer, ethylene propylene diene monomer, filler, rubber oil, lubricant and antioxidant in parts by weight, putting the mixture into an internal mixer, mixing the mixture at the mixing temperature of 170-190 ℃ for 10-30 min, uniformly mixing the rubber and the thermoplastic resin, and then feeding the mixture into a single screw at the set temperature same as the mixing temperature for granulation to obtain the uncrosslinked thermoplastic elastomer intermediate.
(2) Then the thermoplastic elastomer intermediate, the assistant cross-linking agent and the cross-linking agent are prepared according to the parts by weight, and the mixture is extruded and granulated on a double-screw extruder by adopting a dynamic vulcanization process, wherein the vulcanization temperature is 160-200 ℃, and the rotating speed is 200-500 r/min. The dynamic vulcanization process comprises the steps of melting and blending unvulcanized crude rubber in a thermoplastic elastomer intermediate and unvulcanized thermoplastic resin in a high-temperature and high-shear twin-screw, and simultaneously, completely performing a crosslinking reaction on the rubber under the action of a crosslinking agent, crushing the rubber into micron-sized vulcanized rubber particles, uniformly dispersing the micron-sized vulcanized rubber particles in a resin phase, wherein the structure is very stable, the performance of the elastomer can be greatly improved, and finally the dynamically vulcanized thermoplastic elastomer waterproof material is obtained.
The following examples 1 to 5 and comparative examples all adopt the above-mentioned preparation methods except for the formulation of the raw materials.
Example 1: adding 35 parts of polypropylene resin, 15 parts of polyolefin elastomer, 60 parts of ethylene propylene diene monomer, 15 parts of filler, 5 parts of rubber oil, 2 parts of lubricant and 1 part of antioxidant into an internal mixer, carrying out internal mixing for 20min at the internal mixing temperature of 190 ℃, and then adding into a single-screw extruder to obtain intermediate particles; and uniformly mixing the prepared intermediate particles, 0.5 part of cross-linking agent and 2 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder. Extruding finished product particles at the temperature of 120-200 ℃ and the rotating speed of 280-400 r/min in each zone of the extruder screw to obtain a weldable high-resilience dynamic vulcanization thermoplastic elastomer waterproof material; the results of the sample property test are shown in Table 2.
Example 2: adding 30 parts of polypropylene resin, 20 parts of polyolefin elastomer, 50 parts of ethylene propylene diene monomer, 12 parts of filler, 7 parts of rubber oil, 2 parts of lubricant and 0.5 part of antioxidant into an internal mixer, internally mixing for 20min at the temperature of 190 ℃, and then adding into a single-screw extruder to obtain intermediate particles; and uniformly mixing the prepared intermediate particles, 0.5 part of cross-linking agent and 2 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder. The temperature of each zone of the extruder screw is 120-200 ℃, and the rotating speed is 280-400 r/min; extruding finished granules to obtain the dynamic vulcanization thermoplastic elastomer waterproof material; the results of the sample property test are shown in Table 2.
Example 3: adding 30 parts of polypropylene resin, 25 parts of polyolefin elastomer, 50 parts of ethylene propylene diene monomer, 10 parts of filler, 9 parts of rubber oil, 2 parts of lubricant and 0.3 part of antioxidant into an internal mixer, internally mixing for 20min at the temperature of 190 ℃, and then adding into a single-screw extruder to form intermediate particles; and (3) uniformly mixing the prepared intermediate particles, 0.5 part of cross-linking agent and 2 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder. Extruding finished granules at the temperature of 120-200 ℃ and the rotating speed of 280-400 r/min in each zone of a screw of the extruder to obtain the dynamically vulcanized thermoplastic elastomer waterproof material; the results of the sample property test are shown in Table 2.
Example 4: adding 30 parts of polypropylene resin, 30 parts of polyolefin elastomer, 45 parts of ethylene propylene diene monomer, 10 parts of filler, 10 parts of rubber oil, 1.5 parts of lubricant and 0.3 part of antioxidant into an internal mixer, internally mixing for 20min at the temperature of 190 ℃, and then adding into a single-screw extruder to obtain intermediate particles; and uniformly mixing the prepared intermediate particles, 0.5 part of cross-linking agent and 2 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder. Extruding finished granules at the temperature of 120-200 ℃ and the rotating speed of 280-400 r/min in each zone of a screw of the extruder to obtain the dynamically vulcanized thermoplastic elastomer waterproof material; the results of the sample property test are shown in Table 2.
Example 5: 30 parts of polypropylene resin, 35 parts of polyolefin elastomer, 45 parts of ethylene propylene diene monomer, 8 parts of filler, 8 parts of rubber oil, 1.5 parts of lubricant and 0.2 part of antioxidant are added into an internal mixer, and the mixture is internally mixed for 20min at the temperature of 190 ℃, and then added into a single-screw extruder to form intermediate particles. And uniformly mixing the prepared intermediate particles, 0.5 part of cross-linking agent and 2 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder. Extruding finished granules at the temperature of 120-200 ℃ and the rotating speed of 280-400 r/min in each zone of a screw of an extruder to obtain the dynamic vulcanization thermoplastic elastomer waterproof material; the results of the sample property test are shown in Table 2.
Comparative example: the polyolefin elastomer was not added, and otherwise, as in example 1, specifically, 35 parts of polypropylene resin, 0 part of polyolefin elastomer, 60 parts of ethylene propylene diene monomer, 15 parts of filler, 5 parts of rubber oil, 2 parts of lubricant and 1 part of antioxidant were added to an internal mixer, and internal mixing was carried out for 20min at an internal mixing temperature of 190 ℃, followed by addition to a single-screw extruder to give intermediate particles. And uniformly mixing the prepared intermediate particles, 0.5 part of cross-linking agent and 2 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder. Extruding finished granules at the temperature of 120-200 ℃ and the rotating speed of 280-400 r/min in each zone of a screw of an extruder to obtain the dynamic vulcanization thermoplastic elastomer waterproof material; the results of the sample property test are shown in Table 2.
Wherein, the concrete components of the examples 1 to 5 and the comparative example are shown in the following table 1;
table 1: raw material formulations (unit: parts by weight) of examples 1 to 5 and comparative example
Raw materials Example 1 Example 2 Example 3 Example 4 Example 5 Comparative example
Polypropylene resin 35 30 30 30 30 35
Polyolefin elastomer 15 20 25 30 35 0
Ethylene propylene diene monomer 60 50 50 45 45 60
Rubber oil 5 7 9 10 8 5
Filler material 15 12 10 10 8 15
Lubricant agent 2 2 2 1.5 1.5 2
Crosslinking agent 0.5 0.5 0.5 0.5 0.5 0.5
Auxiliary crosslinking agent 2 2 2 2 2 2
Antioxidant agent 1 0.5 0.3 0.3 0.2 1
The raw materials in the above examples 1 to 5 and comparative examples were selected as follows:
(1) Rubber oil: white oil 4010; ethylene propylene diene monomer: EPDM J-3080P, jilin chemical.
(2) Polyolefin elastomer: POE8150 of dow chemical.
(3) Antioxidant: the combination of antioxidant 3450 and antioxidant 2908 in a ratio of 1:1.
(4) A crosslinking agent: 2, 5-bis (tert-butylperoxy) -2, 5-dimethyl-3-hexyne.
(5) Filling: nano calcium carbonate.
(6) Lubricant: paraffin wax and silicone in a ratio of 2:1.
(7) Auxiliary crosslinking agent: N-N-bismaleimide.
(8) Setting the temperature of the screw: the temperatures of the first two zones are respectively 120 ℃ and 140 ℃, and the temperature of the rear zone is set between 160 ℃ and 200 ℃.
Table 2: results of Performance test of the waterproof roll materials prepared in examples 1 to 5 and comparative example
Figure BDA0003873635810000071
Figure BDA0003873635810000081
From the performance test results in table 2, it can be seen that the sample of example 5 has the largest seam peel strength, and the comparative example has the smallest seam peel strength, because the polyolefin elastomer POE ratio is increased, the welding performance of the material is improved, and the flexibility of the material is enhanced by adding the polyolefin elastomer POE, and the elongation is gradually increased along with the increase of the ratio. The addition of a proper amount of POE can improve the elastic recovery rate of the material, but the addition of excessive POE can affect the crosslinking degree of the ethylene propylene diene monomer, damage the unique sea-island structure of the material, and cause the elastic recovery rate of the material to be reduced, and the phenomenon of increasing and then reducing is shown, so that the addition of a proper amount of POE is needed. As can be seen from Table 2, it is suitable to add 25 parts of POE.
In conclusion, the formula is optimized, the adhesion and resilience of the elastomer coiled material are improved, the weldable, high-resilience and recyclable dynamic vulcanized thermoplastic elastomer waterproof material is developed, and the aim is to achieve safe storage, aging resistance, easy construction, easy processing, environmental protection and recycling.
The invention adds proper amount of assistant cross-linking agent, matches with cross-linking agent, makes the ethylene propylene diene monomer fully cross-linked, improves the cross-linking degree, avoids the degradation of polypropylene resin, fully improves the elastic recovery rate of thermoplastic elastomer waterproof material, and can be used in roofs, underground and bridges with complex structures.
The above embodiments are only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the protection scope of the present invention by this means. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (9)

1. A hot-weldable high-resilience dynamically vulcanized ethylene propylene diene monomer waterproof roll material is characterized in that: the raw materials comprise the following components in parts by weight:
15-40 parts of polypropylene resin;
10-40 parts of a polyolefin elastomer;
30-60 parts of ethylene propylene diene monomer;
5 to 25 parts of rubber oil;
5-30 parts of a filler;
0.5 to 5 parts of a lubricant;
0.1 to 1 part of a crosslinking agent;
0.4 to 4 parts of auxiliary crosslinking agent;
0.1 to 3 parts of antioxidant;
the polyolefin elastomer is an ethylene-octene copolymer, the melting temperature of the polyolefin elastomer is 50-120 ℃, the melt index of the polyolefin elastomer is 5.0-30.0 g/10min, and the content of octene is 10-40%;
the rubber is ethylene propylene diene monomer, and the constituent monomers comprise ethylene, propylene and a crosslinking monomer;
the auxiliary crosslinking agent is one or a combination of more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, glycol triacrylate, glycol diacrylate, glycol dimethacrylate, zinc diacrylate, zinc dimethacrylate, triallyl cyanurate, triallyl isocyanurate, N-N-bismaleimide and 1, 2-polybutadiene, and the ratio of the auxiliary crosslinking agent to the crosslinking agent is 4:1.
2. the waterproof roll material according to claim 1, wherein: the polypropylene is a copolymer of ethylene and propylene, the melt index of the polypropylene is 1.0-20.0 g/10min, and the melt temperature is 150-170 ℃.
3. The waterproof roll material according to claim 1, wherein: the filler is one of talcum powder, titanium dioxide, superfine calcium carbonate or kaolin.
4. The waterproof roll material according to claim 1, wherein: the rubber oil is one or a combination of several of white oil, paraffin oil and naphthenic oil; the lubricant is one or a combination of more of silicone, silicone oil, erucamide, stearate, PE wax and paraffin.
5. The waterproof roll material according to claim 1, wherein: the crosslinking agent is organic peroxide, and the organic peroxide is one of 2, 5-bis (tert-butylperoxy) -2, 5-dimethyl-3-hexyne, 2, 5-bis (tert-butylperoxy) -2, 5-dimethylhexane, dicumyl peroxide, tert-butylperoxy isopropyl carbonate, tert-butylcumyl peroxide and di- (tert-butylperoxyisopropyl) benzene.
6. The waterproof roll material according to claim 1, wherein: the antioxidant is any one of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N ' -bis- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, 2' -methylenebis (4-methyl-6-tert-butylphenol), 4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine and N-hexadecyl 3, 5-di-tert-butyl-4-hydroxybenzoic acid.
7. A method for preparing a thermally weldable high-resilience dynamically vulcanized thermoplastic elastomer waterproof roll material, which is used for preparing the waterproof roll material of claims 1 to 6; the method is characterized in that: the method comprises the following steps:
step one, preparation of an intermediate: mixing polypropylene resin, polyolefin elastomer, ethylene propylene diene monomer, filler, rubber oil, lubricant and antioxidant in parts by weight, putting the mixture into an internal mixer, mixing the mixture at the mixing temperature of 170 to 190 ℃ for 10 to 30min to uniformly blend the rubber and the thermoplastic resin, and then feeding the mixture into a single screw at the same set temperature as the mixing temperature for granulation to obtain an uncrosslinked thermoplastic elastomer intermediate;
step two, crosslinking reaction: preparing a thermoplastic elastomer intermediate, an auxiliary crosslinking agent and a crosslinking agent in parts by weight, extruding and granulating on a double-screw extruder by adopting a dynamic vulcanization process, wherein the vulcanization temperature is 160-200 ℃, the rotating speed is 200-500r/min, and the thermoplastic elastomer intermediate, the auxiliary crosslinking agent and the crosslinking agent are subjected to a crosslinking reaction, so that the dynamically vulcanized thermoplastic elastomer waterproof roll material is obtained.
8. The method for preparing a waterproof roll material according to claim 7, characterized in that: the thermoplastic elastomer intermediate comprises polypropylene, a polyolefin elastomer, ethylene propylene diene monomer, a filler, rubber oil, an antioxidant and a lubricant; the weight percentage of the ethylene propylene diene monomer in the matrix is 30 to 60 percent, the weight percentage of the polypropylene resin is 15 to 40 percent, the weight percentage of the polyolefin elastomer is 10 to 40 percent, the weight percentage of the filler is 5 to 30 percent, the weight percentage of the rubber oil is 5 to 25 percent, the weight percentage of the antioxidant is 0.1 to 3 percent, and the weight percentage of the lubricant is 0.5 to 5 percent.
9. The method for preparing a waterproof roll material according to claim 8, wherein: the Mooney viscosity ML (1 + 4) of the ethylene propylene diene monomer is between 40 and 70 at 125 ℃, the ethylene content is between 50 and 70 percent, the crosslinking monomer content is between 2 and 5 percent, and the crosslinking monomer is ethylidene norbornene.
CN202211208309.0A 2022-09-30 2022-09-30 Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof Pending CN115477815A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211208309.0A CN115477815A (en) 2022-09-30 2022-09-30 Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211208309.0A CN115477815A (en) 2022-09-30 2022-09-30 Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN115477815A true CN115477815A (en) 2022-12-16

Family

ID=84393833

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211208309.0A Pending CN115477815A (en) 2022-09-30 2022-09-30 Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115477815A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115678149A (en) * 2022-12-30 2023-02-03 润海铁建科技发展有限公司 High-molecular waterproof coiled material and production method and application thereof
CN116731439A (en) * 2023-06-12 2023-09-12 惠州麦丰密封科技有限公司 High-temperature-resistant modified ethylene propylene diene monomer rubber composition and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101440183A (en) * 2007-11-19 2009-05-27 上海日之升新技术发展有限公司 High oil resistance dynamic vulcanization thermoplastic elastomer material and preparation thereof
CN101486892A (en) * 2009-02-11 2009-07-22 曹天志 Thermal weld EPT rubber water-proof coiled material
CN110437549A (en) * 2019-09-06 2019-11-12 安徽中鼎橡塑制品有限公司 A kind of peroxide cure thermoplastic elastic material and preparation method thereof
CN110964265A (en) * 2019-11-15 2020-04-07 中广核三角洲集团(苏州)特威塑胶有限公司 Dynamic vulcanization thermoplastic elastomer waterproof material and preparation method thereof
CN112694680A (en) * 2020-12-23 2021-04-23 广州大禹防漏技术开发有限公司 Polyolefin elastomer waterproof coiled material and preparation method thereof
CN113799354A (en) * 2021-08-23 2021-12-17 昆山科顺防水材料有限公司 Rubber waterproof coiled material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101440183A (en) * 2007-11-19 2009-05-27 上海日之升新技术发展有限公司 High oil resistance dynamic vulcanization thermoplastic elastomer material and preparation thereof
CN101486892A (en) * 2009-02-11 2009-07-22 曹天志 Thermal weld EPT rubber water-proof coiled material
CN110437549A (en) * 2019-09-06 2019-11-12 安徽中鼎橡塑制品有限公司 A kind of peroxide cure thermoplastic elastic material and preparation method thereof
CN110964265A (en) * 2019-11-15 2020-04-07 中广核三角洲集团(苏州)特威塑胶有限公司 Dynamic vulcanization thermoplastic elastomer waterproof material and preparation method thereof
CN112694680A (en) * 2020-12-23 2021-04-23 广州大禹防漏技术开发有限公司 Polyolefin elastomer waterproof coiled material and preparation method thereof
CN113799354A (en) * 2021-08-23 2021-12-17 昆山科顺防水材料有限公司 Rubber waterproof coiled material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115678149A (en) * 2022-12-30 2023-02-03 润海铁建科技发展有限公司 High-molecular waterproof coiled material and production method and application thereof
CN115678149B (en) * 2022-12-30 2023-03-10 润海铁建科技发展有限公司 High-molecular waterproof coiled material and production method and application thereof
CN116731439A (en) * 2023-06-12 2023-09-12 惠州麦丰密封科技有限公司 High-temperature-resistant modified ethylene propylene diene monomer rubber composition and preparation method thereof

Similar Documents

Publication Publication Date Title
CN115477815A (en) Hot-weldable high-resilience dynamically-vulcanized ethylene propylene diene monomer waterproof roll material and preparation method thereof
CN110964265A (en) Dynamic vulcanization thermoplastic elastomer waterproof material and preparation method thereof
CN103554629B (en) A kind of TPO waterproof roll and production technique thereof
US5266626A (en) Thermoplastic elastomer based on an ethylene/α-olefin copolymer and on polynorbornene
CA1265883A (en) Thermoplastic elastomer composition
CA1277055C (en) Asphalt elastomeric blends
US4113804A (en) Compositions comprising polybutene EPDM and polyolefin
JPS60116431A (en) Joining method of waterproof sheet
US20030113534A1 (en) Adhesive tape for outdoor use
US5177139A (en) Moulding material made from elastomeric polyolefin rubbers, polyethylenes and/or ethylene copolymers and additives; and its use for elastic clamp-proof courses
CN111925661A (en) Butyl rubber/asphalt waterproof material and preparation method thereof
CN104745117A (en) Self-adhesive reactive ethylene-octene copolymer composite waterproof coiled material and production method thereof
CN109721861B (en) Photosensitive self-crosslinking ethylene propylene diene monomer waterproof roll and preparation method thereof
CN113799354A (en) Rubber waterproof coiled material and preparation method thereof
CN112724850B (en) Composite adhesive tape and preparation method thereof
CA2051132A1 (en) Waterproof rubber sheet
JP2006265367A (en) Waterproof sheet
JPS5851121A (en) Heat-shrinkable film or sheet
EP1328572B9 (en) Crosslinked heat shrinkable polypropylene compositions
CN104387681A (en) Aging-resistant weather-resistant waterproof TPO material and preparation method thereof
CN117362843A (en) TPO waterproof roll material meeting B2-level flame retardance and 5000h aging resistance and preparation method thereof
JP3053233B2 (en) Radiation resistant composition
JP3196453B2 (en) Method for producing thermoplastic elastomer composition
JPH0657059A (en) Water-absorptive resin composition
JPS60231748A (en) Waterproof sheet

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination