CN113652031A - Low-compression permanent deformation low-temperature-resistant EPDM (ethylene-propylene-diene monomer) sealing strip as well as preparation method and application thereof - Google Patents

Low-compression permanent deformation low-temperature-resistant EPDM (ethylene-propylene-diene monomer) sealing strip as well as preparation method and application thereof Download PDF

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CN113652031A
CN113652031A CN202110959312.5A CN202110959312A CN113652031A CN 113652031 A CN113652031 A CN 113652031A CN 202110959312 A CN202110959312 A CN 202110959312A CN 113652031 A CN113652031 A CN 113652031A
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low
accelerator
sealing strip
temperature
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余强
许月能
林腾飞
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Fuzhou Fuqiang Precision Co ltd
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    • 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
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • 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
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K

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

Abstract

The invention belongs to the field of rubber sealing strips, and particularly relates to a low-compression permanent deformation low-temperature-resistant EPDM sealing strip and a preparation method and application thereof. The low-compression permanent-deformation low-temperature-resistant EPDM sealing strip comprises the following raw materials in parts by weight: 100 parts of ethylene propylene diene monomer, 20-50 parts of carbon black, 5-10 parts of modified boehmite, 2.0-5.0 parts of tetrabutyl titanate, 0.5-1.0 part of sodium citrate, 3.0-5.0 parts of zinc oxide, 1.0-2.0 parts of stearic acid, 60003.0-5.0 parts of polyethylene glycol, 30-50 parts of softening plasticizer, 1.0 part of accelerator MBT-800.5, 1.0 part of accelerator CBS-801.5-2.0 parts of accelerator ETU-800.5, 1.0 part of accelerator TMTD-800.5, 1.5 parts of anti-aging agent 10101.0 and 1.5 parts of vulcanizing agent S-801.0. The low-compression permanent-deformation low-temperature-resistant EPDM sealing strip and the preparation method thereof have the advantages that the preparation method is simple in process, the materials are easy to obtain, the method is suitable for industrial production, and the prepared EPDM sealing strip is low in compression permanent deformation, good in low-temperature resistance and excellent in sealing performance.

Description

Low-compression permanent deformation low-temperature-resistant EPDM (ethylene-propylene-diene monomer) sealing strip as well as preparation method and application thereof
Technical Field
The invention belongs to the field of rubber sealing strips, and particularly relates to a low-compression permanent deformation low-temperature-resistant EPDM sealing strip and a preparation method and application thereof.
Background
EPDM (ethylene Propylene monomer), an ethylene Propylene Diene monomer, is a copolymer of ethylene, Propylene and a minor amount of a non-conjugated Diene. The main chain of the composite material consists of chemically stable saturated hydrocarbon, and only contains unsaturated double bonds in the side chain, so that the composite material has excellent ozone resistance, heat resistance, weather resistance and other aging resistance, and can be widely used in the fields of automobile parts, waterproof materials for buildings, wire and cable sheaths, heat-resistant rubber tubes, adhesive tapes, automobile sealing parts and the like.
The automobile sealing strip is arranged on a metal plate around an automobile door and mainly plays roles in sealing, dust prevention, water prevention, decoration and the like. Under the car door closed condition, sealing effect realizes through the laminating between sealing strip and the door frame, can prevent that harmful substance such as outside wind, rain and dust from invading in the car to reducible car is in the vibration that produces of in-process positions such as door and window of going, with cleanness and travelling comfort and exquisite perception in keeping the car. Meanwhile, the arrangement of the sealing strip can also improve the working environment of the door part device, prolong the service life of the door part working part, but the elasticity of the existing sealing rubber strip is lost in a low-temperature environment, and the problems of difficult lifting and large door closing force of the automobile glass chute occur.
The properties of EPDM make it attractive in the area of passenger car weatherstrips. According to incomplete statistics, EPDM consumes about 80 million tons worldwide per year as a passenger car weatherstrip. However, with the social progress, people have deeper understanding on the functions of the sealing strip, and the traditional requirements such as air tightness and water tightness do not accord with the current concepts of energy conservation, environmental protection and safety. At present, the performances of the sealing strip of the passenger car in the aspects of low temperature resistance, high rebound resilience, flame retardance and the like become the focus of attention of foreign car enterprises.
More information related to the above can also be found in the following documents. For example, in the Chinese invention patent application CN106496808A, the antifriction and wear resistance of EPDM is improved by adding modified nano graphite powder, and a high-durability mildew-proof automobile sealing strip rubber material is prepared. Chinese patent application CN111295304A forms a sealing strip from an extruded core part made of a thermoplastic material and an extruded sealing section made of an elastomeric material connected to the core part. The sealing section of the sealing strip is made of vulcanized elastomeric material, in particular EPDM, and the core part or a core part section, which is connected to the remainder of the core part, is extruded onto the sealing section while being connected to the vulcanized sealing section, but the sealing strip is prone to problems such as poor yield due to technical maturity and unstable handling of the equipment. In the process of implementing the invention, the inventor finds that the following problems exist in the prior art: at present, although numerous enterprises for producing sealing strips of passenger cars in China exist, the sealing strip processing technology is generally inexperienced, and the sealing strips of doors and windows are not understood, so that the quality level of the sealing strips is not high as a whole. Common problems in the sealing strip industry of domestic passenger vehicles include large size fluctuation, poor comprehensive mechanical physical properties, poor high and low temperature resistance and the like. The functionalization and composite extrusion are the main development trend in the sealing strip industry in the future.
Therefore, in order to meet the current and future market demands, it is necessary to develop a sealing tape of EPDM having sufficiently low compression set and excellent low-temperature resistance.
Disclosure of Invention
In view of the above-mentioned problems of the prior art, it is desirable to provide an EPDM weatherstrip having a low compression set and excellent low-temperature resistance.
To achieve the above object, in a first aspect of the present invention, the inventors provide a low compression set low temperature resistant EPDM weatherstrip comprising, in parts by weight: 100 parts of ethylene propylene diene monomer, 20-50 parts of carbon black, 5-10 parts of modified boehmite, 2.0-5.0 parts of tetrabutyl titanate, 0.5-1.0 part of sodium citrate, 3.0-5.0 parts of zinc oxide, 1.0-2.0 parts of stearic acid, 3.0-5.0 parts of polyethylene glycol, 30-50 parts of softening plasticizer, 0.5-1.0 part of first accelerator, 1.5-2.0 parts of second accelerator, 0.5-1.0 part of third accelerator, 0.5-1.0 part of fourth accelerator, 1.0-1.5 parts of anti-aging agent and 1.0-1.5 parts of vulcanizing agent.
In the invention, boehmite is an inorganic filler with two-dimensional lamellar, has small particle size, large specific surface area and good compression permanent deformation resistance, and can resist crack growth by forming good interface combination with a rubber matrix. The boehmite has low price, larger rigidity and good thermal stability. And by compounding a silane coupling agent, sodium citrate and tetrabutyl titanate, the boehmite is subjected to surface modification, so that the boehmite can be uniformly dispersed in the EPDM rubber matrix and forms good interface combination with the rubber matrix, and the low-temperature-resistant and low-compression permanent deformation performance of the sealing strip is improved.
Sodium citrate and tetrabutyl titanate are used as surface modifiers (modifiers) of boehmite, and have excellent retardation performance. The boehmite surface is further functionalized by modifying and modifying the boehmite surface, so that the boehmite is prevented from agglomerating in a rubber matrix and can be uniformly dispersed, and the boehmite modified boehmite has good compatibility with the rubber matrix and forms good interface combination.
Polyethylene glycol 6000 is used as an additive in the industrial production of vulcanized rubber, so that the wettability and plastic deformation of the rubber and plastic product are improved, the driving force consumption in the production process is reduced, and the service life of the rubber and plastic product is prolonged.
Zinc oxide and stearic acid are used as active agents. The activator has the effect of fully playing the role of the accelerator, thereby activating the vulcanization reaction; and simultaneously, the crosslinking degree and the heat resistance of the vulcanized rubber can be improved. The zinc stearate can be generated by mixing the zinc oxide and the stearic acid, so that the modified boehmite can be more easily dispersed in a rubber system, and then the modified boehmite reacts with an accelerator to generate a zinc salt complex to promote rubber vulcanization.
The vulcanization accelerator, which can be called accelerator for short, is used for accelerating the vulcanization speed, shortening the vulcanization time, reducing the vulcanization temperature, reducing the consumption of vulcanizing agent and simultaneously improving the physical and mechanical properties of vulcanized rubber during rubber vulcanization. The first accelerator is MBT-80. In general, the powdery accelerator MBT is liable to fly and adhere to equipment, and is not liable to be uniformly dispersed during kneading. However, the MBT-80 is easy to prepare and mix, does not cake under normal storage conditions, has good fluidity, does not fly dust, does not cause feeding loss, is easy to eat in various rubber materials and is uniformly dispersed, and the activity of the effective component MBT is ensured. MBT-80 has a broad cure leveling property and a high scorch tendency, and when used as a main accelerator, zinc oxide and stearic acid are required for activation.
The second accelerator is a mixture of CBS-80, 80% of N-cyclohexyl-2-benzothiazole sulfonamide, 20% of polymer and a dispersing agent, is a post-effect accelerator for sulfur vulcanization of rubber, and has the characteristics of excellent scorch resistance and short vulcanization time. It is especially suitable for tyre and damping product and can raise the mechanical performance of the product. The third accelerator is a mixture of ETU-80, 80% of 1, 2-ethylene thiourea, 20% of polymer and a dispersant, is an excellent accelerator for rubber, and has a good accelerating effect on EPDM. The metal oxide is suitable for being used as a vulcanizing agent, and is easy to disperse in a sizing material, and pollution and discoloration are avoided. The fourth accelerator is a mixture of TMTD-80, 80% tetramethylthiuram disulfide, 20% polymer and dispersant. The product can be used as an overspeed vulcanization accelerator in the rubber industry, a vulcanizing agent for low-sulfur or sulfur-free vulcanization, a thiazole accelerator is often used together with the vulcanization accelerator, other accelerators can be used together as an accelerator for continuous rubber materials, free sulfur is slowly decomposed at the temperature of more than 100 ℃, so the product can be used as a vulcanizing agent, and the aging resistance and the heat resistance of the product are good.
The anti-aging agent is a commercial anti-aging agent 1010. The anti-aging agent 1010 can effectively prevent thermal oxidation degradation of rubber in a long-term aging process, is an efficient processing stabilizer, and can improve the color change resistance of the rubber under high-temperature processing conditions.
The vulcanizing agent is commercially available vulcanizing agent S-80. The S-80 has excellent dispersibility, can be quickly mixed with rubber materials, and has the advantages of high dispersibility, easy addition and shortened mixing time. In addition, the S-80 is non-toxic and pollution-free, is suitable for automatic weighing, and meets the requirements of material safety and environmental protection.
Preferably, the method for preparing the modified boehmite comprises the steps of:
adding boehmite into deionized water for dispersion to obtain a boehmite solution;
adding an organic modifier into the boehmite solution according to the mass ratio of the organic modifier to the boehmite solution of 5:100 to carry out organic modification reaction to obtain an organically modified boehmite solution;
and filtering the organic modified boehmite solution by a Buchner funnel, drying at the constant temperature of a forced air drying oven at 60 ℃, and crushing by a ball mill to obtain the modified boehmite.
The organic modifier adopted by the invention can modify the boehmite surface, organically modify the boehmite surface, make the boehmite surface complementarily combined according to space distance occupation, and easily form an interface combined with a rubber matrix.
More preferably, the organic modifier is obtained by compounding a silane coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and 3- (methacryloyloxy) propyl trimethoxy silane according to the mass ratio of 2: 3. Through the compounding of the two coupling agents, the boehmite can be subjected to surface modification, so that the boehmite and the EPDM rubber matrix form good interface combination, the low-temperature resistance of the sealing strip is improved, and the sealing strip is ensured to have lower compression permanent deformation.
Preferably, the grade of the ethylene propylene diene monomer is 4045M. The ethylene propylene diene monomer 4045M is an ethylene propylene diene monomer with low Mooney viscosity, high ethylene content and low third monomer content synthesized by adopting metallocene catalysis technology. The rubber has good low-temperature performance and is easy to mix.
Preferably, the carbon black is a semi-reinforcing carbon black. The carbon black has the semi-reinforcing effect in rubber, and the types of the carbon black are N550, N660, N774 and the like, so that the rubber material has high elongation, low heat generation, high elasticity, good aging resistance and the like.
More preferably, the carbon black is under the designation N550. The N550 is suitable for natural rubber and various synthetic rubbers, is easy to disperse, can endow rubber materials with higher stiffness, and has the advantages of high extrusion speed, small mouth shape expansion and smooth extrusion surface. The vulcanized rubber has good high-temperature performance and heat conductivity, and good reinforcing performance, elasticity and resilience.
Preferably, the softening plasticizer is white oil. The softening plasticizer functions as a lubricant in rubber molecules and promotes a relaxation phenomenon of the polymer for rubber processing.
In a second aspect of the present invention, the inventors provide a method for producing a low compression set low temperature resistant EPDM weatherstrip as described in the first aspect, comprising the steps of:
100 parts of ethylene propylene diene monomer, 20-50 parts of carbon black, 5-10 parts of modified boehmite, 2.0-5.0 parts of tetrabutyl titanate, 0.5-1.0 part of sodium citrate, 3.0-5.0 parts of zinc oxide, 1.0-2.0 parts of stearic acid, 3.0-5.0 parts of polyethylene glycol, 30-50 parts of softening plasticizer, 0.5-1.0 part of first promoter, 1.5-2.0 parts of second promoter, 0.5-1.0 part of third promoter, 0.5-1.0 part of fourth promoter, 1.0-1.5 parts of anti-aging agent and 1.0-1.5 parts of vulcanizing agent are added into an internal mixer for mixing at the mixing temperature of 150 ℃ and filtered to obtain a mixed rubber material;
uniformly hot-mixing the mixed rubber material at 160 ℃ through an open mill, and then extruding and molding to obtain rubber strips; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment to obtain the low-compression permanent deformation low-temperature-resistant EPDM sealing strip.
More preferably, the vulcanization treatment adopts microwave rubber vulcanization equipment, the temperature of the microwave rubber vulcanization equipment is set to 175-185 ℃, and the treatment time is set to 300-350 s.
The microwave vulcanization temperature and time are used for vulcanizing the sealing strip, so that the comprehensive physical properties of the sealing strip meet the use requirements. The temperature and time settings of the microwave rubber vulcanization equipment can affect the vulcanization treatment effect. The temperature is set to be lower than 175 ℃, or the vulcanizing time is lower than 300s, so that the rubber strip and the vulcanizing agent cannot completely act; temperatures above 185 ℃ or curing times above 350 seconds tend to over cure and affect the compression set properties of the seal.
In a third aspect of the present invention, the inventors provide the use of a low compression set low temperature resistant EPDM weatherstrip as described in the first aspect.
Different from the prior art, the technical scheme at least has the following beneficial effects:
according to the technical scheme, the modified boehmite is added to form good interface combination with the EPDM rubber matrix, so that the low-temperature-resistant and low-compression permanent deformation-resistant performance of the sealing strip is improved. Under the using environment, the low-compression permanent deformation low-temperature resistant EPDM sealing strip provided by the technical scheme has a lower compression permanent deformation value and better low-temperature resistance. In addition, the preparation method has simple process and easily obtained materials, and is suitable for industrial production.
Detailed Description
In order to explain technical contents, structural features, and objects and effects of the technical means in detail, the following detailed description is given with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present application.
The information of the commonly used auxiliary agents used in the present invention is as follows:
the filler carbon black is purchased from Jiangxi black cat carbon black GmbH, and the boehmite is purchased from New Material GmbH in Zhongchile, Yangzhou;
the surface modifier is sodium citrate and tetrabutyl titanate, and is purchased from chemical reagents of national medicine group, Inc.;
the additive polyethylene glycol is purchased from chemical reagents of national medicine group, Inc.;
the active agent is zinc oxide and stearic acid, purchased from Kogmai chemical industry Co., Ltd;
the softening plasticizer is white oil purchased from Kogmai chemical Co., Ltd;
the first accelerator is MBT-80, the second accelerator is CBS-80, the third accelerator is ETU-80, the fourth accelerator is TMTD-80, and the accelerator is purchased from Kogmai chemical industry Co., Ltd;
the anti-aging agent is 1010, purchased from Kogmai chemical Co., Ltd;
the vulcanizing agent is S-80 purchased from Kogmai chemical Co., Ltd;
the test methods of the tensile strength, the elongation at break, the Shore A hardness, the compression permanent set and the low temperature resistance are as follows:
tensile strength, elongation at break: reference is made to the method specified in the standard GB/T528-2009.
Shore a hardness: reference is made to the method specified in the standard GB/T531.1-2008.
Compression set: reference is made to the method specified in standard GB/T7759.1-2015.
Low temperature resistance: reference is made to the method specified in the standard GB/T15256-.
Comparative example 1 EPDM weatherstrip and method of making the same
The comparative example provides an EPDM sealing strip and a preparation method thereof, and the EPDM sealing strip comprises the following components in parts by weight: 5 parts of ethylene propylene diene monomer, 20 parts of carbon black, 3 parts of zinc oxide, 1 part of stearic acid, 60003 parts of polyethylene glycol, 30 parts of softening plasticizer, MBT-800.5 parts of accelerator, CBS-801.8 parts of accelerator, ETU-800.6 parts of accelerator, TMTD-801 parts of accelerator, 10101 parts of anti-aging agent and S-801.2 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the sealing strip comprises the following steps:
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 175 ℃, and the microwave vulcanization time is 350s, so as to obtain the EPDM sealing strip.
Example 1 Low compression set low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent-deformation low-temperature-resistant EPDM sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 20 parts of carbon black, 5 parts of modified boehmite, 2 parts of tetrabutyl titanate, 0.5 part of sodium citrate, 3 parts of zinc oxide, 1 part of stearic acid, 60003 parts of polyethylene glycol, 30 parts of softening plasticizer, MBT-800.5 parts of accelerator, CBS-801.8 parts of accelerator, ETU-800.6 parts of accelerator, TMTD-801 parts of accelerator, 10101 parts of anti-aging agent and S-801.2 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the preparation method of the modified boehmite comprises the following steps:
adding 10g of boehmite into 1000ml of deionized water, and performing ultrasonic dispersion for 30min to obtain a boehmite solution;
compounding a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 2:3 to obtain an organic modifier, and slowly adding the organic modifier into the boehmite solution under the action of mechanical stirring to perform organic modification reaction; wherein the mass ratio of the organic modifier to the boehmite solution is 5:100, the stirring time is 60min, the stirring speed is 300rpm, and the reaction temperature is 40 ℃;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min, wherein the temperature of the internal mixer is 150 ℃, and filtering to obtain a mixed rubber material;
uniformly hot-refining the mixed rubber material through an open mill, and then carrying out extrusion molding at the temperature of 160 ℃ to obtain rubber strips; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 175 ℃, and the microwave vulcanization time is 350s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Embodiment 2 low compression permanent deformation low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent-deformation low-temperature-resistant EPDM sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 20 parts of carbon black, 10 parts of modified boehmite, 5 parts of tetrabutyl titanate, 1 part of sodium citrate, 3 parts of zinc oxide, 1 part of stearic acid, 60003 parts of polyethylene glycol, 30 parts of softening plasticizer, 800.6 parts of accelerator MBT, 801.7 parts of accelerator CBS-801.7 parts, 800.7 parts of accelerator ETU-358 parts, 800.8 parts of accelerator TMTD-800.8 parts, 10101 parts of anti-aging agent and 801 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 175 ℃, and the microwave vulcanization time is 340s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Embodiment 3 low compression permanent deformation low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 30 parts of carbon black, 9 parts of modified boehmite, 4.5 parts of tetrabutyl titanate, 1.8 parts of sodium citrate, 4 parts of zinc oxide, 2 parts of stearic acid, 60004 parts of polyethylene glycol, 40 parts of softening plasticizer, MBT-800.7 parts of accelerator, CBS-801.9 parts of accelerator, ETU-800.5 parts of accelerator, TMTD-800.6 parts of accelerator, 10101.1 parts of anti-aging agent and 801.3 parts of vulcanizing agent.
Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 180 ℃, and the microwave vulcanization time is 320s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Embodiment 4 low compression permanent deformation low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 30 parts of carbon black, 6 parts of modified boehmite, 3 parts of tetrabutyl titanate, 1.2 parts of sodium citrate, 4 parts of zinc oxide, 1 part of stearic acid, 60004 parts of polyethylene glycol, 50 parts of softening plasticizer, 800.8 parts of accelerator MBT, 802 parts of accelerator CBS, 800.8 parts of accelerator ETU, 78 parts of accelerator TMTD-800.5, 10101.3 parts of anti-aging agent and 801.5 parts of vulcanizing agent S. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials in the step (1) into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 180 ℃, and the microwave vulcanization time is 310s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Embodiment 5 Low compression permanent deformation low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 40 parts of carbon black, 6 parts of modified boehmite, 3 parts of tetrabutyl titanate, 1.2 parts of sodium citrate, 4 parts of zinc oxide, 2 parts of stearic acid, 60005 parts of polyethylene glycol, 40 parts of softening plasticizer, MBT-801 parts of accelerator, CBS-801.5 parts of accelerator, ETU-800.9 parts of accelerator, TMTD-800.5 parts of accelerator, 10101.4 parts of anti-aging agent and S-801.5 parts of vulcanizing agent.
Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 175 ℃, and the microwave vulcanization time is 330s, so as to obtain the low-compression permanent deformation low-temperature resistant EPDM sealing strip.
Embodiment 6 low compression permanent deformation low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 40 parts of carbon black, 8 parts of modified boehmite, 4 parts of tetrabutyl titanate, 0.8 part of sodium citrate, 4 parts of zinc oxide, 1 part of stearic acid, 60005 parts of polyethylene glycol, 30 parts of softening plasticizer, MBT-800.9 parts of accelerator, CBS-801.6 parts of accelerator, ETU-801 parts of accelerator, TMTD-800.5 parts of accelerator, 10101.5 parts of anti-aging agent and S-801.1 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 180 ℃, and the microwave vulcanization time is 350s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Example 7 Low compression set low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 45 parts of carbon black, 9 parts of modified boehmite, 4.5 parts of tetrabutyl titanate, 0.8 part of sodium citrate, 5 parts of zinc oxide, 1 part of stearic acid, 60005 parts of polyethylene glycol, 50 parts of softening plasticizer, 800.8 parts of accelerator MBT, 801.6 parts of accelerator CBS-8, 800.8 parts of accelerator ETU, 800.6 parts of accelerator TMTD-10101.4 parts of anti-aging agent and 801.4 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 185 ℃, and the microwave vulcanization time is 350 seconds, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Embodiment 8 low compression permanent deformation low temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 45 parts of carbon black, 7 parts of modified boehmite, 3.5 parts of tetrabutyl titanate, 0.7 part of sodium citrate, 5 parts of zinc oxide, 2 parts of stearic acid, 60005 parts of polyethylene glycol, 40 parts of softening plasticizer, MBT-800.7 parts of accelerator, CBS-801.7 parts of accelerator, ETU-800.7 parts of accelerator, TMTD-800.9 parts of accelerator, 10101 parts of anti-aging agent and S-801 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 185 ℃, and the microwave vulcanization time is 330s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
Example 9 Low compression set Low temperature resistant EPDM weatherstrip and preparation method thereof
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 50 parts of carbon black, 10 parts of modified boehmite, 5 parts of tetrabutyl titanate, 1 part of sodium citrate, 5 parts of zinc oxide, 2 parts of stearic acid, 60004 parts of polyethylene glycol, 50 parts of softening plasticizer, MBT-801 parts of accelerator, CBS-801.5 parts of accelerator, ETU-800.5 parts of accelerator, TMTD-800.8 parts of accelerator, 10101.2 parts of anti-aging agent and S-801.2 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 175 ℃, and the microwave vulcanization time is 330s, so as to obtain the low-compression permanent deformation low-temperature resistant EPDM sealing strip.
Example 10 Low compression set Low temperature resistant EPDM weatherstrip and method of making the same
The embodiment provides a low-compression permanent deformation low-temperature resistant EPDM (ethylene-propylene-diene monomer) sealing strip which comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 50 parts of carbon black, 5 parts of modified boehmite, 2.5 parts of tetrabutyl titanate, 0.6 part of sodium citrate, 4 parts of zinc oxide, 1 part of stearic acid, 60003 parts of polyethylene glycol, 30 parts of softening plasticizer, MBT-800.5 parts of accelerator, CBS-801.9 parts of accelerator, ETU-800.9 parts of accelerator, TMTD-800.7 parts of accelerator, 10101 parts of anti-aging agent and S-801.5 parts of vulcanizing agent. Wherein the ethylene propylene diene monomer is 4045M, the carbon black is N550, and the softening plasticizer is white oil. The preparation method of the low-compression permanent deformation low-temperature resistant EPDM sealing strip comprises the following steps:
the modified boehmite was prepared in the same manner as in example 1;
adding the raw materials into an internal mixer according to the proportion, mixing for 10min at the temperature of 150 ℃, and filtering to obtain a mixed rubber material;
and (3) carrying out extrusion molding on the mixed rubber material after the mixed rubber material is uniformly heated through an open mill at the temperature of 160 ℃. Obtaining an adhesive tape; and continuously conveying the rubber strip to microwave rubber vulcanization equipment for vulcanization treatment, wherein the microwave vulcanization temperature is 185 ℃, and the microwave vulcanization time is 320s, so that the low-compression permanent deformation low-temperature resistant EPDM sealing strip is obtained.
The amounts of the respective raw material components of the sealing tape and the production methods thereof provided in the above comparative example 1 and examples 1 to 10 are shown in tables 1 and 2, respectively.
TABLE 1 amount of raw material components for sealing tape of comparative example 1 and examples 1 to 10
Figure BDA0003221609320000141
Figure BDA0003221609320000151
TABLE 2 Process parameters for the preparation of comparative example 1 and examples 1 to 10
Figure BDA0003221609320000152
Figure BDA0003221609320000161
The physical properties of the low compression set low temperature resistant EPDM weatherstrips prepared in examples 1-10 and comparative example 1 were measured, respectively, and the results are shown in Table 3.
TABLE 3 weather strip Performance parameter test results for comparative example 1 and examples 1-10
Figure BDA0003221609320000162
As can be seen from the test data in the table above, the tensile strength, elongation at break, shore a hardness, compression set, low temperature resistance, etc. of the other examples are superior to those of comparative example 1. Example 9 had a tensile strength of at most 19.2MPa and example 7 had a compression set of at least 26 mm. Overall, the overall performance of the EPDM is enhanced with the increased content of the modified boehmite filler; the microwave vulcanization time is suitably reduced and the compression set of the EPDM is reduced. All the examples were better in tensile strength, compression set and low temperature resistance than comparative example 1. By adjusting the formula and the process parameters, the tensile strength of the embodiment 10 reaches 18.8MPa, the elongation at break reaches 326%, and the Shore A hardness is 87; keeping the compression ratio at 25% and 70 ℃ for 72h, then releasing the compression, recovering the sample in a free state, enabling the sample to rebound for 35mm, and enabling the compression permanent deformation to be smaller; it can be maintained at-40 deg.C for 22 hr, and has elasticity and no crack. Therefore, the low-compression permanent-deformation low-temperature-resistant EPDM sealing strip provided by the technical scheme of the invention has a lower compression permanent-deformation value and better low-temperature resistance.
The preparation method provided by the technical scheme has the advantages of simple process, easily obtained materials and suitability for industrial production, and the prepared EPDM sealing strip has low compression permanent deformation, good low temperature resistance and excellent sealing performance.
It should be noted that, although the above embodiments have been described herein, the invention is not limited thereto. Therefore, based on the innovative concepts of the present invention, the technical solutions of the present invention can be directly or indirectly applied to other related technical fields by making changes and modifications to the embodiments described herein or by using equivalent structures or equivalent processes performed in the present specification, and are included in the scope of the present invention.

Claims (10)

1. A low-compression permanent deformation low-temperature resistant EPDM sealing strip is characterized by comprising the following components in parts by weight:
100 parts of ethylene propylene diene monomer, 20-50 parts of carbon black, 5-10 parts of modified boehmite, 2.0-5.0 parts of tetrabutyl titanate, 0.5-1.0 part of sodium citrate, 3.0-5.0 parts of zinc oxide, 1.0-2.0 parts of stearic acid, 3.0-5.0 parts of polyethylene glycol, 30-50 parts of softening plasticizer, 0.5-1.0 part of first accelerator, 1.5-2.0 parts of second accelerator, 0.5-1.0 part of third accelerator, 0.5-1.0 part of fourth accelerator, 1.0-1.5 parts of anti-aging agent and 1.0-1.5 parts of vulcanizing agent.
2. The low compression set low temperature resistant EPDM weatherstrip according to claim 1 wherein said modified boehmite is prepared by the steps of:
adding boehmite into deionized water for dispersion to obtain a boehmite solution;
adding an organic modifier into the boehmite solution according to the mass ratio of the organic modifier to the boehmite solution of 5:100 to carry out organic modification reaction to obtain an organically modified boehmite solution;
and filtering the organic modified boehmite solution, drying filter residues, and grinding by a ball mill to obtain the modified boehmite with the particle size of about 1-20 mu m.
3. The EPDM weather strip with low compression set and low temperature resistance of claim 2, wherein the organic modifier is a silane coupling agent γ - (2, 3-glycidoxy) propyl trimethoxy silane and 3- (methacryloyloxy) propyl trimethoxy silane compounded in a mass ratio of 2: 3.
4. The low compression set low temperature resistant EPDM weatherstrip of claim 1 wherein said EPDM rubber is 4045M.
5. The low compression set low temperature resistant EPDM weatherstrip of claim 1 wherein said carbon black is a semi-reinforcing carbon black.
6. The low compression set low temperature resistant EPDM weatherstrip of claim 5 wherein said carbon black is designated N550.
7. The low compression set low temperature resistant EPDM weatherstrip according to claim 1 wherein said softening plasticizer is white oil.
8. A method of manufacturing a low compression set low temperature resistant EPDM weatherstrip according to any one of claims 1 to 7 comprising the steps of:
100 parts of ethylene propylene diene monomer, 20-50 parts of carbon black, 5-10 parts of modified boehmite, 2.0-5.0 parts of tetrabutyl titanate, 0.5-1.0 part of sodium citrate, 3.0-5.0 parts of zinc oxide, 1.0-2.0 parts of stearic acid, 3.0-5.0 parts of polyethylene glycol, 30-50 parts of softening plasticizer, 0.5-1.0 part of first promoter, 1.5-2.0 parts of second promoter, 0.5-1.0 part of third promoter, 0.5-1.0 part of fourth promoter, 1.0-1.5 parts of anti-aging agent and 1.0-1.5 parts of vulcanizing agent are added into an internal mixer for mixing at the mixing temperature of 150 ℃ and filtered to obtain a mixed rubber material;
uniformly heating the mixed rubber material at 160 ℃, and then extruding and molding to obtain an adhesive tape; and vulcanizing the rubber strip to obtain the low-compression permanent deformation low-temperature resistant EPDM sealing strip.
9. The method as claimed in claim 8, wherein the vulcanization process is carried out by using a microwave rubber vulcanization device, the temperature of the microwave rubber vulcanization device is set to 175-185 ℃, and the processing time is set to 300-350 s.
10. Use of a low compression set low temperature resistant EPDM weatherstrip as claimed in any one of claims 1 to 7.
CN202110959312.5A 2021-08-20 2021-08-20 Low-compression permanent deformation low-temperature-resistant EPDM (ethylene-propylene-diene monomer) sealing strip as well as preparation method and application thereof Pending CN113652031A (en)

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CN106496809A (en) * 2016-10-09 2017-03-15 闻承岳 A kind of waterproof anti-corrosion weather strip for automobile elastomeric material and preparation method thereof
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Application publication date: 20211116