CN110240760B - Insulating flame-retardant ethylene propylene diene monomer rubber hose composition and preparation method thereof - Google Patents
Insulating flame-retardant ethylene propylene diene monomer rubber hose composition and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
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- C08L23/02—Compositions 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/28—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances natural or synthetic rubbers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C08L2203/00—Applications
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- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses an insulating flame-retardant ethylene propylene diene monomer rubber hose composition which is characterized by comprising the following components in parts by weight: 100 parts of EPDM 5890F; 2-6 parts of kaolin; 3-8 parts of zinc oxide; 1-3 parts of stearic acid; 2-5 parts of paraffin; 1-3 parts of an anti-aging agent MB; 50-70 parts of carbon black SP 6400A; 130-190 parts of flame retardant; 10-30 parts of paraffin oil; 1-2 parts of sulfur; 10-15 parts of calcium oxide; 1.6-3 parts of an accelerator; the accelerant comprises 0.5-0.8 part of BZ accelerant, 0.7-1.2 parts of TRA accelerant, 0.2-0.5 part of DM accelerant and 0.2-0.5 part of accelerant TT; the flame retardant is 80-100 parts of aluminum hydroxide, 20-40 parts of zinc borate, 10-20 parts of antimony trioxide and 20-30 parts of decabromodiphenylethane, and the invention also aims to provide a preparation method of the insulating flame-retardant ethylene propylene diene monomer hose composition, which meets the mechanical strength requirement of rubber on the premise of meeting the electrical insulation and insulation resistance of vulcanized rubber.
Description
Technical Field
The invention belongs to the technical field of rubber, and particularly relates to an insulating flame-retardant ethylene propylene diene monomer rubber hose composition and a preparation method thereof.
Background
The rubber hose is one of the wiring rubber products in the motor train unit, and the parts are positioned in the motor train unit body and outside the motor train unit body. Various wires are threaded inside the hose, the hose mainly protects the internal cables under the action of mechanical external force, and the internal cables are also protected against external heat sources, Ethylene Propylene Diene Monomer (EPDM) is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, and is widely applied due to excellent electrical insulation, low density, high filling property, low temperature resistance, heat resistance, ozone resistance, weather resistance and the like, and accounts for about 7% of the total consumption of synthetic rubber in the world, and is located in the third place, but the hose has poor flame retardant property and poor insulating property.
As ethylene propylene diene monomer is known as non-self-reinforcing rubber, carbon black is required to be added for reinforcing the ethylene propylene diene monomer to achieve certain mechanical strength, however, the carbon black is a conductive material, and the mechanical property is increased but the insulating property is reduced along with the increase of the proportional amount of the carbon black in the ethylene propylene diene monomer.
At present, the flame retardant property of the rubber hose composition usually adopts halogen flame retardant, and the rubber hose composition has the advantages of small using amount, high flame retardant efficiency and wide adaptability, but has the serious defects of generating a large amount of smoke and toxic and corrosive gas during combustion and having great harm.
The prior art therefore remains to be improved.
Disclosure of Invention
The invention provides an insulating flame-retardant ethylene propylene diene monomer rubber hose composition, and aims to provide an ethylene propylene diene monomer rubber composition with excellent flame-retardant performance and insulating performance.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
an insulating flame-retardant ethylene propylene diene monomer hose composition comprises the following components in parts by weight:
100 parts of EPDM 5890F; 2-6 parts of kaolin; 3-8 parts of zinc oxide; 1-3 parts of stearic acid and 2-5 parts of paraffin; 1-3 parts of an anti-aging agent MB; 50-70 parts of carbon black SP 6400A; 130-190 parts of flame retardant; 10-30 parts of paraffin oil; 1-2 parts of sulfur; 10-15 parts of calcium oxide; 1.6-3 parts of an accelerator;
the accelerant comprises 0.5-0.8 part of BZ accelerant, 0.7-1.2 parts of TRA accelerant, 0.2-0.5 part of DM accelerant and 0.2-0.5 part of accelerant TT;
the flame retardant is 80-100 parts of aluminum hydroxide, 20-40 parts of zinc borate, 10-20 parts of antimony trioxide and 20-30 parts of decabromodiphenylethane.
The invention also provides a preparation method of the insulating flame-retardant rubber hose composition, which comprises the following steps:
(1) weighing: weighing the raw materials according to the proportion in the formula; (ii) a
(2) Pretreatment of raw materials: uniformly stirring the carbon black SP6400A weighed in the step (1) with aluminum hydroxide and paraffin oil, and performing ultrasonic activation for 5-7 hours for later use;
(3) primary pressurizing and mixing: ethylene propylene diene monomer EPDM5890F, kaolin, zinc oxide, an anti-aging agent MB, paraffin and stearic acid are added into an internal mixer for mixing, the top plug pressure is 05-0.6MPa, and the time is 2-3 minutes;
(4) secondary pressurizing and mixing: adding the carbon black SP6400A treated in the step (1) and aluminum hydroxide into the rubber material mixed in the step (3), wherein the upper top plug pressure is 0.5-0.6 MPa;
(5) thirdly, pressurizing and mixing, namely adding zinc borate, antimony trioxide, decabromodiphenylethane into the rubber material mixed in the step (4) for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the finishing temperature is 140-;
(6) and (3) sheet discharging: discharging the mixed rubber material obtained in the step (5) onto an open mill, thinly passing the rubber material on the open mill for 3-4 times to cool the rubber material to 70-80 ℃, then uniformly adding sulfur, an accelerant and calcium oxide, pouring the rubber for 3-4 times, finally adjusting the roll distance of the open mill to 1mm, and carrying out sheet-feeding cooling after thinly passing;
(7) and (3) hot smelting and strip discharging: preheating the roll temperature of the open mill to 50-60 ℃, then placing the rubber material treated in the step (6) on the open mill, wherein the single-time rubber material preheating is 50-60kg, and stripping the rubber material after the rubber material is uniformly preheated and the surface is smooth, wherein the stripping thickness is 7-10mm, and the width is 50-60 mm;
(8) hot air vulcanization: and (3) placing the rubber strip prepared in the step (7) into an extruder for extrusion, wherein the temperature of a screw is set to be 55-75 ℃, and the temperature of a machine head is set to be 80-90 ℃.
Further, when the vulcanization extrusion in the step (8) is carried out, the screw tube core is filled with 0.1MPa of air pressure, and hot air vulcanization is adopted for vulcanization.
The hot air vulcanization is three-section oven hot air vulcanization, wherein the first-section hot air vulcanization temperature is 190-200 ℃, the second-section hot air vulcanization temperature is 180-190 ℃, and the third-section hot air vulcanization temperature is 170-180 ℃. The invention has the beneficial effects that:
1. the electrical insulation performance of the rubber refined by selecting a proper proportion is increased to 1000V under the voltage of 1000V, and the insulation resistance is more than or equal to 1000M omega; the oxygen index is more than or equal to 30 percent to meet the performance requirement, the tensile strength of vulcanized rubber is more than or equal to 12Mpa, and the elongation at break is more than or equal to 500 percent; on the premise of meeting the electrical insulation and insulation resistance of vulcanized rubber, the mechanical strength requirement of the rubber is met.
2. According to the invention, before mixing, the carbon black is activated, and during activation, ultrasonic treatment is carried out together with aluminum hydroxide and paraffin oil serving as flame retardants, and during ultrasonic treatment, the paraffin oil is dissolved in the carbon black and the aluminum hydroxide and is uniformly stirred, and after ultrasonic treatment, the solubility of the paraffin oil and an inorganic flame retardant, namely aluminum hydroxide, is greatly increased, so that the surface activation effect is achieved, the reinforcing effect of the carbon black and the aluminum hydroxide is increased, meanwhile, the ultrasonic treatment on the aluminum hydroxide also increases the active groups on the surface, the dispersibility of the aluminum hydroxide is increased during later mixing, and the ultrasonic treatment is carried out on the carbon black and the aluminum hydroxide before mixing, so that the problem that pores appear on the cross section of vulcanized dense rubber is solved, and the cross section of a product after vulcanization is dense and has no pores.
3. The method comprises the steps of mixing carbon black, aluminum hydroxide and paraffin oil together, performing ultrasonic treatment, avoiding the problem of caking, activating the surface of the carbon black by ultrasonic treatment under a slightly alkaline environment together with the paraffin oil and the aluminum hydroxide, so that the insulating property of the carbon black cannot be influenced, the paraffin oil is an indispensable plasticizer in the formula, performing ultrasonic treatment together with a flame retardant aluminum hydroxide without additionally adding a treating agent, and avoiding other influences during later rubber mixing.
4. According to the invention, kaolin is added into the formula, the ethylene propylene diene monomer EPDM5890F and the kaolin are mixed together during primary mixing, so that the mechanical strength of the ethylene propylene diene monomer body can be increased, the plasticity of the rubber is increased, and a small amount of cations can be generated during multiple mixing and rubbing processes during secondary pressure mixing and tertiary pressure mixing, so that the insulating property and the flame retardant property of the prepared rubber material are enhanced.
5. The invention fills 0.1Mpa air pressure to the screw tube core in the extrusion process, the pressurization can ensure that the hose can play a supporting role when the rubber hose is extruded, and the vulcanization adopts the hot air three-section vulcanization, the product wall thickness is uniform and is not easy to deform after the mode is formed, and the problem that the rubber is easy to fracture surface air holes in the rubber non-pressure vulcanization process is fundamentally solved.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
Example one
An insulating flame-retardant ethylene propylene diene monomer hose composition comprises the following components in parts by weight:
100 parts of EPDM 5890F; 2 parts of kaolin; 3 parts of zinc oxide; 1.2 parts of stearic acid; 2 parts of paraffin; 1 part of an anti-aging agent MB; 50 parts of carbon black SP 6400A; 100 parts of aluminum hydroxide; 40 parts of zinc borate; 10 parts of antimony trioxide; 10 parts of decabromodiphenylethane; 10 parts of paraffin oil; 1 part of sulfur; 0.8 part of accelerator BZ; 1.2 parts of accelerator TRA; 0.5 part of accelerator DM; 0.5 part of accelerator TT; 10 parts of calcium oxide.
A preparation method of an insulating flame-retardant rubber hose composition comprises the following steps:
(1) weighing: weighing the raw materials according to the proportion in the formula; (ii) a
(2) Pretreatment of raw materials: uniformly stirring the carbon black SP6400A weighed in the step (1) with aluminum hydroxide and paraffin oil, ultrasonically activating for 5 hours, fishing out the carbon black SP6400A and the aluminum hydroxide, and draining for later use;
(3) primary pressurizing and mixing: ethylene propylene diene monomer EPDM5890F, kaolin, zinc oxide, an anti-aging agent MB, paraffin and stearic acid are added into an internal mixer for mixing, the upper ram pressure is 0.5MPa, and the time is 3 minutes;
(4) secondary pressurizing and mixing: adding the carbon black SP6400A treated in the step (1) and aluminum hydroxide into the rubber material mixed in the step (3), wherein the upper top plug pressure is 0.5 MPa;
(5) thirdly, pressurizing and mixing, namely adding zinc borate, antimony trioxide and decabromodiphenylethane into the rubber material mixed in the step (4) for mixing, wherein the upper plug pressure is 0.5MPa, and the finishing temperature is 140 ℃;
(6) and (3) sheet discharging: discharging the rubber material obtained in the step (3) onto an open mill, thinly passing the rubber material on the open mill for 3-4 times to cool the rubber material to 80 ℃, then uniformly adding sulfur, an accelerator and calcium oxide, pouring the rubber for 3 times, finally adjusting the roll distance of the open mill to 1mm, and carrying out thinning and sheet cooling;
(7) and (3) hot smelting and strip discharging: the method comprises the steps of preheating the roll temperature of an open mill to 60 ℃, then placing the preheated rubber material on the open mill, wherein the single-time preheating of the rubber material is 55kg, and after the rubber material is uniformly preheated and has a smooth surface, the rubber material is stripped down to the thickness of 7-10mm, wherein the thickness of the stripped rubber material is set to be 8 mm, the width of the stripped rubber material is set to be 50-60mm, and the thickness of the stripped rubber material is set to be 8 mm.
(8) Hot air vulcanization: and (3) placing the rubber strip prepared in the step (7) in an extruder for extrusion, setting the temperature of a screw to be 75 ℃, setting the temperature of a machine head to be 90 ℃, filling the air pressure of 0.1MPa into a screw tube core during vulcanization extrusion, vulcanizing by adopting hot air, wherein the hot air vulcanization is three-section oven hot air vulcanization, the first-section hot air vulcanization temperature is 190-200 ℃, the second-section hot air vulcanization temperature is 180-190 ℃, and the third-section hot air vulcanization temperature is 170-180 ℃.
Comparative example 1
An insulating flame-retardant ethylene propylene diene monomer hose composition is consistent with the first embodiment in terms of weight fraction, and is only different from the first embodiment in that kaolin is not added.
Preparation method of insulating flame-retardant ethylene propylene diene monomer rubber hose composition is same as that of embodiment one
Comparative example No. two
An insulating flame-retardant ethylene propylene diene monomer hose composition is calculated according to weight fractions and is consistent with the embodiment.
The preparation method of the insulating flame-retardant ethylene propylene diene monomer hose composition is the same as that of the first embodiment, and only the second step is omitted.
Comparative example No. three
An insulating flame-retardant ethylene propylene diene monomer hose composition is calculated according to weight fractions and is consistent with the embodiment.
The preparation method of the insulating flame-retardant ethylene propylene diene monomer hose composition is the same as that of the first embodiment, and only the step 8 is that the pipe core of the screw rod is not pressurized.
Example two
An insulating flame-retardant ethylene propylene diene monomer hose composition comprises the following components in parts by weight:
100 parts of PDM 5890F; 4 parts of kaolin; 5 parts of zinc oxide; 2 parts of stearic acid; 3 parts of paraffin; 1.5 parts of an anti-aging agent MB; 60 parts of carbon black SP 6400A; 90 parts of aluminum hydroxide; 30 parts of zinc borate; 15 parts of antimony trioxide; 25 parts of decabromodiphenylethane; 15 parts of paraffin oil; 1.2 parts of sulfur; 0.7 part of accelerator BZ; 1 part of accelerator TRA; 0.4 part of accelerator DM; 0.4 part of accelerator TT; 12 parts of calcium oxide.
The preparation method of the insulating flame-retardant ethylene propylene diene monomer hose composition is the same as that of the first embodiment.
EXAMPLE III
An insulating flame-retardant ethylene propylene diene monomer hose composition comprises the following components in parts by weight:
100 parts of EPDM 5890F; 6 parts of kaolin; 6 parts of zinc oxide; 2.2 parts of stearic acid; 4 parts of paraffin; 2 parts of an anti-aging agent MB; 70 parts of carbon black SP 6400A; 80 parts of aluminum hydroxide; 30 parts of zinc borate; 20 parts of antimony trioxide; 20 parts of decabromodiphenylethane; 30 parts of paraffin oil; 1.5 parts of sulfur; 0.5 part of accelerator BZ; 0.8 part of accelerator TRA; 0.2 part of accelerator DM; 0.2 part of accelerator TT; 15 parts of calcium oxide.
The preparation method of the insulating flame-retardant ethylene propylene diene monomer hose composition is the same as that of the first embodiment.
The rubber materials of examples 1-3 and comparative examples 1-3 of the invention are subjected to performance test, wherein the tensile strength and the elongation at break of the rubber are tested according to the method specified in GB/T528-2009; the electrical insulation performance was tested according to the method specified in TB/T2843-2015; determination of the Combustion Properties of rubber oxygen index method according to
The test is carried out by the method specified in GB/T10707-2008, and the detection results are shown in Table 1.
Table 1:
compared with the comparative examples 1-2, the addition of kaolin, the tensile strength, the elongation at break and other mechanical properties of the carbon black and the aluminum hydroxide after the common ultrasonic treatment are obviously higher than those of the comparative examples 1-2, and meanwhile, the prepared rubber has excellent flame retardant property and insulating property.
Compared with the comparative example 3, the examples 1-3 show that the appearance of the rubber can be obviously improved by adopting hot air vulcanization and pressurizing the screw tube core during extrusion, the technical index of meeting the requirements of customers, namely the electrical insulation performance of the rubber, is more than or equal to 1000 MOmega under the condition of pressurizing 1000V voltage; the oxygen index is more than or equal to 30 percent, the tensile strength of vulcanized rubber is more than or equal to 12Mpa, and the elongation at break is more than or equal to 500 percent.
The foregoing is only a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the principle of the invention, and such modifications and improvements are also considered to be within the scope of the invention.
Claims (2)
1. An insulating flame-retardant ethylene propylene diene monomer hose composition is characterized by comprising the following components in parts by weight: 100 parts of EPDM 5890F; 2-6 parts of kaolin; 3-8 parts of zinc oxide; 1-3 parts of stearic acid; 2-5 parts of paraffin; 1-3 parts of an anti-aging agent MB; 50-70 parts of carbon black SP 6400A; 130-190 parts of flame retardant; 10-30 parts of paraffin oil; 1-2 parts of sulfur; 10-15 parts of calcium oxide; 1.6-3 parts of an accelerator;
the accelerant comprises 0.5-0.8 part of BZ accelerant, 0.7-1.2 parts of TRA accelerant, 0.2-0.5 part of DM accelerant and 0.2-0.5 part of accelerant TT;
the flame retardant is 80-100 parts of aluminum hydroxide, 20-40 parts of zinc borate, 10-20 parts of antimony trioxide and 20-30 parts of decabromodiphenylethane;
the preparation method of the rubber hose composition comprises the following steps:
(1) weighing: weighing the raw materials according to the proportion in the formula;
(2) pretreatment of raw materials: uniformly stirring the carbon black SP6400A weighed in the step (1) with aluminum hydroxide and paraffin oil, and performing ultrasonic activation for 5-7 hours for later use; (3) primary pressurizing and mixing: ethylene propylene diene monomer EPDM5890F, kaolin, zinc oxide, an anti-aging agent MB, paraffin and stearic acid are added into an internal mixer for mixing, the top plug pressure is 05-0.6MPa, and the time is 2-3 minutes;
(4) secondary pressurizing and mixing: adding the carbon black SP6400A treated in the step (1) and aluminum hydroxide into the rubber material mixed in the step (3), wherein the upper top plug pressure is 0.5-0.6 MPa;
(5) thirdly, pressurizing and mixing, namely adding zinc borate, antimony trioxide and decabromodiphenylethane into the rubber material mixed in the step (4) for mixing, wherein the upper plug pressure is 0.5-0.6MPa, and the finishing temperature is 140-;
(6) and (3) sheet discharging: discharging the rubber material obtained in the step (3) onto an open mill, thinly passing the rubber material on the open mill for 3-4 times to cool the rubber material to 70-80 ℃, then uniformly adding sulfur, an accelerator and calcium oxide, pouring the rubber for 3-4 times, finally adjusting the roll distance of the open mill to 1mm, and carrying out thin passing and then sheet cooling;
(7) and (3) hot smelting and strip discharging: preheating the roll temperature of an open mill to 50-60 ℃, then placing the preheated rubber material on the open mill, wherein 50-60kg of rubber material is preheated in one time, and stripping the rubber material after the rubber material is uniformly preheated and has a smooth surface, wherein the stripping thickness is 7-10mm, and the width is 50-60 mm;
(8) hot air vulcanization: placing the rubber strip prepared in the step (7) in an extruder for extrusion, wherein the temperature of a screw is set to be 55-75 ℃, and the temperature of a machine head is set to be 80-90 ℃; and (3) filling the tube core of the screw rod with the air pressure of 0.1MPa, and vulcanizing by adopting hot air.
2. The method of claim 1, wherein the hot air vulcanization is a three-stage oven hot air vulcanization, the first stage hot air vulcanization temperature is 190-200 ℃, the second stage hot air vulcanization temperature is 180-190 ℃, and the three-stage hot air vulcanization temperature is 170-180 ℃.
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