CN102276928A - Olefin rubber high-flame-retardant oil-resistant heat-shrinkable bush and preparation method thereof - Google Patents
Olefin rubber high-flame-retardant oil-resistant heat-shrinkable bush and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an olefin rubber high-flame-retardant oil-resistant heat-shrinkable bush. The olefin rubber high-flame-retardant oil-resistant heat-shrinkable bush is prepared from basic materials of olefin rubber granules such as ethylene propylene diene monomer (EPDM), ethylene-ethyl acrylate copolymer (EEA) and ethylene-octene copolymer (POE), as well as silicon rubber (methyl ethylene silicon rubber), a special environment-friendly halogen-free compound flame retardant, a composite antioxidant and related aids by using equipment such as an internal mixer, an extruder, an electronic accelerator, a heating expanding machine and the like. The product does not contain harmful substances such as heavy metal, halogen and the like, and has high fire resistance and low smoke; the oxygen index of the material reaches 45; the fire resistance of the product passes UL94-5VA grade through a test; the product can be used at the temperature of between -50 and 150 DEG C for a long time; when the product is used for a short time, the temperature reaches 250 DEG C; and the product has excellent oil (aviation oil, fuel oil, machine oil, lubricating oil and the like) resistance.
Description
Technical field
The present invention relates to a kind of olefines rubber high flame retardant oil resistant heat-shrinkable T bush and preparation method thereof.
Background technology
At present the general use temperature scope of olefines heat-shrink tube is :-40～125 ℃, the product oil-proofness is relatively poor, does not possess flame retardant resistance, and general vulcanization adopts High Temperature High Pressure, and sulfuration cost height, speed are slow.
Tradition olefines rubber heat-shrink tube all is to adopt to add vulcanizing agent in prescription, High Temperature High Pressure sulfuration in curing tube or mould, and vulcanization rate is slow, poor adherence, sulfuration expense height.
Summary of the invention
The objective of the invention is provides a kind of olefines rubber high flame retardant oil resistant heat-shrinkable T bush and preparation method thereof at the shortcoming of present olefines heat-shrink tube production technique and product performance existence, the heat-shrinkable T bush that obtains does not contain hazardous and noxious substances such as heavy metal, halogen, has higher flame retardant properties, the amount of being fuming is low, oil-proofness is strong, can be in the medium-term and long-term use of-50～150 ℃ environment.
For realizing above purpose, technical solution of the present invention is:
A kind of preparation method of olefines rubber high flame retardant oil resistant heat-shrinkable T bush may further comprise the steps:
The first step: product pellet preparation: EPDM, EEA, POE, methyl vinyl silicone rubber, magnesium hydroxide, zinc borate, methyl phenyl silicone oil, composite antioxidant, linking agent TMPTMA, white oil, zinc stearate and paraffin are joined in the Banbury mixer, temperature 80-130 ℃, banburying 8-10 minute, then that banburying is good material is drained in the parallel double-screw granulation unit, melt extrude, die face cutting is dried after the particle dehydration under water, obtains the product pellet; The working temperature of forcing machine is: 110 ± 5 ℃ in a district, 120 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 145 ± 5 ℃ in four districts, 120 ± 5 ℃ in five districts; The ratio of used EPDM, EEA, POE, methyl vinyl silicone rubber, magnesium hydroxide, zinc borate, methyl phenyl silicone oil, oxidation inhibitor, linking agent TMPTMA, white oil, zinc stearate, paraffin is: 60-80:20-10:20-10:5-10:100-120:5-10::0.5-1::0.3-0.6:0.3-0.6:3-5:0.5-1:1-2;
Second step: the extruding of linear polymer heat-shrink tube: the plastic pellet for preparing is joined in the single screw extrusion machine, extrude all slick tubing of inside and outside wall, the tubing of extruding is wrapped on the take-up reel; The working temperature of single screw extrusion machine is: 100 ± 5 ℃ in a district, 125 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 125 ± 5 ℃ in four districts, 110 ± 5 ℃ in five districts;
The 3rd step: the cross-linking radiation of heat-shrink tube: the tubing that will extrude carries out cross-linking radiation through rumbatron and becomes cross-linked thermoset polymer, and irradiation dose is 15-18Mrad;
The 4th step: tubing add thermal enlargement: the tubing behind the cross-linking radiation, expands the expansion temperature through heating dilator continuously: 130 ± 10 ℃, the water cooling typing of expansion back obtains finished product olefines rubber high flame retardant oil resistant heat-shrinkable T bush.
Described oxidation inhibitor is made up of oxidation inhibitor 1 and oxidation inhibitor 2, and the consumption weight ratio of oxidation inhibitor 1 and oxidation inhibitor 2 is: 1:0.66-1:1.5; Oxidation inhibitor 1 is antioxidant 300 or is the mixture of 70wt% antioxidant 1010 and 30wt% oxidation inhibitor DSTDP that oxidation inhibitor 2 is the mixture of 60wt% oxidation inhibitor PNX102,20wt% oxidation inhibitor 168 and 20wt% oxidation inhibitor PS800.
The present invention also provides the olefines rubber high flame retardant oil resistant that makes as stated above heat-shrinkable T bush.
Product test data of the present invention (detecting the station, Wuhan by national light industry plastic prod quality surveillance provides)
This product and the contrast of other heat-shrink tube performance advantage:
From top contrast as can be seen, product has stronger advantage on crosslinking method, flame retardant resistance, price, hardness, use temperature scope.
The present invention adopts the polyolefins rubber grain: the EPDM(ethylene-propylene diene copolymer), the EEA(ethylene-ethyl acrylate copolymer), the POE(ethylene-octene copolymer) as base mateiral, cooperate silicon rubber (methyl vinyl silicone rubber), extraordinary environment friendly halogen-free fireproof agent, composite antioxidant and relevant auxiliary agent, be prepared from through equipment such as Banbury mixer, forcing machine, rumbatron, heating dilators, the product that makes does not contain hazardous and noxious substances such as any heavy metal and halogen.Product is after the irradiation of rumbatron high-power electron beam, and linear macromolecule part segment produces crosslinked, becomes " thermoset " material with " memory effect ", and heating and the several times postcooling typing that expanded in diameter is extremely original promptly get this product.This product possesses very high flame retardant properties, the amount of being fuming is low, the material oxygen index is up to 45, the test of product flame retardant properties is by the UL94-5VA level, can be in the medium-term and long-term use of-50～150 ℃ environment, use temperature reaches 250 ℃ in short-term, and oil resistant uses oily temperature to reach 90 ℃, has excellent oil resistant (aero oil, oil fuel, machinery oil, lubricated wet goods) performance.This product non-stop run temperature range is :-50 ℃ ~ 150 ℃, and 90 ℃ of minimum shrinkage temperatures, 175 ℃ of minimum complete shrinkage temperatures.The oxygen index of product (OI) is up to 45, and the test of product flame retardant properties is by the UL94-5VA level.Product can be widely used in the protection and the lining of electric wire, high-performing car wire harness, electronics, mechanical wire harness, instrument, the connection of housing cabling etc., can substitute part fluorine material and silicon rubber, possesses stronger price advantage in the high temperature heat shrinkable pipe material.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment
A kind of olefines rubber high flame retardant oil resistant heat-shrinkable T bush and preparation method thereof, this preparation method may further comprise the steps successively:
The first step: product pellet preparation: in Banbury mixer, add the 60-80KgEPDM(ethylene-propylene diene copolymer by the following stated order, Japan's import, model EP57P), 20-10KgEEA, 20-10KgPOE, 5-10Kg methyl vinyl silicone rubber, start Banbury mixer then, 80-130 ℃ of banburying temperature, banburying 1-2 minute; Adding 100-120Kg magnesium hydroxide, 5-10Kg zinc borate, 0.5-1Kg methyl phenyl silicone oil, 0.3-0.6Kg oxidation inhibitor 1,0.2-0.3Kg, oxidation inhibitor 2,0.2-0.3Kg, linking agent TMPTMA, 3-5Kg10 white oil, 0.5-1Kg zinc stearate, 1-2Kg paraffin then joins in the Banbury mixer, continue banburying 7-8 minute, the material that banburying is good is drained in the parallel double-screw granulation unit after allowing, melt extrude, die face cutting under water, particle dehydration back oven dry is prepared into the product pellet; The working temperature of forcing machine is: 110 ± 5 ℃ in a district, 120 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 145 ± 5 ℃ in four districts, 120 ± 5 ℃ in five districts.
Second step: the extruding of linear polymer heat-shrink tube: the plastic pellet for preparing is joined in the single screw extrusion machine, extrude all slick tubing of inside and outside wall, the tubing of extruding is wrapped on the take-up reel.The working temperature of single screw extrusion machine is: 100 ± 5 ℃ in a district, 125 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 125 ± 5 ℃ in four districts, 110 ± 5 ℃ in five districts.
The 3rd step: the cross-linking radiation of heat-shrink tube: the tubing that will extrude carries out cross-linking radiation through rumbatron and becomes cross-linked thermoset polymer, and irradiation dose is 15-18Mrad;
The 4th step: tubing add thermal enlargement: the tubing behind the cross-linking radiation, expands the expansion temperature through heating dilator continuously: 130 ± 10 ℃, the water cooling typing of expansion back obtains finished product at last.
The used starting material explanation of the present invention:
EPDM:The graft modification ethylene-propylene diene copolymer, grafted monomer: the AN(vinyl cyanide), percentage of grafting 15%
EEA:Ethylene-ethyl acrylate copolymer, EA content 30%
POE:Ethylene-octene copolymer, model POE8656
Silicon rubber:Methyl vinyl silicone rubber
Magnesium hydroxide:The activation rank, high purity, Mg (OH)
2Content 〉=99.99%, specific surface area: 4.0-6.0m
2/ g, particle size: 0.7-1.0 μ m.
Zinc borate:Halogen-free flame retardants, first grade
Methyl phenyl silicone oil:Lubricant
Oxidation inhibitor 1:Be antioxidant 300 or 70% antioxidant 1010+30% oxidation inhibitor DSTDP
Oxidation inhibitor 2:60% oxidation inhibitor PNX102+20% oxidation inhibitor 168+20% oxidation inhibitor PS800
Linking agent TMPTMA:Trimethylolpropane trimethacrylate
White oil:No. 10 white oils, lubricant
Zinic stearas:Activator
Paraffin:Lubricant
Embodiment 1: a kind of olefines rubber high flame retardant oil resistant heat-shrinkable T bush and preparation method thereof, and this preparation method may further comprise the steps successively:
The first step: product pellet preparation: in Banbury mixer, add 60KgEPDM(graft modification ethylene-propylene diene copolymer by the following stated order, grafted monomer: the AN(vinyl cyanide), percentage of grafting 15%), 20KgEEA(ethylene-ethyl acrylate copolymer, EA content 30%, ethyl propenoate content (weight), 20KgPOE(ethylene-octene copolymer, model POE8656), 5Kg methyl vinyl silicone rubber (110-2 type, molecular weight 650000, contents of ethylene 0.16%), start Banbury mixer then, 80-130 ℃ of banburying temperature, banburying 1-2 minute; Adding 100 Kg magnesium hydroxides, 5Kg zinc borate, 0.5Kg methyl phenyl silicone oil, 0.2Kg oxidation inhibitor 1 (70% antioxidant 1010+30% oxidation inhibitor DSTDP), 0.2Kg oxidation inhibitor 2,0.3Kg linking agent TMPTMA, 3Kg white oil, 0.5Kg zinc stearate, 1Kg paraffin then joins in the Banbury mixer, continue banburying 7-8 minute, the material that banburying is good is drained in the parallel double-screw granulation unit after allowing, melt extrude, die face cutting under water, particle dehydration back oven dry is prepared into the product pellet; The working temperature of forcing machine is: 110 ± 5 ℃ in a district, 120 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 145 ± 5 ℃ in four districts, 120 ± 5 ℃ in five districts.
Second step: the extruding of linear polymer heat-shrink tube: the plastic pellet for preparing is joined in the single screw extrusion machine, extrude all slick tubing of inside and outside wall, the tubing of extruding is wrapped on the take-up reel.The working temperature of single screw extrusion machine is: 100 ± 5 ℃ in a district, 125 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 125 ± 5 ℃ in four districts, 110 ± 5 ℃ in five districts.
The 3rd step: the cross-linking radiation of heat-shrink tube: the tubing that will extrude carries out cross-linking radiation through rumbatron and becomes cross-linked thermoset polymer, and irradiation dose is 15-18Mrad;
The 4th step: tubing add thermal enlargement: the tubing behind the cross-linking radiation, expands through heating dilator continuously, add the thermal enlargement temperature: 130 ± 10 ℃, the water cooling typing of expansion back obtains finished product at last.
Embodiment 2:
With embodiment 1, asynchronous is the first step: get 80KgEPDM, 10KgEEA, 10KgPOE, 10Kg methyl vinyl silicone rubber, 120Kg magnesium hydroxide, 10Kg zinc borate, 1Kg methyl phenyl silicone oil, 0.3Kg oxidation inhibitor 1 (antioxidant 300), 0.3Kg oxidation inhibitor 2,0.6Kg linking agent TMPTMA, 5Kg white oil, 1Kg zinc stearate, 2Kg paraffin.
Embodiment 3:
With embodiment 1, different is the first step: get 70KgEPDM, 15KgEEA, 15KgPOE, 8Kg methyl vinyl silicone rubber, start Banbury mixer then, 80-130 ℃ of banburying temperature, banburying 1-2 minute; Add 110Kg magnesium hydroxide, 8Kg zinc borate, 0.8Kg methyl phenyl silicone oil, 0.25Kg oxidation inhibitor 1,0.25Kg oxidation inhibitor 2,0.5Kg linking agent TMPTMA, 5Kg white oil, 0.8Kg zinc stearate, 1.5Kg paraffin then.
Claims (3)
1. the preparation method of an olefines rubber high flame retardant oil resistant heat-shrinkable T bush may further comprise the steps:
The first step: product pellet preparation: EPDM, EEA, POE, methyl vinyl silicone rubber, magnesium hydroxide, zinc borate, methyl phenyl silicone oil, composite antioxidant, linking agent TMPTMA, white oil, zinc stearate and paraffin are joined in the Banbury mixer, temperature 80-130 ℃, banburying 8-10 minute, then that banburying is good material is drained in the parallel double-screw granulation unit, melt extrude, die face cutting is dried after the particle dehydration under water, obtains the product pellet; The working temperature of forcing machine is: 110 ± 5 ℃ in a district, 120 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 145 ± 5 ℃ in four districts, 120 ± 5 ℃ in five districts; The ratio of used EPDM, EEA, POE, methyl vinyl silicone rubber, magnesium hydroxide, zinc borate, methyl phenyl silicone oil, oxidation inhibitor, linking agent TMPTMA, white oil, zinc stearate, paraffin is: 60-80:20-10:20-10:5-10:100-120:5-10:0.5-1:0.3-0.6:0.3-0.6:3-5:0.5-1:1-2;
Second step: the extruding of linear polymer heat-shrink tube: the plastic pellet for preparing is joined in the single screw extrusion machine, extrude all slick tubing of inside and outside wall, the tubing of extruding is wrapped on the take-up reel; The working temperature of single screw extrusion machine is: 100 ± 5 ℃ in a district, 125 ± 5 ℃ in two districts, 135 ± 5 ℃ in three districts, 125 ± 5 ℃ in four districts, 110 ± 5 ℃ in five districts;
The 3rd step: the cross-linking radiation of heat-shrink tube: the tubing that will extrude carries out cross-linking radiation through rumbatron and becomes cross-linked thermoset polymer, and irradiation dose is 15-18Mrad;
The 4th step: tubing add thermal enlargement: the tubing behind the cross-linking radiation, expands the expansion temperature through heating dilator continuously: 130 ± 10 ℃, the water cooling typing of expansion back obtains finished product olefines rubber high flame retardant oil resistant heat-shrinkable T bush.
2. preparation method according to claim 1 is characterized in that: described oxidation inhibitor is made up of oxidation inhibitor 1 and oxidation inhibitor 2, and the consumption weight ratio of oxidation inhibitor 1 and oxidation inhibitor 2 is: 1:0.66-1:1.5; Oxidation inhibitor 1 is antioxidant 300 or is the mixture of 70wt% antioxidant 1010 and 30wt% oxidation inhibitor DSTDP that oxidation inhibitor 2 is the mixture of 60wt% oxidation inhibitor PNX102,20wt% oxidation inhibitor 168 and 20wt% oxidation inhibitor PS800.
3. the olefines rubber high flame retardant oil resistant heat-shrinkable T bush that makes by claim 1 or 2 described methods.
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| CN 201110163950 CN102276928B (en) | 2011-06-17 | 2011-06-17 | Olefin rubber high-flame-retardant oil-resistant heat-shrinkable bush and preparation method thereof |
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| CN 201110163950 CN102276928B (en) | 2011-06-17 | 2011-06-17 | Olefin rubber high-flame-retardant oil-resistant heat-shrinkable bush and preparation method thereof |
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| CN102786743A (en) * | 2012-06-18 | 2012-11-21 | 青岛科技大学 | High and low temperature resistant and oil resistant blending material and preparation method thereof |
| CN103087373A (en) * | 2012-06-11 | 2013-05-08 | 深圳市沃尔核材股份有限公司 | Radiation crosslinked chloroprene rubber heat shrinkable tube and production method thereof |
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| CN103087373A (en) * | 2012-06-11 | 2013-05-08 | 深圳市沃尔核材股份有限公司 | Radiation crosslinked chloroprene rubber heat shrinkable tube and production method thereof |
| CN102786743A (en) * | 2012-06-18 | 2012-11-21 | 青岛科技大学 | High and low temperature resistant and oil resistant blending material and preparation method thereof |
| CN102786743B (en) * | 2012-06-18 | 2015-05-20 | 青岛科技大学 | High and low temperature resistant and oil resistant blending material and preparation method thereof |
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