CN105218898B - Preparation method for radiation-crosslinked oil-resistant thermal shrink material - Google Patents
Preparation method for radiation-crosslinked oil-resistant thermal shrink material Download PDFInfo
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- CN105218898B CN105218898B CN201510785889.3A CN201510785889A CN105218898B CN 105218898 B CN105218898 B CN 105218898B CN 201510785889 A CN201510785889 A CN 201510785889A CN 105218898 B CN105218898 B CN 105218898B
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Abstract
The invention relates to a preparation method for a radiation-crosslinked oil-resistant thermal shrink material. According to the radiation-crosslinked oil-resistant thermal shrink material, the technical problem that the current radiation-crosslinked oil-resistant thermal shrink material does not have high oil resistance, ageing resistance, high strength and relatively good flexibility simultaneously is solved. The radiation-crosslinked oil-resistant thermal shrink material comprises nitrile rubber, an ethylene-vinyl acetate copolymer, chlorinated polyethylene, an antioxidant, zinc oxide, stearic acid, carbon black, a flame retardant, a crosslinking aid and a plasticizer. The preparation method comprises the following steps: (1) mixing and granulating; (2) extruding particles granulated in the step (1) into a tubular material; (3) carrying out electron beam radiation crosslinking on the tubular material by virtue of an electron accelerator; and (4) heating the tubular material in an infrared heating tank, radially expanding the heated tubular material by virtue of an expansion machine, cooling and shaping by virtue of water, and trimming the tubular material by virtue of a slicer. The preparation method is applied to the preparation of the radiation-crosslinked oil-resistant thermal shrink material.
Description
Technical field
The present invention relates to a kind of preparation method of crosslinking with radiation oil resistant material contracting with heat.
Background technology
In general, elastomeric material has relatively low glass transition temperature, and being difficult to prepare at normal temperatures has thermal contraction
Property material, but want just be prepared by rubber and thermoplastic resin into heat-shrinkage material using some characteristics of rubber.
The main VITON type oil resistant heat-shrinkable tubes and specific rubber with fluorubber as primary raw material of existing oil resistant material contracting with heat is at present
The DR oil resistant heat-shrink tubes of raw material, their oil resistances do not reach GB12528.11-2003 standards far, and expensive.At present
Some Patents are such as：It is common using ethene, ethylene-vinyl acetate copolymer and ethene ternary in Chinese patent CN103044744A
Semihard oil resistant material contracting with heat prepared by polymers, hardness is higher but intensity is relatively low, there is its limitation applied.Chinese patent
Using haloflex for primary raw material prepares material contracting with heat in CN103709539A, due to haloflex decomposition temperature in itself
Degree is relatively low to have a strong impact on its heat aging performance.It is prepared by primary raw material that polyethylene is utilized in Chinese patent CN102532643A
Oil resistant material contracting with heat under high temperature mineral oil environment can vast scale it is swelling and influence basic performance.Accordingly, it would be desirable to develop one
Oil resistant kind high, ageing-resistant, high intensity and flexible preferably material contracting with heat.
The content of the invention
The present invention is cannot be ageing-resistant while meet oil resistant high in order to solve current crosslinking with radiation oil resistant material contracting with heat,
High intensity and flexible preferably technical problem, and a kind of preparation method of crosslinking with radiation oil resistant material contracting with heat is provided.
A kind of crosslinking with radiation oil resistant material contracting with heat of the invention by weight by 40 parts~60 parts of nitrile rubber, 30 parts
~50 parts of vinyl-vinyl acetate copolymer, 0 part~20 parts haloflexes, 1 part~3 parts of antioxidant, 3 parts~5 parts
Zinc oxide, 1 part~2 parts of stearic acid, 5 parts~15 parts of carbon black, 10 parts~60 parts of fire retardant, 1 part~3 parts of assistant crosslinking agent
Plasticizer composition with 4 parts~6 parts.
A kind of preparation method of crosslinking with radiation oil resistant material contracting with heat of the invention is carried out according to the following steps：
First, mixing granulator：By weight by 40 parts~60 parts of nitrile rubber, 30 parts~50 parts of ethylene-acetate second
Enoate copolymer, 0 part~20 parts haloflexes, 1 part~3 parts of antioxidant, 3 parts~5 parts of zinc oxide, 1 part~2 parts hard
Resin acid, 5 parts~15 parts of carbon black, 10 parts~60 parts of fire retardant, 1 part~3 parts of assistant crosslinking agent and 4 parts~6 parts of plasticizer
In input double roll mill, 10min~15min is kneaded under conditions of preceding roll temperature is 130 DEG C and rear roll temperature is 140 DEG C,
Then granulated in comminutor, obtain hybrid particles；
The 2nd, step one is granulated the particle extrusion molding for obtaining with extruder turns into tubing；
3rd, the tubing for being obtained step 2 with electron accelerator is 1.2MeV~4MeV, irradiation dose in beam energy
It is that 80kGy~200kGy and radiation dose rate are to carry out crosslinking electron beam irradiation under conditions of 10kGy/min~20kGy/min,
Insoluble three-dimensional net structure tubing is not melted；
4th, the insoluble three-dimensional net structure tubing that do not melt that step 3 is obtained is placed in infrared heating case, is in temperature
10min~20min is heated under conditions of 130 DEG C~140 DEG C, radial direction expansion then is carried out to the tubing after heating using expansion machinery
, be water-cooled sizing, then with cutting knife deburring after, obtain crosslinking with radiation oil resistant material contracting with heat.
The present invention uses the preferable nitrile rubber of oil resistivity and vinyl-vinyl acetate copolymer as stock, it
All architectural features with radiation-cross-linkable, because vinyl-vinyl acetate copolymer has certain crystal property, can be with
Can change to freeze and discharge the entropy elastic force of cross-linked network, with the molecule for preparing material contracting with heat for shape-memory material is provided
Structural requirement, but their solubility parameter is respectively 21.1 (J/cm3)1/2With 16.72 (J/cm3)1/2, differ larger, it is necessary to enter
Row increase-volume is processed.The present invention is using crosslinking electron beam irradiation and its with the addition method that is combined of compatilizer haloflex to fourth
The compatibility of nitrile rubber and vinyl acetate resins intermingling material optimizes treatment, and original blending is broken from structure
The interface cohesion mode of material, forms firm chemical bonding, so as to improve based on nitrile rubber and ethane-acetic acid ethyenyl ester
Phase region stability between copolymer, makes the mechanics of material, and the performance such as heat-resisting is greatly improved, and may be made with oil resistant
The functional high molecule material of the thermal shape memory of performance, is expected to solve asking for the supporting material contracting with heat oil resistant difference of oil resistant cable
Topic, import substitutes, its meaning is very great.
Advantages of the present invention：
Crosslinking with radiation oil resistant material contracting with heat in the present invention has preferable oil resistance, through No. 2 standard oils in 100 DEG C of warps
The aging after-drawing strength retentions of 70h are crossed better than 65%, elongation at break conservation rate is better than 70%；Pyrocondensation material prepared by the present invention
Material has preferable heat endurance, and at 121 DEG C after 168h is aging, stretching strength retentivity is better than 85%, elongation at break
Conservation rate is better than 65%；The present invention prepare material contracting with heat normal temperature Tensile strength be better than 13MPa, elongation at break 250%~
400%, Shore A hardness 80~95, specific insulation is more than 1 × 1014Ω cm, with mechanical strength it is big, it is flexible the features such as,
Can be used for oil resistant cable annex and require the environment and occasion of oil resistant, there is good industrialization prospect.
Specific embodiment：
Specific embodiment one：Present embodiment is a kind of crosslinking with radiation oil resistant material contracting with heat, by weight by 40 parts
~60 parts of nitrile rubber, 30 parts~50 parts of vinyl-vinyl acetate copolymer, 0 part~20 parts haloflexes, 1 part~3
Part antioxidant, 3 parts~5 parts of zinc oxide, 1 part~2 parts of stearic acid, 5 parts~15 parts of carbon black, 10 parts~60 parts fire-retardant
Agent, 1 part~3 parts of assistant crosslinking agent and 4 parts~6 parts of plasticizer composition.
Specific embodiment two：Present embodiment is with the difference of specific embodiment one：In described nitrile rubber
The mass fraction of acrylonitrile is 34%~46%.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment is with the difference of specific embodiment one or two：Described ethene-second
The mass fraction of the vinyl acetate of vinyl acetate copolymer is 14%~22%.Other and specific embodiment one or two-phase
Together.
Specific embodiment four：Present embodiment is with the difference of specific embodiment one to three：Described chlorination gathers
The mass fraction of the chlorine of ethene is 35%~40%.Other are identical with specific embodiment one to three.
Specific embodiment five：Present embodiment is with the difference of specific embodiment one to four：Described antioxidant is
One or two mixture in antioxidant 1010 and irgasfos 168.Other are identical with specific embodiment one to four.
Specific embodiment six：Present embodiment is with the difference of specific embodiment one to five：Described fire retardant is
One or two mixture in silane coupler modified magnesium hydroxide and silane coupler modified aluminium hydroxide.Other
It is identical with specific embodiment one to five.
Specific embodiment seven：Present embodiment is with the difference of specific embodiment one to six：Described assistant crosslinking agent
It is trimethylol-propane trimethacrylate or trimethylolpropane trimethacrylate.Other and specific embodiment one to six
It is identical.
Specific embodiment eight：Present embodiment is with the difference of specific embodiment one to seven：Described plasticizer is
Dioctyl phthalate or dibutyl phthalate.Other are identical with specific embodiment one to seven.
Specific embodiment nine：Present embodiment is a kind of preparation method of crosslinking with radiation oil resistant material contracting with heat, specifically
Carry out according to the following steps：
First, mixing granulator：By weight by 40 parts~60 parts of nitrile rubber, 30 parts~50 parts of ethylene-acetate second
Enoate copolymer, 0 part~20 parts haloflexes, 1 part~3 parts of antioxidant, 3 parts~5 parts of zinc oxide, 1 part~2 parts hard
Resin acid, 5 parts~15 parts of carbon black, 10 parts~60 parts of fire retardant, 1 part~3 parts of assistant crosslinking agent and 4 parts~6 parts of plasticizer
In input double roll mill, 10min~15min is kneaded under conditions of preceding roll temperature is 130 DEG C and rear roll temperature is 140 DEG C,
Then granulated in comminutor, obtain hybrid particles；
The 2nd, step one is granulated the particle extrusion molding for obtaining with extruder turns into tubing；
3rd, the tubing for being obtained step 2 with electron accelerator is 1.2MeV~4MeV, irradiation dose in beam energy
It is that 80kGy~200kGy and radiation dose rate are to carry out crosslinking electron beam irradiation under conditions of 10kGy/min~20kGy/min,
Insoluble three-dimensional net structure tubing is not melted；
4th, the insoluble three-dimensional net structure tubing that do not melt that step 3 is obtained is placed in infrared heating case, is in temperature
10min~20min is heated under conditions of 130 DEG C~140 DEG C, radial direction expansion then is carried out to the tubing after heating using expansion machinery
, be water-cooled sizing, then with cutting knife deburring after, obtain crosslinking with radiation oil resistant material contracting with heat.
Specific embodiment ten：Present embodiment is with the difference of specific embodiment nine：
The mass fraction of acrylonitrile is 34%~46% in nitrile rubber described in step one；
The mass fraction of the vinyl acetate of the vinyl-vinyl acetate copolymer described in step one is 14%~22%；
The mass fraction of the chlorine of the haloflex described in step one is 35%~40%；
Antioxidant described in step one is one or two the mixture in antioxidant 1010 and irgasfos 168；
Fire retardant described in step one is silane coupler modified magnesium hydroxide and silane coupler modified hydroxide
One or two mixture in aluminium；
Assistant crosslinking agent described in step one is trimethylol-propane trimethacrylate or trimethylolpropane tris propylene
Acid esters；
Plasticizer described in step one is dioctyl phthalate or dibutyl phthalate.
Other are identical with specific embodiment nine.
Beneficial effects of the present invention are verified by tests below：
Experiment one：This experiment is a kind of preparation method of crosslinking with radiation oil resistant material contracting with heat, is specifically entered according to the following steps
Capable：
First, mixing granulator：By weight by 40 parts of nitrile rubber, 40 parts of vinyl-vinyl acetate copolymer, 20
Part haloflex, 1.8 parts of antioxidant, 3 parts of zinc oxide, 1 part of stearic acid, 15 parts of carbon black, 20 parts of fire retardant,
In 3 parts of assistant crosslinking agent and 5 parts of plasticizer input double roll mill, it is 140 DEG C with rear roll temperature to be 130 DEG C in preceding roll temperature
Under conditions of knead 15min, then in comminutor granulate, obtain hybrid particles；
The 2nd, step one is granulated the particle extrusion molding for obtaining with extruder turns into a diameter of 40mm, and tube wall thickness is 3.3mm's
Tubing；
3rd, the tubing for being obtained step 2 with electron accelerator is that 1.2MeV, irradiation dose are in beam energy
140kGy and radiation dose rate are not melted insoluble three dimensional network to carry out crosslinking electron beam irradiation under conditions of 15kGy/min
Network structural tube；
4th, the insoluble three-dimensional net structure tubing that do not melt that step 3 is obtained is placed in infrared heating case, is in temperature
15min is heated under conditions of 130 DEG C, the tubing after heating is radially expanded using expansion machinery then, it is fixed to be water-cooled
Type, then with cutting knife deburring after, obtain the thermal contraction casing tube of a diameter of 80mm.
The mass fraction of acrylonitrile is 41.5% in nitrile rubber described in step one；
The mass fraction of the vinyl acetate of the vinyl-vinyl acetate copolymer described in step one is 14%；
The mass fraction of the chlorine of the haloflex described in step one is 40%；
1.8 parts described in step one of antioxidant is made up of 1.2 parts of antioxidant 1010 and 0.6 part of irgasfos 168；
Fire retardant described in step one is silane coupler modified magnesium hydroxide；
Assistant crosslinking agent described in step one is trimethylolpropane trimethacrylate；
Plasticizer described in step one is dioctyl phthalate.
After the thermal contraction casing tube of a diameter of 80mm prepared by experiment one is put into 130 DEG C of baking oven retraction, test material
Energy：Ambient temperature mechanical properties：Tensile strength 19.5Mpa, elongation at break 300%；Shape recovery rate 100%；Shore A hardness 90；
Specific insulation 2.4 × 1014Ω·cm；At 121 DEG C by after 168h hot air agings, stretching strength retentivity 95% is broken
Percent retention of elongation 70%；Through No. 2 standard oils at 100 DEG C after 72h is aging, stretching strength retentivity 70%, extension at break
Rate conservation rate 80%.
Experiment two：This experiment is a kind of preparation method of crosslinking with radiation oil resistant material contracting with heat, is specifically entered according to the following steps
Capable：
First, mixing granulator：By weight by 50 parts of nitrile rubber, 50 parts of vinyl-vinyl acetate copolymer,
2.4 parts of antioxidant, 5 parts of zinc oxide, 1.75 parts of stearic acid, 10 parts of carbon black, 30 parts of fire retardant, 3 parts help crosslinking
In agent and 5 parts of plasticizer input double roll mill, mixed under conditions of preceding roll temperature is 130 DEG C and rear roll temperature is 140 DEG C
Refining 15min, then granulates in comminutor, obtains hybrid particles；
The 2nd, step one is granulated the particle extrusion molding for obtaining with extruder turns into a diameter of 40mm, and tube wall thickness is 3.3mm's
Tubing；
3rd, the tubing for being obtained step 2 with electron accelerator is that 1.2MeV, irradiation dose are in beam energy
180kGy and radiation dose rate are not melted insoluble three dimensional network to carry out crosslinking electron beam irradiation under conditions of 15kGy/min
Network structural tube；
4th, the insoluble three-dimensional net structure tubing that do not melt that step 3 is obtained is placed in infrared heating case, is in temperature
15min is heated under conditions of 130 DEG C, the tubing after heating is radially expanded using expansion machinery then, it is fixed to be water-cooled
Type, then with cutting knife deburring after, obtain the thermal contraction casing tube of a diameter of 80mm.
The mass fraction of acrylonitrile is 41.5% in nitrile rubber described in step one；
The mass fraction of the vinyl acetate of the vinyl-vinyl acetate copolymer described in step one is 18%；
2.4 parts described in step one of antioxidant is made up of 1.8 parts of antioxidant 1010 and 0.6 part of irgasfos 168；
Fire retardant described in step one is silane coupler modified magnesium hydroxide；
Assistant crosslinking agent described in step one is trimethylolpropane trimethacrylate；
Plasticizer described in step one is dioctyl phthalate.
After the thermal contraction casing tube of a diameter of 80mm prepared by experiment one is put into 130 DEG C of baking oven retraction, test material
Energy：Ambient temperature mechanical properties：Tensile strength 16.5Mpa, elongation at break 320%；Shape recovery rate 100%；Shore A hardness 88；
Specific insulation 3.5 × 1014Ω·cm；At 121 DEG C by after 168h hot air agings, stretching strength retentivity 95% is broken
Percent retention of elongation 80%；Through No. 2 standard oils at 100 DEG C after 72h is aging, stretching strength retentivity 72%, extension at break
Rate conservation rate 83%.
Claims (1)
1. a kind of preparation method of crosslinking with radiation oil resistant material contracting with heat, it is characterised in that the preparation of crosslinking with radiation oil resistant material contracting with heat
Method is carried out according to the following steps：
First, mixing granulator：By weight by 40 parts of nitrile rubber, 40 parts of vinyl-vinyl acetate copolymer, 20 parts
Haloflex, 1.8 parts of antioxidant, 3 parts of zinc oxide, 1 part of stearic acid, 15 parts of carbon black, 20 parts of fire retardant, 3 parts
Assistant crosslinking agent and 5 parts of plasticizer input double roll mill in, be 130 DEG C in preceding roll temperature and rear roll temperature be 140 DEG C
Under the conditions of knead 15min, then in comminutor granulate, obtain hybrid particles；
The 2nd, step one is granulated the particle extrusion molding for obtaining with extruder turns into a diameter of 40mm, and tube wall thickness is the pipe of 3.3mm
Material；
3rd, the tubing for being obtained step 2 with electron accelerator beam energy be 1.2MeV, irradiation dose be 140kGy and
Radiation dose rate is not melted insoluble three-dimensional net structure pipe to carry out crosslinking electron beam irradiation under conditions of 15kGy/min
Material；
4th, the insoluble three-dimensional net structure tubing that do not melt that step 3 is obtained is placed in infrared heating case, is 130 DEG C in temperature
Under conditions of heat 15min, then using expansion machinery the tubing after heating is radially expanded, be water-cooled sizing, so
Afterwards with after cutting knife deburring, the thermal contraction casing tube of a diameter of 80mm is obtained；
The mass fraction of acrylonitrile is 41.5% in nitrile rubber described in step one；
The mass fraction of the vinyl acetate of the vinyl-vinyl acetate copolymer described in step one is 14%；
The mass fraction of the chlorine of the haloflex described in step one is 40%；
1.8 parts described in step one of antioxidant is made up of 1.2 parts of antioxidant 1010 and 0.6 part of irgasfos 168；
Fire retardant described in step one is silane coupler modified magnesium hydroxide；
Assistant crosslinking agent described in step one is trimethylolpropane trimethacrylate；
Plasticizer described in step one is dioctyl phthalate；
After the thermal contraction casing tube of described a diameter of 80mm is put into 130 DEG C of baking oven retraction, ambient temperature mechanical properties：Tensile strength
19.5Mpa, elongation at break 300%；Shape recovery rate 100%；Shore A hardness 90；Specific insulation 2.4 × 1014Ω·cm；
At 121 DEG C by after 168h hot air agings, stretching strength retentivity 95%, elongation at break conservation rate 70%；Through No. 2 standards
Oil at 100 DEG C after 72h is aging, stretching strength retentivity 70%, elongation at break conservation rate 80%.
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| CN101696293A (en) * | 2009-10-28 | 2010-04-21 | 江苏达胜热缩材料有限公司 | Semi-conducting low-medium voltage fire retardant single-wall heat-shrinkable tube and preparation method thereof |
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| CN103073756A (en) * | 2013-01-19 | 2013-05-01 | 北京化工大学 | High-ductility, low-smoke, environment-friendly, flame-retardant and oil-proof cable material |
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5929070B2 (en) * | 2011-09-22 | 2016-06-01 | 横浜ゴム株式会社 | Expandable rubber composition for tire and method for producing foam |
| CN104212051A (en) * | 2014-09-04 | 2014-12-17 | 扬州市好年华橡塑有限公司 | 90 DEG C irradiation cross-linked, low-smoke, halogen-free and flame-retardant polyolefin oil-resistant cable material and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696293A (en) * | 2009-10-28 | 2010-04-21 | 江苏达胜热缩材料有限公司 | Semi-conducting low-medium voltage fire retardant single-wall heat-shrinkable tube and preparation method thereof |
| CN102504367A (en) * | 2011-11-05 | 2012-06-20 | 天津鹏翎胶管股份有限公司 | Chemigum composition for preparing rubber flexible pipe |
| CN103073756A (en) * | 2013-01-19 | 2013-05-01 | 北京化工大学 | High-ductility, low-smoke, environment-friendly, flame-retardant and oil-proof cable material |
| CN103589008A (en) * | 2013-10-15 | 2014-02-19 | 广东奥美格传导科技股份有限公司 | Irradiation-crosslinked wear-resistant oil-resistant cable |
| CN103694551A (en) * | 2013-12-21 | 2014-04-02 | 深圳市沃尔核材股份有限公司 | Irradiation crosslinking environment-friendly fire-retardant material for non-foaming pipe wall in heat shrinkage and application thereof |
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