CN105086015A - Radiation crosslinking low smoke halogen-free flame-retardant low temperature shrinkable polyolefin heat shrinkable materials - Google Patents
Radiation crosslinking low smoke halogen-free flame-retardant low temperature shrinkable polyolefin heat shrinkable materials Download PDFInfo
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- CN105086015A CN105086015A CN201510549844.6A CN201510549844A CN105086015A CN 105086015 A CN105086015 A CN 105086015A CN 201510549844 A CN201510549844 A CN 201510549844A CN 105086015 A CN105086015 A CN 105086015A
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Abstract
The invention provides radiation crosslinking polyolefin heat shrinkable materials which are low smoke halogen-free flame-retardant and are shrinkable when the temperature is less than 50 DEG C. The radiation crosslinking polyolefin heat shrinkable materials are prepared by mixing trans-1,4-polyisoprene, special rubber white carbon black, a complex antioxidant, a halogen-free flame retardant, an antismoke agent, a lubricant and a cross-linking agent, extruding and granulating, extruding and forming a tube, and radiation crosslinking. The radiation crosslinking polyolefin heat shrinkable materials can be made into heat shrinkable devices, the performance is good, the raw materials are easy to obtain, the preparation method is simple, the price is low, and the materials are suitable for industrial production.
Description
Technical field
The present invention relates to a kind of low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation and preparation method thereof, can be used for thermal contraction device.
Background technology
The shrinkage temperature of current commercial radiation cross-linking flame-retardant polyolefin heat-shrinkable material is generally more than 120 DEG C, but at some special occasions, as precision electronic element or medical macromolecular materials, shrink under such high temperatures easily make electronic component or living organism impaired, therefore need shrinkage temperature at 90 DEG C and following in these occasions.So Low Temperature Thermal shrink-down material is succeeded in developing in market in succession.The LRS-1 type low-temperature heat-shrinkage tube that company limited of Changchun Pyrocondensation produces belonging to Changchun Inst. of Applied Chemistry, Chinese Academy of Sciences is made up of crosslinked polyolefin materials, and shrinkage temperature is 90 DEG C.The A-1 of Woosuck company of Korea S, A-2, A-4, A-5 type flame-retardant polyolefin heat-shrinkable material, Korea S KDK company limited A-4 type flame-retardant polyolefin heat-shrinkable material, the RT-102 of Raychem company of the U.S., the flame-retardant polyolefin heat-shrinkable materials such as RT-876, their shrinkage temperature is all at 90 DEG C or following.But these products all adopt halogen containing flame-retardant, poisonous, mordant hydrogen halide in a large number will be produced during halogen containing flame-retardant burning, and be easy to etching electronic element or organic object, cause secondary disaster.Although the company also had develops not halogen-containing polyolefin heat-shrinkable material, as the A-2HF type environment protection polyolefin heat-shrinkable material of KDK company limited of Korea S, it is not again low-temperature shrink (product description see each enterprise).So people expect to have one, and not only low cigarette was not halogen-containing fire-retardant but also can (≤90 DEG C) flame-retardant polyolefin heat-shrinkable material of shrinking at a lower temperature.
Patent CN101108909A disclose a kind of low-smoke non-halogen flame-retardant and under lesser temps (≤90 DEG C) contractile irradiated crosslinked polyalkene heat-shrinkage material.System is by ethylene-vinyl acetate copolymer, and terpolymer EP rubber and oxidation inhibitor, halogen-free flame retardants, smoke suppressor, lubricant and crosslinking coagent through mixing extruding pelletization, then are extruded into pipe, form through radiation crosslinking.But it is the shrink-down material of 90 DEG C, does not belong to low-temperature shrink.Due to some special occasions, as needs such as medical treatment, need to develop the lower shrink-down material of shrinkage temperature.
Summary of the invention
For the problems referred to above, the invention provides a kind of Novel radiation cross-linking flame-retardant polyolefin heat-shrinkable material, there is low-smoke non-halogen flame-retardant and the heat-shrinkage material lower than the large function of 50 DEG C of low-temperature shrinks two.
The invention provides the method preparing above-mentioned low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation.
Meanwhile, the invention provides the purposes of above-mentioned low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation.
Low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation of the present invention is made up of than ground material following weight:
Above-mentioned substance is all commercially available.
Wherein, anti-form-1, the weight ratio of 4-polyisoprene can be 30,35,40,45,50,55 or 60 etc.
The weight ratio of specialty elastomer can be 40,45,50,55 or 60 etc.
The weight ratio of White Carbon black can be 5,7,10,13 or 15 etc.
The weight ratio of composite antioxidant can be 0.5,1,1.5,2,2.5,3,3.5 or 4 etc.
The weight ratio of efficient halogen-free anti-inflaming agent can be 5,6,7,8,9 or 10 etc.
The weight ratio of trimeric cyanamide complex compound can be 10,13,15,17 or 20 etc.
Smoke suppressor MoO
3weight ratio can be 0,1,2,3,4 or 5 etc.
The weight ratio of lubricant divalent metal Metallic stearates can be 1,1.5,2,2.5 or 3 etc.
The weight ratio of polyfunctional group (methyl) acrylate can be 1,1.5,2,2.5 or 3 etc.
The weight ratio of colour batch can be 0,1,2,3,4 or 5 etc.
The commercially available composite antioxidant sold, recommend the composite antioxidant adopting the weight ratio of phenolic antioxidant and ester kind antioxidant to be followed successively by 0.5: 1 ~ 3, wherein weight ratio can be 0.5:1,0.5:1.5,0.5:2,0.5:2.5 or 0.5:3 etc.
Preferably, described specialty elastomer is the combination that amorphous state, nodeless mesh or degree of crystallinity to be less than in the rubber of 10% any one or at least two kinds, the typical but non-limiting example of described combination has: the combination of the rubber of amorphous state and nodeless mesh, nodeless mesh and degree of crystallinity are less than the combination of the rubber of 10%, and amorphous state, nodeless mesh and degree of crystallinity are less than the combination light of the rubber of 10%; If the degree of crystallinity of specialty elastomer is excessive more than 10%, can make its with anti-form-1, in 4-polyisoprene blending and modifying process, the structure of blend is changed, causes the shrinkage temperature of the finished product to increase.
Described specialty elastomer is ethylene-propylene rubber(EPR), ethene-vinyl acetate rubber, natural rubber, the combination of any one or at least two kinds in styrene-butadiene rubber(SBR) or cis-1,4-polybutadiene rubber, described combination typical case but limiting examples have: the combination of ethylene-propylene rubber(EPR) and ethene-vinyl acetate rubber, the combination of natural rubber and styrene-butadiene rubber(SBR), the combination of styrene-butadiene rubber(SBR) and cis-1,4-polybutadiene rubber, ethylene-propylene rubber(EPR), the combination of ethene-vinyl acetate rubber and natural rubber, the combination of styrene-butadiene rubber(SBR) and cis-1,4-polybutadiene rubber, ethylene-propylene rubber(EPR), the combination of ethene-vinyl acetate rubber and natural rubber, ethylene-propylene rubber(EPR), ethene-vinyl acetate rubber, natural rubber, the combination etc. of styrene-butadiene rubber(SBR) and cis-1,4-polybutadiene rubber.
Above-mentioned ester kind antioxidant can be β-propanedioic acid stearyl (antioxidant 1076), the four seasons four alcohol ester (antioxidant 1010), Tyox B (oxidation inhibitor DLDP), thio-2 acid stearyl (oxidation inhibitor DSTP), β-cyclohexyl propionate (oxidation inhibitor 121), thio-2 acid two (tetradecyl ester) (oxidation inhibitor DMTDP), thio-2 acid two (tridecyl) ester (oxidation inhibitor 711), lauryl-thio-2 acid octadecyl ester mixture (oxidation inhibitor 1212), 1, 3, the combination of any one or at least two kinds in 5-triisocyanate (antioxidant 3114) or trilauryl trithiophosphite (anti-aging agent TLTTP), described combination typical case but limiting examples have: β-propanedioic acid stearyl (antioxidant 1076) and the combination in the four seasons four alcohol ester (antioxidant 1010), the combination of β-cyclohexyl propionate (oxidation inhibitor 121) and thio-2 acid two (tetradecyl ester) (oxidation inhibitor DMTDP), the combination etc. of thio-2 acid two (tridecyl) ester (oxidation inhibitor 711) and lauryl-thio-2 acid octadecyl ester mixture (oxidation inhibitor 1212).。
Phenolic antioxidant (anti-aging agent) can be 2, 4, 6-tri-tert-butylphenol (anti-aging agent Q46), 2, 5-ditert-butylhydro quinone (anti-aging agent NS-7), 4, 4 '-bis-(2, 6-di-tert-butylphenol (anti-aging agent 712), 4, 4 '-methylene-bis (2, 6-di-tert-butylphenol) (anti-aging agent 702), 2, the combination of any one or at least two kinds in 6-di-tert-butyl-4-methylphenol (oxidation inhibitor OC) or styrenated phenol (antioxidant SP), described combination typical case but limiting examples have: 2, 4, 6-tri-tert-butylphenol (anti-aging agent Q46) and 2, the combination of 5-ditert-butylhydro quinone (anti-aging agent NS-7), 4, 4 '-bis-(2, 6-di-tert-butylphenol (anti-aging agent 712) and 4, 4 '-methylene-bis (2, 6-di-tert-butylphenol) combination of (anti-aging agent 702), 2, the combination etc. of 6-di-tert-butyl-4-methylphenol (oxidation inhibitor OC) and styrenated phenol (antioxidant SP).
Described crosslinked resist is polyfunctional group (methyl) acrylate monomer, as Viscoat 295 (TMPTA), trimethylolpropane trimethacrylate (TMPTMA), the combination of any one or at least two kinds in tri (propylene glycol) diacrylate (TPGPA) or pentaerythritol triacrylate (PEPA), described combination typical case but limiting examples have: the combination of Viscoat 295 (TMPTA) and trimethylolpropane trimethacrylate (TMPTMA), the combination etc. of tri (propylene glycol) diacrylate (TPGPA) and pentaerythritol triacrylate (PEPA).
Described colour batch is generally pigment, to convert shades of colour, is convenient to distinguish use.Push away to deposit and add relative weight than the pigment being 1 ~ 4.
The preparation method of low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation of the present invention is by anti-form-1, after 4-polyisoprene and specialty elastomer and white carbon black, composite antioxidant, efficient halogen-free anti-inflaming agent, trimeric cyanamide complex compound, smoke suppressor MoO3, lubricant divalent metal Metallic stearates, polyfunctional group (methyl) acrylate and colour batch carry out blending and modifying, adopt Radiation Crosslinking Method preparation.
Specifically, described preparation method comprises the following steps:
(1) by anti-form-1,4-polyisoprene, specialty elastomer, white carbon black, composite antioxidant, efficient halogen-free anti-inflaming agent, trimeric cyanamide complex compound, smoke suppressor MoO
3, lubricant divalent metal Metallic stearates, polyfunctional group (methyl) acrylate and colour batch carry out mixing after mixing;
(2) mixing uniform forming materials is carried out radiation crosslinking process;
(3) the material hot water through radiation crosslinking process is heated, then carry out stretching or expanding, and cool to room temperature under external force.
Preferably, in described step (1), mixing time is 3 ~ 10min, such as 3min, 5min, 6min, 8min or 10min etc.
Preferably, in described step (2), the irradiation dose of radiation crosslinking process is 5 ~ 30Mard, such as 5Mard, 10Mard, 15Mard, 20Mard, 25Mard or 30Mard etc.
The purposes of described radiation crosslinking flame-retardant polyolefin material, its thermal contraction device comprising heat-shrinkable tube shunk for low-smoke non-halogen flame-retardant and low temperature (30 ~ 55 DEG C).
Low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation of the present invention can be used for preparing various thermal contraction device, comprises heat-shrinkable tube.It not only solves at some special occasions as precision electronic element and all kinds of medical high score material require low-temperature shrink, it can shrink completely at lower than 50 DEG C, also solve over when Halogen flame-retardant heat-shrinkable material burns simultaneously and discharge secondary disaster such as macro-corrosion poisonous hydrogen halide corrosion precision electronic element and organic object etc., the a large amount of smog also solving harm loss of life and personal injury and property damage and generation hinder the problem of rescue and pollutant atmosphere, it is a kind of non-harmful cleaning article of low-smoke non-halogen flame-retardant of environment-friendly type, and its use temperature is high, electrical property is excellent, preparation method is simple and easy, raw material is easily purchased, cheap.So be suitable for suitability for industrialized production.
Embodiment
To contribute to understanding the present invention by following embodiment, but content of the present invention can not be limited.
Embodiment 1:
At mixing facilities 120 DEG C, add anti-form-1,4-polyisoprene 40 parts, adds 50 parts, ethylene-propylene rubber(EPR) successively after plasticating, White Carbon black 7 parts, composite antioxidant 2 parts, efficient halogen-free anti-inflaming agent 7 parts, 15 parts, trimeric cyanamide complex compound, lubricant divalent metal Metallic stearates 1 part, 1 part, trimethylol propane trimethyl vinylformic acid, even post-tensioning of plasticating is in blocks, and pelletizing after cooling, uses twin screw extruder granulation, single screw extrusion machine is extruded into pipe, then uses 20Mrad irradiation dose irradiation.Pipe embryo after irradiation is expanded and is put in place at the temperature of 100 DEG C, cooling and shaping.The complete shrinkage temperature of this Low Temperature Thermal shrink sleeve is 50 DEG C.
Embodiment 2:
At mixing facilities 120 DEG C, add anti-form-1,4-polyisoprene 30 parts, after plasticating, add ethene-vinyl acetate rubber 40 parts successively, White Carbon black 5 parts, composite antioxidant 0.5 part, efficient halogen-free anti-inflaming agent 5 parts, 10 parts, trimeric cyanamide complex compound, smoke suppressor MoO
33 parts, lubricant divalent metal Metallic stearates 2 parts, Viscoat 295 2 parts, colour batch 3 parts, even post-tensioning of plasticating is in blocks, and pelletizing after cooling, uses twin screw extruder granulation, single screw extrusion machine is extruded into pipe, then uses 5Mrad irradiation dose irradiation.Pipe embryo after irradiation is expanded and is put in place at the temperature of 100 DEG C, cooling and shaping.The complete shrinkage temperature of this Low Temperature Thermal shrink sleeve is 45 DEG C.
Embodiment 3:
At mixing facilities 120 DEG C, add anti-form-1,4-polyisoprene 60 parts, after plasticating, add ethene-vinyl acetate rubber 60 parts successively, White Carbon black 15 parts, composite antioxidant 4 parts, efficient halogen-free anti-inflaming agent 10 parts, 20 parts, trimeric cyanamide complex compound, smoke suppressor MoO
35 parts, lubricant divalent metal Metallic stearates 3 parts, Viscoat 295 3 parts, colour batch 5 parts, even post-tensioning of plasticating is in blocks, and pelletizing after cooling, uses twin screw extruder granulation, single screw extrusion machine is extruded into pipe, then uses 30Mrad irradiation dose irradiation.Pipe embryo after irradiation is expanded and is put in place at the temperature of 100 DEG C, cooling and shaping.The complete shrinkage temperature of this Low Temperature Thermal shrink sleeve is 45 DEG C.
Comparative example is the embodiment 1 in patent CN101108909A.
Measure radiation-crosslinked low smoke no halide flame retaining low-temperature shrink polyolefine heat-shrinkable tubular material prepared by above-described embodiment 1-3 and comparative example, result is as shown in table 1.
Table 1: radiation-crosslinked low smoke no halide flame retaining low-temperature shrink polyolefine heat-shrinkable tubular material properties test table
In sum, can find out that low-temp thermoshrinking halogen-free polyolefine material with properties of radiation cross-linking, low smoke and flame retardation of the present invention can be used for preparing various thermal contraction device, comprise heat-shrinkable tube.It not only solves at some special occasions as precision electronic element and all kinds of medical high score material require low-temperature shrink, it can shrink completely at lower than 50 DEG C, also solve over when Halogen flame-retardant heat-shrinkable material burns simultaneously and discharge secondary disaster such as macro-corrosion poisonous hydrogen halide corrosion precision electronic element and organic object etc., the a large amount of smog also solving harm loss of life and personal injury and property damage and generation hinder the problem of rescue and pollutant atmosphere, it is a kind of non-harmful cleaning article of low-smoke non-halogen flame-retardant of environment-friendly type, and its use temperature is high, electrical property is excellent, preparation method is simple and easy, raw material is easily purchased, cheap.So be suitable for suitability for industrialized production.
Applicant states, the present invention illustrates detailed construction feature of the present invention and treatment process by above-described embodiment, but the present invention is not limited to above-mentioned detailed construction feature and treatment process, namely do not mean that the present invention must rely on above-mentioned detailed construction feature and treatment process could be implemented.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the increase of accessory, the concrete way choice etc. of parts selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (9)
1. a polyolefin heat-shrinkable material for radiation crosslinking flame-retardant, is characterized in that, is made up of the material of following weight ratio:
Described composite antioxidant is made up of the oxidation inhibitor of following weight ratio, phenolic antioxidant: ester kind antioxidant=0.5: 1 ~ 3.
2. material as claimed in claim 1, is characterized in that, described specialty elastomer is the combination that amorphous state, nodeless mesh or degree of crystallinity to be less than in the rubber of 10% any one or at least two kinds;
Preferably, described specialty elastomer is the combination of any one or at least two kinds in ethylene-propylene rubber(EPR), ethene-vinyl acetate rubber, natural rubber, styrene-butadiene rubber(SBR) or cis-1,4-polybutadiene rubber.
3. material as claimed in claim 1 or 2, it is characterized in that, described ester kind antioxidant is β-propionic acid octadecyl ester, pentaerythritol tetrathioglycollate, Tyox B, thio-2 acid octadecyl ester, β-cyclohexyl propionate, thio-2 acid two (tetradecyl ester), thio-2 acid two (tridecyl) ester, lauryl-thio-2 acid octadecyl ester mixture, 1,3, the combination of any one or at least two kinds in 5-triisocyanate or trilauryl trithiophosphite.
4. the material as described in any one of claim 1-3, it is characterized in that, described phenolic antioxidant is 2,4,6-tri-tert-butylphenol, 2,5-ditert-butylhydro quinone, 4,4 '-bis-(2,6-di-tert-butylphenol), 4,4 '-methylene-bis (2,6-di-tert-butylphenol), the combination of any one or at least two kinds in 2,6-di-tert-butyl-4-methylphenol or styrenated phenol.
5. the material as described in any one of claim 1-4, it is characterized in that, described multi-functional (methyl) acrylate cross linked dose is Viscoat 295, the combination of any one or at least two kinds in trimethylol propane trimethyl vinylformic acid, tri (propylene glycol) diacrylate or pentaerythritol triacrylate.
6. the preparation method of the polyolefin heat-shrinkable material of the radiation crosslinking flame-retardant as described in any one of claim 1-5, it is characterized in that, described method is by anti-form-1, after 4-polyisoprene and specialty elastomer and white carbon black, composite antioxidant, efficient halogen-free anti-inflaming agent, trimeric cyanamide complex compound, smoke suppressor MoO3, lubricant divalent metal Metallic stearates, polyfunctional group (methyl) acrylate and colour batch carry out blending and modifying, adopt Radiation Crosslinking Method preparation.
7. preparation method as claimed in claim 6, it is characterized in that, described preparation method comprises the following steps:
(1) by anti-form-1,4-polyisoprene, specialty elastomer, white carbon black, composite antioxidant, efficient halogen-free anti-inflaming agent, trimeric cyanamide complex compound, smoke suppressor MoO
3, lubricant divalent metal Metallic stearates, polyfunctional group (methyl) acrylate and colour batch carry out mixing after mixing;
(2) mixing uniform forming materials is carried out radiation crosslinking process;
(3) the material hot water through radiation crosslinking process is heated, then carry out stretching or expanding, and cool to room temperature under external force.
8. preparation method as claimed in claims 6 or 7, is characterized in that, in described step (1), mixing time is 3 ~ 10min;
Preferably, in described step (2), the irradiation dose of radiation crosslinking process is 5 ~ 30Mard.
9. a purposes for the radiation crosslinking flame-retardant polyolefin material as described in any one of claim 1-5, is characterized in that the thermal contraction device comprising heat-shrinkable tube shunk for low-smoke non-halogen flame-retardant and low temperature (30 ~ 55 DEG C).
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|---|---|---|---|---|
| CN106317589A (en) * | 2016-08-18 | 2017-01-11 | 苏州泰斯拓伟机电设备有限公司 | Radiation crosslinking butadiene styrene rubber heat shrink tube and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106317589A (en) * | 2016-08-18 | 2017-01-11 | 苏州泰斯拓伟机电设备有限公司 | Radiation crosslinking butadiene styrene rubber heat shrink tube and preparation method thereof |
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