CN109777086A - A kind of halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting and preparation method thereof - Google Patents
A kind of halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting and preparation method thereof Download PDFInfo
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- CN109777086A CN109777086A CN201910049587.8A CN201910049587A CN109777086A CN 109777086 A CN109777086 A CN 109777086A CN 201910049587 A CN201910049587 A CN 201910049587A CN 109777086 A CN109777086 A CN 109777086A
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Abstract
The invention discloses a kind of halogen-free flameproof polyether polyurethane elastomers of high-temp resisting high-humidity resisting, include following components by mass fraction: 45~65 parts of polyether polyurethane elastomer；10~20 parts of polyolefin plastomers；5~10 parts of compatilizer；0.2~1 part of crosslinking agent；20~30 parts of phosphor nitrogen combustion inhibitor.The present invention select low-crystallinity POP with it is polyurethane elastomer blended, in the case where raw material is easy to get, reduce the adsorption capacity of polymer surfaces and hydrone, it is equipped with chemical reaction crosslinking technology again, it is contemplated that while compatibility, and increase heat-resistant stability, the application is by being added crosslinking agent simultaneously, the every component made crosslinks reaction, to improve the heatproof heat resistance of the application adult, the application is allowed to pass through test in double 85,1000 hours.
Description
Technical field
The present invention relates to macromolecular elastomer Material Fields, and in particular to a kind of halogen-free flameproof polyether-type of high-temp resisting high-humidity resisting
Polyurethane elastomer and preparation method thereof.
Background technique
TPU is by the diisocyanates molecule such as '-diphenylmethane diisocyanate (MDI) or toluene di-isocyanate(TDI) (TDI)
With high molecular material made of macromolecular polyol, the common reactive polymeric of low molecular polylol (chain extender).Its molecular structure
The hard block that is obtained by '-diphenylmethane diisocyanate (MDI) or toluene di-isocyanate(TDI) (TDI) and chain extender reaction with
And diisocyanate molecules and the macromolecular polyol such as '-diphenylmethane diisocyanate (MDI) or toluene di-isocyanate(TDI) (TDI)
React what obtained soft segment was alternately constituted.TPU has brilliant high-tension, high-tensile strength, tough and ageing-resistant characteristic,
Be widely applied with health care, electronic apparatus, industry and sport etc., with incomparable strong of other plastic materials
Spend height, good toughness, wear-resisting, cold-resistant, oil resistant, the characteristics such as water-fast, ageing-resistant, weatherability, at the same he with high waterproofness penetrability,
Many excellent functions such as windproof, cold-proof, antibacterial, mould proof, warming, uvioresistant and energy release.
In the past several years, TPU different cables using it is upper just gradually replace many materials, especially PVC and
Synthetic rubber, such as power cable, it is necessary to winding storage, and the cable unwound under extreme weather conditions outdoors, either
Those needs are pulled in the earth's surface of rock, the cable dragged on desert or ice and snow, or are to need to impregnate in water,
It the cable of specific physicals processing such as need to wind and bend.TPU has unmatched toughness and rigidity, low temperature as cable material
Flexibility, wearability, resistance to environment and weatherability, these characteristics all extend the durability and service life of cable, therefore TPU line
Cable is mainly used in electric power energy cable such as wind-power electricity generation, construction, mining, winding and spring cable；Communication cable such as phone, number
According to, military and fiber optic cables；Geography exploration cable such as land and marine cable, seabed and continental shelf cable；Automotive wire bundle is such as anti-
Locked system-ABS；Industrial cable such as robot cable, signal transmssion line, lorry/steamer/aircraft cable, subway, machine
Field and communal facility cable；Also just like spring wire, image and tone frequency channel wire, medical equipment cable.
Halogen-free flameproof polyether polyurethane elastomer is to measure seldom one in transformed lines show and TPU product inside TPU
Kind subdivision field, but but can not be substituted for specific use, such as automotive wire bundle, automobile parts side
Face.Automotive wire bundle and automobile charging pile cable etc. propose heat-proof water to said material and " two of double eight or five " require, resistance to excessively
Hot water test method be 80 DEG C put 7 days after survey physical property retention rate, it is desirable that the retention rate of tensile strength and elongation at break be greater than etc.
In 75%, and " test method of double eight or five " is material to be put into 85 DEG C, 1000 hours in the climatic chamber of 85% humidity,
Physical property retention rate is surveyed afterwards, it is desirable that the retention rate of tensile strength and elongation at break is more than or equal to 70%.To pass through heat-proof water aging
Test is relatively easy, but wants that " this test of double eight or five " is but very difficult, and halogen-free anti-inflaming polyurethane divides polyether-type and polyester
Type, guards escorting prisoners is his maximum deficiency that polyester-type is water-fast, polyether polyurethane hydrolysis are obviously got well than polyester-type, but existing
Halogen-free flameproof polyether polyurethane, such as the A78P4766 that Hensel is advanced in years, there are also the 1185A FHF of BASF also can't pass this survey
Examination, therefore, how to design it is a kind of can by " the halogen-free flameproof polyether polyurethane elastomer of the test of double eight or five " 1000 hours, with
Meet the problem of requirement of the automobile industry to polyurethane material is this field urgent need to resolve.
Summary of the invention
The technical problem to be solved in the present invention is to provide it is a kind of can be in 85 DEG C, the climatic chamber of 85% humidity
The halogen-free flameproof polyether-type of high-temp resisting high-humidity resisting of the retention rate of 1000 hours tensile strengths and elongation at break more than or equal to 70%
Polyurethane elastomer.
In order to solve the above technical problem, the present invention provides scheme be: a kind of halogen-free flameproof polyethers of high-temp resisting high-humidity resisting
Type polyurethane elastomer, includes following components by mass fraction:
Further, the polyether polyurethane elastomer is by polyether polyol and methyl diphenylene diisocyanate
It is copolymerized.
Further, the polyether polyol is Polyoxypropylene diol or polytetrahydrofuran ether dihydric alcohol.
Further, the crosslinking agent is peroxide cross-linking agent；The compatilizer is maleic anhydride grafted elastomeric.
Further, the elastomer in the maleic anhydride grafted elastomeric is by POP and EVM press matter using rubbe amount ratio 1:1
~1:3 is blended to obtain；The crosslinking agent is 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane, dual-tert-butyl peroxidating
Diisopropyl benzene or phenolic resin.
Further, the phosphor nitrogen combustion inhibitor is hypo-aluminum orthophosphate.
Further, further including the antioxidant of 0.3~0.8 mass parts, the antioxidant includes amine antioxidants and divides
The weight ratio of phosphite antioxidant of the son amount greater than 600, the amine antioxidants and the phosphite antioxidant is 2:5
~1:1.
Further, the amine antioxidants are 4,4'- bis- (propyloxy phenyl base) diphenylamines, the phosphite ester antioxygen
Agent is bis- (2,4-dicumylphenyl) pentaerythritol diphosphites.
The application further provides a kind of system of the halogen-free flameproof polyether polyurethane elastomer of above-mentioned high-temp resisting high-humidity resisting
Preparation Method, comprising the following steps:
S1, the polyether polyurethane elastomer is dried 2~4 hours under the conditions of 70~90 DEG C；
S2, by the polyolefin plastomers and the phosphor nitrogen combustion inhibitor and described poly- after step S1 drying
Ether-based polyurethane elastomer, the compatilizer are 50~200rpm, are uniformly mixed under conditions of 50~60 DEG C；
S3, crosslinking agent is added after mixing velocity is reduced to 30~50rpm, continuess to mix uniform mixed material；
S4, the mixed material is granulated to obtain the halogen-free flameproof polyether-type of the high-temp resisting high-humidity resisting through double screw extruder
Polyurethane elastomer.
Further, drying time is 2~5 hours in the step S1；Incorporation time is 2~5 in the step S2
Minute；Incorporation time is 1~2 minute in the step S3；In the step S4, the conveying section of the double screw extruder
Temperature is 120 DEG C~160 DEG C, and melting cut section temperature is 160 DEG C~180 DEG C, and compression mixing section temperature is 160 DEG C~200 DEG C,
Measuring homogenizing zone temperature is 170 DEG C~190 DEG C, and screw slenderness ratio is 40~48:1,100~200rpm of screw speed.
Beneficial effects of the present invention: the present invention select low-crystallinity POP with it is polyurethane elastomer blended, be easy to get in raw material
In the case where, the adsorption capacity of polymer surfaces and hydrone is reduced, then be equipped with chemical reaction crosslinking technology, it is contemplated that compatibility
While, and heat-resistant stability is increased, while the application crosslinks reaction by the way that crosslinking agent, the every component made is added,
To improve the heatproof heat resistance of the application adult, the application is allowed to pass through test in double 85,1000 hours.
Specific embodiment
The present invention is further explained in the light of specific embodiments, so that those skilled in the art can be preferably
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
It should be understood that the following noun that the application occurs is the special technology noun of this field, art technology
Personnel can be beyond all doubt confirmation the noun meaning:
Double 25, i.e. 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane；
POP, i.e. polyolefin plastomers；
The copolymer of EVM rubber, i.e. ethylene and vinyl acetate is commonly called as second Warburg Pincus rubber.
Embodiment 1
The preparation method is as follows:
S1, after ratio weighs raw material by weight, first by 62 parts of polyether polyurethane elastomer 70~90 DEG C baking oven into
Row drying pretreatment；
S2,10 parts of POP, 5 parts of compatilizer, 20 parts of hypo-aluminum orthophosphate, 0.5 part of antioxidant throwing are uniformly mixed in high mixer；
S3, dried polyether polyurethane elastomer is added, pours into 25 0.5 parts of the crosslinking agent pair dissolved with butanone,
It is again turned on high mixer to be uniformly mixed, 50 DEG C of mixing temperature；
S4, the material mixed obtain high-temp resisting high-humidity resisting 1000 hours improved halogen-free flameproofs through double-screw extruding pelletizing
Polyether polyurethane elastomer.Each area's temperature setting of screw rod are as follows: 150 DEG C of an area, two 160 DEG C of areas, three 170 DEG C of areas, four areas 170
DEG C, five 180 DEG C of areas, six 180 DEG C of areas, seven 180 DEG C of areas, eight 180 DEG C of areas, nine 175 DEG C of areas, ten 175 DEG C of areas, 170 DEG C of head.Screw rod
Revolving speed 150rpm.Wherein, an area~2nd area are material conveying section, and 3rd area~5th area are melting cut section, and 6th area~9th area are pressure
Contracting mixing section, tenth area~11st area are homogenizing metering section.Screw slenderness ratio is 44:1.
Embodiment 2
The preparation method is as follows:
S1, after ratio weighs raw material by weight, first by 55 parts of polyether polyurethane elastomer 70~90 DEG C baking oven into
Row drying pretreatment；
S2,0.5 part of 15 parts of POP, 5 parts of compatilizer, 24 parts of hypo-aluminum orthophosphate, antioxidant investment high mixer are uniformly mixed；
S3, dried polyether polyurethane elastomer is added, pours into 25 0.5 parts of the initiator pair dissolved with butanone,
It is again turned on high mixer to be uniformly mixed, 55 DEG C of mixing temperature；
The halogen-free flameproof polyether-type that S4, the material mixed obtain high-temp resisting high-humidity resisting improvement through double-screw extruding pelletizing is poly-
Urethane elastomer.Wherein, each area's temperature setting of screw rod are as follows: 150 DEG C of an area, two 160 DEG C of areas, three 170 DEG C of areas, four 170 DEG C of areas, five
180 DEG C of area, six 180 DEG C of areas, seven 180 DEG C of areas, eight 180 DEG C of areas, nine 175 DEG C of areas, ten 175 DEG C of areas, 170 DEG C of head.Screw speed
150rpm.Wherein, an area~2nd area are material conveying section, and 3rd area~5th area are melting cut section, and 6th area~9th area are that compression is mixed
Section is refined, tenth area~11st area are homogenizing metering section.Screw slenderness ratio is 44:1.
Embodiment 3
The preparation method is as follows:
S1, after ratio weighs raw material by weight, first by 45 parts of polyether polyurethane elastomer 70~90 DEG C baking oven into
Row drying pretreatment；
S2,20 parts of POP, 10 parts of compatilizer, 23.5 parts of hypo-aluminum orthophosphate, 0.5 part of antioxidant are thrown in high mixer mixing
It is even, 60 DEG C of mixing temperature；
S3, dried polyether polyurethane elastomer is added, pours into 1 part of crosslinking agent phenolic resin dissolved with butanone,
High mixer is again turned on to be uniformly mixed；
The halogen-free flameproof polyether-type that S4, the material mixed obtain high-temp resisting high-humidity resisting improvement through double-screw extruding pelletizing is poly-
Urethane elastomer.Each area's temperature setting of screw rod are as follows: 150 DEG C of an area, two 160 DEG C of areas, three 180 DEG C of areas, four 180 DEG C of areas, five areas 190
DEG C, six 190 DEG C of areas, seven 190 DEG C of areas, eight 190 DEG C of areas, nine 180 DEG C of areas, ten 180 DEG C of areas, 11 180 DEG C of areas, 190 DEG C of head.Spiral shell
Bar revolving speed 200rpm (rev/min).Wherein, an area~2nd area are material conveying section, and 3rd area~6th area are to melt cut section, seven
Area~tenth area are compression mixing section, and Shi Yiqu~No.12 District is homogenizing metering section.Screw slenderness ratio is 48:1.
In the above embodiments, polyether polyurethane elastomer is model BASF 1180A, shore hardness 80A；
POP uses Tao Shi 475HM；Compatilizer is maleic anhydride grafted elastomeric, wherein the elastomer being grafted is POP (model
475HM) it is kneaded and is prepared according to mass ratio 1:2 proportion with EVM (model 500HV).
Wherein, initiator is double 25 or phenolic resin.
Wherein, antioxidant is the compound of the phosphite antioxidant of amine antioxidants and molecular weight greater than 600, front and back two
The compounding weight ratio 2:3 of person.The amine antioxidants are 4,4'- bis- (propyloxy phenyl base) diphenylamines, specially U.S. Kang Pu
The product 445 of company；High molecular weight phosphite antioxidant is bis- (2,4-dicumylphenyl) pentaerythrite diphosphorous acids
Ester, specially the new patent product S-9228 of U.S. Dover company.
In addition, present invention also provides following reference examples as control:
Comparative example 1
It is made of following composition of raw materials:
The preparation method is as follows:
S1, after weighing raw material in raw material weight ratio, the first baking by 53 parts of polyether polyurethane elastomer at 70~90 DEG C
Case carries out drying pretreatment；
S2, by 54 parts of POP, 24 parts of phosphor nitrogen combustion inhibitor, 0.5 part of antioxidant, anti-hydrolysis agent (aggretion type carbodiimides)
It throws for 1.5 parts and is uniformly mixed in high mixer；
S3, dried polyether polyurethane elastomer is added, is again turned on high mixer and is uniformly mixed；
S4, the material mixed obtain halogen-free flameproof polyether polyurethane elastomer through double-screw extruding pelletizing.Screw rod
Each area's temperature setting are as follows: 150 DEG C of an area, two 160 DEG C of areas, three 180 DEG C of areas, four 180 DEG C of areas, five 190 DEG C of areas, six 190 DEG C of areas, seven
190 DEG C of area, eight 190 DEG C of areas, nine 180 DEG C of areas, ten 180 DEG C of areas, 11 180 DEG C of areas, 190 DEG C of head.Screw speed 200rpm.Its
In, an area~2nd area are material conveying section, and 3rd area~6th area are melting cut section, and 7th area~tenth area are to compress mixing section, 11
Area~No.12 District is homogenizing metering section.Screw slenderness ratio is 48:1.
Comparative example 2
It is made of following composition of raw materials:
Preparation method is identical as comparative example 1, and details are not described herein.
Granulated particles are made in the above process to be injection moulded through injection molding machine, injection temperature is 180 DEG C, 50 DEG C of mould temperature, cooling
After be cut into dumbbell plate and carry out tensile strength and fire-retardant equal test.
The performance test results are as shown in table 1:
Table 1
As can be seen from the above table, high-temp resisting high-humidity resisting of the present invention improves its heat-proof water of halogen-free flame resistance polyurethane elastomer and resistance to
High temperature and humidity performance improvement is obvious, and performance change is little under double 85,1000 hours test conditions, and tensile strength and fracture are stretched
The retention rate of long rate is greater than 70%, while the comprehensive performance of product is also improved, and uses addition anti-hydrolysis agent and irradiation
The effect of the application is not achieved in the method for crosslinking.
On the basis of the above, the application also further provides several feasible embodiments, as shown in table 2, these realities
The preparation method for applying example is identical as Examples 1 to 3, and details are not described herein:
Table 2 is the composition of raw materials (unit: mass parts) of embodiment 4~6
Table 2
Polyether polyurethane elastomer, compatilizer, phosphor nitrogen combustion inhibitor, antioxidant and the embodiment 1 that embodiment 4~6 uses
~3 is identical；The crosslinking agent of embodiment 4 and embodiment 5 is dual-tert-butyl dicumyl peroxide；The crosslinking agent of embodiment 6 is
Phenolic resin.
In the application, polyether polyol is that main chain contains ehter bond (- R-O-R -), and end group or side group contain greater than 2
The oligomer of hydroxyl (- OH).In the application, polyethers generally uses propylene glycol polyethers, molecular weight of the molecular weight for 800~2000
For 400~4000 trimethylolpropane polyethers or the polytetrahydrofuran of terminal hydroxy group.In addition, preparing used in adhesive for polyurethane
Polyethers requirement is more stringent, in addition to hydroxyl value, acid value, it is desirable that should be less than 10 containing potassium, sodium ion amount, water content is no less than 0.05%
It is then possible to generate gel.
The application can be by the reason of test in double 85,1000 hours: in the application, polyether polyurethane elastomer tool
Have good water resistance, impact resistance and low temperature properties, secondly, in POP octene be easy to generate active function groups be crosslinked agent initiation
Chemical crosslinking, and hardness, fusing point are low, crystallinity is low, it is suitable for the macromolecule resin as grafting that yield strength is high, and because its
, by the way that the two to be blended to and is added crosslinking agent, POP can be made to graft on poly- so hydrolysis ability is fine for non-polar resin
Ether-based polyurethane elastomer and further occurrence chemical crosslinking, thus make the application finally finished product obtained have it is good water-fast
Xie Xing, temperature tolerance.
In addition, fire retardant uses hypo-aluminum orthophosphate in the application, hypo-aluminum orthophosphate has long-term water resistance, can be further
Improve the water resistance of the application.
Although the present invention only gives above embodiments to illustrate performance of the invention, those skilled in the art exist
It under the inspiration of this above embodiments, is easy to show that some variations of the invention may be implemented, for example, feed components can be
Change in the range of present invention provide that, the content of each component can present invention provide that variation range in change.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
1. a kind of halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting, which is characterized in that by mass fraction include with
Lower component:
2. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as described in claim 1, which is characterized in that described
Polyether polyurethane elastomer is copolymerized by polyether polyol and methyl diphenylene diisocyanate.
3. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as claimed in claim 2, which is characterized in that described
Polyether polyol is Polyoxypropylene diol or polytetrahydrofuran ether dihydric alcohol.
4. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as described in claim 1, which is characterized in that described
Crosslinking agent is peroxide cross-linking agent；The compatilizer is maleic anhydride grafted elastomeric.
5. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as claimed in claim 4, which is characterized in that described
Elastomer in maleic anhydride grafted elastomeric is blended to obtain by POP with EVM press matter using rubbe amount ratio 1:1~1:3；The crosslinking agent
For 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane, dual-tert-butyl dicumyl peroxide or phenolic resin.
6. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as described in claim 1, which is characterized in that described
Phosphor nitrogen combustion inhibitor is hypo-aluminum orthophosphate.
7. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as described in claim 1, which is characterized in that also wrap
The antioxidant of 0.3~0.8 mass parts is included, the antioxidant includes that the phosphite ester of amine antioxidants and molecular weight greater than 600 is anti-
The weight ratio of oxygen agent, the amine antioxidants and the phosphite antioxidant is 2:5~1:1.
8. the halogen-free flameproof polyether polyurethane elastomer of high-temp resisting high-humidity resisting as claimed in claim 7, which is characterized in that described
Amine antioxidants are 4,4'- bis- (propyloxy phenyl base) diphenylamines；The phosphite antioxidant is bis- (2,4-dicumylphenyls)
Pentaerythritol diphosphites.
9. a kind of halogen-free flameproof polyether polyurethane elastomer of such as high-temp resisting high-humidity resisting according to any one of claims 1 to 8
Preparation method, comprising the following steps:
S1, the polyether polyurethane elastomer is dried 2~4 hours under the conditions of 70~90 DEG C；
S2, by the polyolefin plastomers and the phosphor nitrogen combustion inhibitor and by the step S1 drying after the polyether-type
Polyurethane elastomer, the compatilizer are uniformly mixed under conditions of 50~200rpm, 50~60 DEG C；
S3, crosslinking agent is added after mixing velocity is reduced to 30~50rpm, continuess to mix uniform mixed material；
S4, the mixed material is granulated to obtain the poly- ammonia of halogen-free flameproof polyether-type of the high-temp resisting high-humidity resisting through double screw extruder
Ester elastomer.
10. a kind of preparation method as claimed in claim 9, which is characterized in that in the step S1, drying time is 2~5 small
When；
Incorporation time is 2~5 minutes in the step S2；
Incorporation time is 1~2 minute in the step S3；
In the step S4, the conveying section temperature of the double screw extruder is 120 DEG C~160 DEG C, and melting cut section temperature is
160 DEG C~180 DEG C, compression mixing section temperature is 160 DEG C~200 DEG C, and metering homogenizing zone temperature is 170 DEG C~190 DEG C, and screw rod is long
Diameter ratio is 40~48:1,100~200rpm of screw speed.
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| CN110487667B (en) * | 2019-09-19 | 2024-05-10 | 北京高能时代环境技术股份有限公司 | Material moisture content detector |
| CN110685036A (en) * | 2019-10-12 | 2020-01-14 | 江苏馨德高分子材料股份有限公司 | Production method of flame-retardant and oil-stain-resistant TPE (thermoplastic elastomer) yarn |
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