CN105885186A - Polyvinylidene difluoride-based thermoplastic vulcanized rubber and preparation method thereof - Google Patents
Polyvinylidene difluoride-based thermoplastic vulcanized rubber and preparation method thereof Download PDFInfo
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- CN105885186A CN105885186A CN201610262025.8A CN201610262025A CN105885186A CN 105885186 A CN105885186 A CN 105885186A CN 201610262025 A CN201610262025 A CN 201610262025A CN 105885186 A CN105885186 A CN 105885186A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0869—Acids or derivatives thereof
- C08L23/0884—Epoxide containing esters
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Abstract
The invention discloses polyvinylidene difluoride-based thermoplastic vulcanized rubber and a preparation method thereof. The polyvinylidene difluoride-based thermoplastic vulcanized rubber is composed of, by weight parts, 70-90 parts of ethylene-butyl acrylate-glycidyl methacrylate copolymer rubber, 10-30 parts of polyvinylidene fluoride, 0.5-2 parts of amine curing agent, 0.1-5 parts of free radical stabilizer, 0.05-1 part of antioxidant 0.1-3 parts of anti-aging agent and 1-20 parts of plasticizer. The thermoplastic vulcanized rubber obtained according to the preparation method has the advantages of being high in strength, large in elongation, good in resilience and excellent in thermoplasticity and the like. The preparation method is simple, and industrialization is achieved easily.
Description
Technical field
The present invention relates to technical field of polymer materials, particularly relate to a kind of based on polyvinylidene fluoride
TPV of alkene and preparation method thereof.
Background technology
Current traditional rubber is prepared by vulcanizing, formed product processing difficulties, and is unfavorable for back
Receiving, reuse, environmental pollution is serious.The progress of dynamic vulcanization method maximum is that employing is low
The existing processing method of cost, the most existing polymer is blended and prepares TPE, have
The advantage of low cost, greatly extends the kind of TPE.Compared with copoly type TPE, TPV
There is the upper limit and use temperature height, the advantage of the little and resistance to hydrocarbon medium of Compression Set.TPV exists
Show the character of rubber under room temperature, at high temperature can as plastics melt-processed, permissible
Fast, economical and easily machine-shaping, and can recycle after using, have become as one
Plant very important novel high polymer material.
TPV (TPV) is mainly made up of two parts, and one is plastics, as even
Continuous phase, two is that the rubber of crosslinking is as dispersion phase.The rubber that TPV selects at present mainly has sky
So rubber, butadiene-styrene rubber, butadiene rubber, nitrile rubber, acrylate rubber, ethylene/vinegar
Acid ethylene rubber, ethylene propylene diene rubber, neoprene or their blend, the plastics of selection
Mainly include polypropylene, polyethylene, polyamide, SAN, polyphenyl second
Alkene, Merlon or their mixture.Current most typical TPV is ethylene propylene diene rubber
(EPDM) prepare through dynamic vulcanization with polypropylene (PP), be a large amount of solid cures
EPDM microgranule is dispersed in continuous print PP phase the macromolecular elastomer material formed.Generally
EPDM content in TPV is 60-70wt%.Dynamic vulcanization makes to disperse in PP plastic substrate
EPDM particle diameter less than 2 μm, and make rubber well combine with the characteristic of plastics,
Obtain the elastomeric material of excellent combination property.But traditional EPDM/PP thermoplastic elastomer (TPE)
Hot strength is the highest, drawing of such as EPDM/PP (60/40, wt/wt) TPV
Stretch intensity and be even below 10MPa.
It is obvious that in order to meet various demand, more and more different types of TPV are developed.
Existing fluorubber product mostly is block copolymer, complicated process of preparation, and price is higher, melt
Viscosity is big, is unfavorable for processing, is mainly used in some the most high-end fields.Blending type is poly-partially
Fluorothene thermoplastic elastic can be prepared by methods such as melt blending, increase-volume, dynamic vulcanizations.
Elastomer with Kynoar as continuous phase, rubber as dispersion phase, both inherited Kynoar
Thermoplasticity and other excellent properties, again due in elastomer crosslinked rubber particles contribution and
There is preferable elastic recovery.The research and development of this kind of elastomer, to Kynoar
The relatively low of the variation of elastomer kind, technology difficulty and cost has important far-reaching significance.
Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer (PTW) rubber is a kind of
Polarity specific rubber, compares traditional several big class rubber and has a lot of advantages, currently for
The composite study on the modification of PTW rubber is the most fewer, and the research of this respect is for extension
The application of PTW rubber is particularly important.By processability good for PTW, adhesiveness,
Heat-resisting quantity combines with PVDF Good All-around Property, for new type high temperature oil-resisting type
The exploitation of PVDF thermoplastic elastomer (TPE) has important directive significance.
Summary of the invention
In view of this, it is an object of the invention to propose a kind of thermoplasticity based on Kynoar
The preparation method of vulcanite, to obtain, intensity is high, percentage elongation is big, high resilience, oil resistivity
By force, thermoplastic property excellent, use temperature range TPV widely.
Based on above-mentioned purpose, a kind of based on Kynoar the thermoplastic vulcanizates that the present invention provides
Rubber is made up of according to respective weight following raw material: PTW 70～90 parts, polyvinylidene fluoride
Alkene 10～30 parts, amine curing agents 0.5～2 parts, free radical stabilizer 0.1～5 parts, antioxidant
0.05～1 part, age resistor 0.1～3 parts, plasticizer 1～20 parts.
It is preferred that amine vulcanizer is chosen as N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxy
The amino silicones such as silane, it is ensured that reaction condition is more gentle and preparation based on poly-inclined fluorine
Ethylene thermoplastic's vulcanite has preferable processing characteristics and mechanical performance.
It is preferred that the reaction optimum temperature of described vulcanizing agent is 190 DEG C, it is ensured that sulfuration is anti-
Answering temperature, the TPV thermoplasticity of preparation is strong, and excellent combination property.
Alternatively, described free radical stabilizer is 2,2,6,6-tetramethyl piperidines-nitrogen-oxide, from
Free radical can be caught when peroxide fast decoupled, it is to avoid locally by the existence of based stabilizer
Excessively crosslinking and cause the decline of TPV mechanical performance, and be captured at the same temperature from
Can be slowly released again by base, thus reach cure efficiency more preferably, evenly.
Alternatively, described antioxidant is at least one in irgasfos 168 and antioxidant 1010,
Can stop or reduce Ethylene-butyl acrylate-methacrylic acid during dynamic vulcanization
Glycidyl ester copolymer rubber and the thermal degradation of Kynoar.
Alternatively, described age resistor is 2,2,4-trimethyl-1,2-dihydroquinoline polymer, N-ring
In hexyl-N'-diphenyl-para-phenylene diamine and N-(1,3-dimethyl) butyl-N'-diphenyl-para-phenylene diamine extremely
Few one.
Alternatively, described plasticizer is ester plasticizer, including dioctyl adipate, citric acid
At least one in ester, dibutyl sebacate, di-n-octyl sebacate and trioctyl trimellitate (TOTM).
Ester plasticizer and Kynoar and Ethylene-butyl acrylate-methyl propenoic acid glycidyl
Acrylate copolymer rubber has the good compatibility, therefore, it is possible to prepared by improving to a greater extent
The elasticity of thermoplastic sulfurized rubber, regulate its hardness, its cost can also be reduced simultaneously.
Present invention also offers a kind of described TPV based on Kynoar
Preparation method, comprises the following steps:
First by Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber, gather
Vinylidene, free radical stabilizer and age resistor according to weight at 180 DEG C～190 DEG C
Elastomeric compound is obtained by two-roll mill or banbury or screw extruder mix homogeneously, mixed
Sweetening process is identical with tradition rubber mixing-milling technique；Then by above-mentioned elastomeric compound, amine curing agents,
Antioxidant and plasticizer according to weight at 180 DEG C～190 DEG C by banbury or
Screw extruder melt blending 5～10min, finally give a kind of with Kynoar as matrix,
Cross-linked ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer rubber is dispersion phase
TPV.
Alternatively, described closed-smelting machine rotor rotating speed 50～200 revs/min, preferably 80～100 turns/
Minute.
Alternatively, described screw extruder rotating speed 80-300 rev/min, preferably 100～200 turns/
Minute.
From the above it can be seen that the one that the present invention provides is based on polyvinylidene fluoride alkylene rubber
Preparation method can realize on conventional polymer material processing plant, low cost, easily real
Existing industrialized production.The TPV that the preparation method provided according to the present invention is obtained
There is the features such as resilience is good, intensity is high, thermoplastic property is excellent, can be directly used for extrusion molding,
Compression molding is to prepare various thermoplastic elastomer article.Additionally, the additive of trace, such as
Coloring agent, processing aid etc. do not interfere with the key property of this TPV.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with tool
Body embodiment, the present invention is described in more detail.
Embodiment 1
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g, gather
Vinylidene 150g, 2,2,6,6-tetramethyl piperidine-nitrogen-oxide 2.5g, 2,2,4-trimethyl-1,2-
Dihydroquinoline polymer 2.5g banbury mixing 10min obtain elastomeric compound (blending condition:
Temperature is 190 DEG C, and rotor speed is 80 revs/min), then by elastomeric compound and amine curing agents
2.5g, dibutyl sebacate 15g, 1010 antioxidant 2.5g and 168 antioxidant 0.5g are close
In refining machine, melt blending 10min obtains TPV (blending condition: temperature is
190 DEG C, rotor speed is 80 revs/min).By TPV by vulcanizing press heat
Molded, obtain the thick flaked thermoplastic's vulcanite of 1mm, and be cut into according to relevant criterion
Standard batten is used for Mechanics Performance Testing, and every test result is listed in table 1.
Embodiment 2
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g, gather
Vinylidene 150g, 2,2,6,6-tetramethyl piperidine-nitrogen-oxide 2.5g, 2,2,4-trimethyl-1,2-
Dihydroquinoline polymer 2.5g banbury mixing 10min obtain elastomeric compound (blending condition:
Temperature is 190 DEG C, and rotor speed is 80 revs/min), then by elastomeric compound and amine curing agents
5g, dibutyl sebacate 15g, 1010 antioxidant 2.5g and 168 antioxidant 0.5g are in banburying
In machine melt blending 10min obtain TPV (blending condition: temperature is 190 DEG C,
Rotor speed is 80 revs/min).TPV is hot-forming by vulcanizing press,
Obtain the thick flaked thermoplastic's vulcanite of 1mm, and be cut into standard batten according to relevant criterion
For Mechanics Performance Testing, every test result is listed in table 1.
Embodiment 3
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g, gather
Vinylidene 150g, 2,2,6,6-tetramethyl piperidine-nitrogen-oxide 2.5g, 2,2,4-trimethyl-1,2-
Dihydroquinoline polymer 2.5g banbury mixing 10min obtain elastomeric compound (blending condition:
Temperature is 190 DEG C, and rotor speed is 80 revs/min), then by elastomeric compound and amine curing agents
7.5g, dibutyl sebacate 15g, 1010 antioxidant 2.5g and 168 antioxidant 0.5g are close
In refining machine, melt blending 10min obtains TPV (blending condition: temperature is
190 DEG C, rotor speed is 80 revs/min).By TPV by vulcanizing press heat
Molded, obtain the thick flaked thermoplastic's vulcanite of 1mm, and be cut into according to relevant criterion
Standard batten is used for Mechanics Performance Testing, and every test result is listed in table 1.
Embodiment 4
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g, gather
Vinylidene 150g, 2,2,6,6-tetramethyl piperidine-nitrogen-oxide 2.5g, 2,2,4-trimethyl-1,2-
Dihydroquinoline polymer 2.5g banbury mixing 10min obtain elastomeric compound (blending condition:
Temperature is 190 DEG C, and rotor speed is 80 revs/min), then by elastomeric compound and amine curing agents
10g, dibutyl sebacate 15g, 1010 antioxidant 2.5g and 168 antioxidant 0.5g are in banburying
In machine melt blending 10min obtain TPV (blending condition: temperature is 190 DEG C,
Rotor speed is 80 revs/min).TPV is hot-forming by vulcanizing press,
Obtain the thick flaked thermoplastic's vulcanite of 1mm, and be cut into standard batten according to relevant criterion
For Mechanics Performance Testing, every test result is listed in table 1.
Embodiment 5
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g, gather
Vinylidene 150g, 2,2,6,6-tetramethyl piperidine-nitrogen-oxide 2.5g, 2,2,4-trimethyl-1,2-
Dihydroquinoline polymer 2.5g banbury mixing 10min obtain elastomeric compound (blending condition:
Temperature is 180 DEG C, and rotor speed is 80 revs/min), then by elastomeric compound and amine curing agents
5g, dibutyl sebacate 15g, 1010 antioxidant 2.5g and 168 antioxidant 0.5g are in banburying
In machine melt blending 10min obtain TPV (blending condition: temperature is 180 DEG C,
Rotor speed is 80 revs/min).TPV is hot-forming by vulcanizing press,
Obtain the thick flaked thermoplastic's vulcanite of 1mm, and be cut into standard batten according to relevant criterion
For Mechanics Performance Testing, every test result is listed in table 1.
Embodiment 6
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g, gather
Vinylidene 150g, 2,2,6,6-tetramethyl piperidine-nitrogen-oxide 10g, 2,2,4-trimethyl-1,2-
Dihydroquinoline polymer 2.5g banbury mixing 10min obtain elastomeric compound (blending condition:
Temperature is 190 DEG C, and rotor speed is 50 revs/min), then by elastomeric compound and amine curing agents
5g, dibutyl sebacate 15g, 1010 antioxidant 2.5g and 168 antioxidant 0.5g are in banburying
In machine melt blending 10min obtain TPV (blending condition: temperature is 190 DEG C,
Rotor speed is 50 revs/min).TPV is hot-forming by vulcanizing press,
Obtain the thick flaked thermoplastic's vulcanite of 1mm, and be cut into standard batten according to relevant criterion
For Mechanics Performance Testing, every test result is listed in table 1.
Comparative example 1
By Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 450g with
Kynoar 150g melt blending 10min in banbury obtain blend (blending condition:
Temperature is 180 DEG C, and rotor speed is 50 revs/min).By blend by vulcanizing press hot pressing
Molding, obtains the thick flaked thermoplastic's vulcanite of 1mm, and is cut into mark according to relevant criterion
Quasi-batten is used for Mechanics Performance Testing, and every test result is listed in table 1.
Comparative example 2
By ethylene-propylene rubber (EPDM) 300g, cumyl peroxide 3g, 2,2,6,6-
Tetramethyl piperidine-nitrogen-oxide 2.5g, 2,2,4 trimethyl 1,2 dihydroquinoline polymer 2.5g
Elastomeric compound (blending condition: temperature is 80 DEG C, and rotor turns is obtained with banbury mixing 10min
Speed is 50 revs/min), then by elastomeric compound and polypropylene 200g, dibutyl sebacate 15g,
1010 antioxidant 2.5g and 168 antioxidant 0.5g melt blending 10min in banbury obtain
TPV (blending condition: temperature is 170 DEG C, rotor speed is 50 revs/min).
TPV is hot-forming by vulcanizing press, obtain lamellar heat thick for 1mm
Plasticity vulcanite, and it is cut into standard batten for Mechanics Performance Testing according to relevant criterion, respectively
Item test result is listed in table 1.
It should be noted that Kynoar used in various embodiments above and comparative example, poly-third
Alkene, Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber and EPDM make
At 50 DEG C, 12h all it is vacuum dried with front.Kynoar used is that rich green wood is liked in Shanghai three
Material limited company product, polypropylene used is Sinopec product, ethylene-acrylic acid
Butyl ester-glycidyl methacrylate copolymer rubber is du pont company's product, used
EPDM is Dow Chemical Products.Other chemical assistants are commercially available prod, and purity is
More than 97%.
The step of prepared thermoplastic elastic material based on Kynoar compacting sheet material
Including: first prepared thermoplastic elastic material based on Kynoar is put into mould
Hot pressing on vulcanizing press (hot pressing temperature 200 DEG C, hot pressing time 8min, hot pressing pressure
10MPa) colding pressing (cold pressing time 5min, and cold pressing pressure 5MPa), making thickness is 1mm again
Sheet material, for tensile property and hardness test.
Wherein use electronic tensile test machine (Instron5967) at room temperature by national standard
The tensile property of GB/T 528-2009 test sample, draw speed is 200mm/min；Use
Shore D type hardness tester meter is according to the hardness of standard GB/T/T 531.1-2008 test sample.
Table 1 embodiment and thermoplastic elastomer (TPE) material based on Kynoar in comparative example
The performance parameter of material
The TPV based on Kynoar obtained by the present invention and biography at present
System TPV is compared has the advantages such as intensity is high, resilience is good, it is possible to meets and is subtracting
Blanket, car internal and external ornament product, medical equipment, the application of the aspect such as sport shoes.With comparative example
The thermoplastic vulcanizates rubber that the EPDM rubber of commercialization is prepared is used with polypropylene dynamic vulcanization in 2
Glue is compared, TPV based on the Kynoar stretching obtained in embodiment 1～6
Intensity increases, and 100% stretching strength is also improved, and elongation at break is higher simultaneously.
With comparative example 1 is provided without Ethylene-butyl acrylate-methacrylic acid contracting prepared by dynamic vulcanization
Water glyceride copolymer rubber/polyvinylidene blending is compared, the base obtained in embodiment 1～6
TPV hot strength in Kynoar improves 2～7 times, and 100% stretches by force surely
Degree improves 1～4 times, and hardness significantly improves simultaneously.Therefore, present invention is to conventional thermal
The breakthrough on composition of raw materials and performance of the plasticity vulcanite.The present invention provide based on poly-
The thermoplastic elastic material viscosity of vinylidene is relatively low, can be directly used for extrusion molding or heat
Molded, to prepare various thermoplastic elastomer article.Additionally, trace or a small amount of additive,
Such as processing aid, coloring agent, hydrolysis-resisting agent etc. will not thermoplastic elastic materials described in shadow
Key property.
Those of ordinary skill in the field are it is understood that the foregoing is only being embodied as of the present invention
Example, is not limited to the present invention, all within the spirit and principles in the present invention, done
Any modification, equivalent substitution and improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a TPV based on Kynoar, it is characterized in that, it is made up of according to respective weight following raw material: Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber 60～90 parts, Kynoar 10～40 parts, amine curing agents 0.5～2 parts, free radical stabilizer 0.1～5 parts, antioxidant 0.05～1 part, age resistor 0.1～3 parts, plasticizer 1～20 parts.
A kind of TPV based on Kynoar the most according to claim 1, it is characterised in that curing temperature controls at 190 DEG C.
One the most according to claim 1 is based on Kynoar TPV, it is characterised in that described free radical stabilizer is 2,2,6,6-tetramethyl piperidines-nitrogen-oxide.
A kind of TPV based on Kynoar the most according to claim 1, it is characterised in that described antioxidant is at least one in irgasfos 168 and antioxidant 1010.
A kind of TPV based on Kynoar the most according to claim 1, it is characterized in that, described age resistor is 2,2,4-trimethyl-1, at least one in 2-dihydroquinoline polymer, N cyclohexyl N' phenyl P phenylene diamine and N-(1,3-dimethyl) butyl-N'-diphenyl-para-phenylene diamine.
A kind of TPV based on Kynoar the most according to claim 1, it is characterised in that described plasticizer is at least one in dioctyl adipate, citrate, dibutyl sebacate, di-n-octyl sebacate and trioctyl trimellitate (TOTM).
7. the preparation method of a TPV based on Kynoar, it is characterised in that said method comprising the steps of:
First by two-roll mill or banbury or screw extruder mix homogeneously, Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer rubber, Kynoar, free radical stabilizer and age resistor being obtained elastomeric compound according to weight at 180 DEG C～190 DEG C, calendering process is identical with tradition rubber mixing-milling technique；Then by above-mentioned elastomeric compound, amine curing agents, antioxidant and plasticizer according to weight at 180 DEG C～190 DEG C by banbury or screw extruder melt blending 5～10min, finally give a kind of with Kynoar as matrix, cross-linked ethylene-propylene acid butyl ester-glycidyl methacrylate copolymer rubber TPV as dispersion phase.
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| CN201610262025.8A CN105885186A (en) | 2016-04-25 | 2016-04-25 | Polyvinylidene difluoride-based thermoplastic vulcanized rubber and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107227025A (en) * | 2017-06-30 | 2017-10-03 | 上海至正道化高分子材料股份有限公司 | A kind of special high temperature resistant radiation hardness Insulation Material of nuclear power station and preparation method thereof |
| US20190203026A1 (en) * | 2016-09-07 | 2019-07-04 | Solvay Specialty Polymers Italy S.P.A. | Fluorine-containing thermoplastic elastomer composition |
| CN114656742A (en) * | 2022-04-18 | 2022-06-24 | 西北工业大学 | Preparation method of alloy type creep-resistant fluorine-containing thermoplastic elastomer |
-
2016
- 2016-04-25 CN CN201610262025.8A patent/CN105885186A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190203026A1 (en) * | 2016-09-07 | 2019-07-04 | Solvay Specialty Polymers Italy S.P.A. | Fluorine-containing thermoplastic elastomer composition |
| CN107227025A (en) * | 2017-06-30 | 2017-10-03 | 上海至正道化高分子材料股份有限公司 | A kind of special high temperature resistant radiation hardness Insulation Material of nuclear power station and preparation method thereof |
| CN114656742A (en) * | 2022-04-18 | 2022-06-24 | 西北工业大学 | Preparation method of alloy type creep-resistant fluorine-containing thermoplastic elastomer |
| CN114656742B (en) * | 2022-04-18 | 2024-05-03 | 西北工业大学 | Preparation method of alloy type creep-resistant fluorine-containing thermoplastic elastomer |
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