CN110054815A - A kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer and preparation method thereof - Google Patents
A kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer and preparation method thereof Download PDFInfo
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- CN110054815A CN110054815A CN201810047779.0A CN201810047779A CN110054815A CN 110054815 A CN110054815 A CN 110054815A CN 201810047779 A CN201810047779 A CN 201810047779A CN 110054815 A CN110054815 A CN 110054815A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The present invention provides a kind of nitrile rubber/nylon thermoplastic's elastomers and preparation method thereof of dynamic vulcanization preparation.According to mass fraction meter, composition: 100 parts of nitrile rubber, 6,30 ~ 90 parts of nylon, 0.1 ~ 5 part of vulcanizing agent, 0.1 ~ 5 part of vulcanization aid, 0.01 ~ 3 part of stabilizer, 0.1 ~ 5 part of anti-aging agent, 0.1 ~ 5 part of antioxidant.The present invention is first uniformly mixed nitrile rubber in room temperature mixer with crosslinking agent, cross-linking aid, stabilizer and anti-aging agent and carries out rubber granulation, it is stirred evenly in high-speed mixer with nylon particle and other components again later, the rubber and nylon mixture that mix finally is put into progress dynamic vulcanization in double screw extruder and prepare nitrile rubber/nylon thermoplastic's elastomer.Nitrile rubber of the invention/nylon thermoplastic's elastomer cost performance is high, saves hot Banbury mixing step, and low energy consumption for simple production process, can be carried out continuously the preparation of double screw extruder dynamic vulcanization.
Description
Technical field
The present invention relates to a kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomers and preparation method thereof, belong to high score
Sub- field of material processing.
Background technique
Dynamic vulcanization thermoplastic elastomer (TPV) is the height for being prepared existing plastics and blend rubber by dynamic vulcanization technology
Performance thermoplastic elastomer (TPE), have both elasticity and thermoplasticity, can reprocessabilty use and recycle, the feature of environmental protection is significant with economy.
Currently, high temperature resistant oil resistance is the focus on research direction of TPV, most representative in this kind of TPV is polyester
Analog thermoplastic elastomer and polyamide-type thermoplastic elastomer, exploitation and market development speed are more than Polyolefin Plastics dynamic sulphur
Change elastomer.The exploitation of external high-performance TPV focuses primarily upon the U.S., European Union and Japan, with specific rubber hydrogenated nitrile-butadiene rubber
(HNBR), acrylic rubber (ACM), ethylene-acrylate rubber (AEM), silicon rubber (MVQ), fluorubber (FKM) etc. are dispersed phase,
Using engineering plastics such as nylon (PA), polyurethane, polyester or fluororesin as continuous phase.The high-performance TPV such as ACM/PA being commercialized at present,
There is the contradiction in performance and cost in AEM/PA, MVQ/PA, EVM/PA etc., price is overall expensive, and some TPV such as MVQ/PA,
The oil resistance of EVM/PA also needs to improve, therefore high heat resistance oil resistant automotive rubber products are not substituted by TPV also extensively.Domestic high-performance
Heat-resisting oil resistant TPV does not have commercialization also.General automobile vulcanizate extrudate density about 1.3g/cm3 is even higher, the density of TPV
Between 1.05 ~ 1.15 g/cm3, isometric substitution can loss of weight 10% ~ 15%, reduction product weight and the environmental requirement for meeting material.
NBR has excellent oil resistivity, and PA has excellent heat-resisting, oil resistivity and barrier property, the equal band of both materials
Polarized group has preferable compatibility, and the NBR/PA TPV that is prepared by both Material claddings becomes to be studied both at home and abroad
One important goal.
The vulcanizing system of NBR is mainly with sulphur system, efficient vulcanization system and peroxide vulcanizing system.Above-mentioned three big sulphur
Change system is mainly used for the vulcanization under lower temperature, for example, 180 DEG C once.When more than 200 DEG C, sulfur cross-linking system and effectively
Vulcanizing system faces the decline of heat resistance, peroxide vulcanizing system although thermal-oxidative aging property with higher, but by
In the crosslinking feature of peroxide, crosslinking rate at high temperature is very fast, this prepares heat to rubber especially dynamic vulcanization
It is unacceptable for thermoplastic elastic.At present for dynamic vulcanization prepares NBR/ nylon thermoplastic elastomer, mainly there is three
Kind technical solution: first is that with NBR and low melting point nylon such as nylon 12 or terpolyamide, the thermoplasticity of this technical solution preparation
Elastomer has deficiency in terms of oil resistant heatproof, and price is more expensive；Second is that being moved with hydrogenated nitrile-butadiene rubber and nylon 12 or nylon 6
State vulcanization, the major drawbacks of this elastomer are that cost performance is low, do not have and value is widely applied；Third is that with common NBR and nylon 6 into
The cost performance of Mobile state vulcanization, this scheme is high, but high to formula and equipment requirement, and Preparation equipment mainly uses high temperature mixing
Machine, rather than double screw extruder.Preparation process is that addition NBR and anti-aging agent mix after nylon 6 is melted first in hot Banbury
It closes, until NBR and nylon add vulcanizing agent dynamic vulcanization after mixing, the advantages of this method is that rubber can be mixed with resin
Close uniformly, and disadvantage is exactly the high requirements on the equipment, and energy consumption is high, and can not continuous production, the temperature field in preparation process can not be uniform
Control, final material performance is uneven and potential NBR degradation.The fusing point of nylon 6 and nylon66 fiber or its copolymer nylon is more than
210 DEG C, at such high temperatures, the curingprocess rate of rubber quickly, if without NBR is uniformly mixed with nylon in advance be added sulphur
Agent, rubber generation are sharply reacted, and leading to NBR, also sufficiently just crosslinking is not reunited for shearing dispersion, can not be uniformly dispersed into resin
Small particles, this is unacceptable to thermoplastic elastomer (TPE).Especially peroxide vulcanizing system even more needs first NBR and Buddhist nun
Dragon is pre-mixed in hot Banbury could uniformly be added vulcanizing agent.Therefore from the angle of material cost performance and continuous and stable production
Degree sets out, and it is still to solve the problems, such as at present that developing, which can be suitble to double screw extruder continuously to prepare NBR/ nylon thermoplastic's elastomer,.
Summary of the invention
1. the purpose of the present invention
Regarding the issue above, the present invention provides a kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer and its
Preparation method.The present invention selects the NBR of high acrylonitrile content, selects nylon 6 to have excellent high temperature resistant oil resistant characteristic, passes through two
The good compatibility of person, and to vulcanizing system it is meticulous preferably, allow to save hot Banbury carry out nitrile rubber with
The high temperature of nylon is pre-mixed this process, is directly thrown into dynamic vulcanization in double screw extruder, the thermoplastic elastomer (TPE) of preparation
Material cost performance is high, requires equipment and technique low.
2. technical solution
The object of the invention can be achieved through the following technical solutions:
100 parts by weight of nitrile rubber
20 ~ 90 parts by weight of nylon
0.1~5 parts by weight of vulcanizing agent
0.1~5 parts by weight of vulcanization aid
0.01~3 parts by weight of stabilizer
0.1~3 parts by weight of anti-aging agent
0.1~3 parts by weight of antioxidant
Wherein its Mooney viscosity 30 ~ 60 of the nitrile rubber, acrylonitrile content 25 ~ 45%, preferably acrylonitrile content 30 ~ 42%, institute
Stating nylon is nylon 6.
The vulcanizing agent is peroxide vulcanizing agent；Including the bis- butylperoxyisopropyl benzene of 1,3-, the bis- tertiary fourths of 1,4-
Base peroxy isopropyl base benzene, 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 2,5- dimethyl -2,5- di-t-butyl mistake
Oxygroup -3- hexin.
The vulcanization aid be TAIC, 0.1 ~ 5 part of dosage.
The stabilizer is hindered amines or phosphite-type stabilisers, 0.01 ~ 5 part of dosage, preferably 0.1 ~ 3 part.
The present invention provides a kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's method for producing elastomers, it is characterised in that
The following steps are included:
(1) rubber granulation: first nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxidant are mixed in room temperature mixer
It closes uniformly, rubber granulation is carried out in rubber comminutor；
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle in high-speed mixer, the rubber and Buddhist nun mixed
Imperial mixture is put into and carries out dynamic vulcanization in double screw extruder, and 190 ~ 230 DEG C of extruder temperature, 150 ~ 400rpm of screw speed.
3. beneficial effect
The present invention is preferred by nitrile rubber vulcanizing system, mentions 190 DEG C of sulfurizing times of peroxide cure NBR substantially
Height, before carrying out dynamic crosslinking in 200 DEG C ~ 240 DEG C of double screw extruder, give more time carry out nitrile rubber with
Shearing distribution and dispersion between nylon, avoid the reunion of nitrile rubber caused by the sharply crosslinking of NBR peroxide, accomplish to connect
Continuous dynamic vulcanization prepares thermoplastic elastomer (TPE).
Specific embodiment
Comparative example 1
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
The bis- butylperoxyisopropyl benzene 1.5 of 1,3-
TAIC 1
Anti-aging agent 445 1.5
Antioxidant 1,098 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 200rpm.
Tie rod is unsuccessful during dynamic vulcanization, can not tie rod pelletizing.
Comparative example 2
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
2,5- dimethyl -2,5- two (t-butylperoxy) hexane 1
TAIC 1
Anti-aging agent 445 1.5
Antioxidant 245 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 200rpm.
Tie rod is unsuccessful during dynamic vulcanization, can not tie rod pelletizing.
Comparative example 3
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
The bis- butylperoxyisopropyl benzene 1.5 of 1,3-
TAIC 1
Stabilizer 701 0.2
Anti-aging agent 445 1.5
Antioxidant 1,098 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 150rpm.
During dynamic vulcanization can continuous tie rod pelletizing, but tie rod appearance is rougher.
Implement 1
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
The bis- butylperoxyisopropyl benzene 1.5 of 1,3-
TAIC 1
Stabilizer 701 0.2
Anti-aging agent 445 1.5
Antioxidant 1,098 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 200rpm.
During dynamic vulcanization can continuous tie rod pelletizing, tie rod appearance is more smooth.
Embodiment 2
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
2,5- dimethyl -2,5- two (t-butylperoxy) hexane 1
TAIC 1
Stabilizer 701 0.2
Anti-aging agent 445 1.5
Antioxidant 245 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 200rpm.
During dynamic vulcanization can continuous tie rod pelletizing, tie rod appearance is more smooth.
Embodiment 3
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
The bis- butylperoxyisopropyl benzene 1 of 1,3-
TAIC 1
Stabilizer 701 0.2
Anti-aging agent 445 1.5
Antioxidant 1,098 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 200rpm.
During dynamic vulcanization can continuous tie rod pelletizing, tie rod appearance is more smooth.
Embodiment 4
Nitrile rubber nylon dynamic vulcanization formula composition is as follows, and each component is based on parts by weight.
Nitrile rubber 100
Nylon 6 66.7
The bis- butylperoxyisopropyl benzene 1.5 of 1,3-
TAIC 1
Stabilizer 701 0.5
Anti-aging agent 445 1.5
Antioxidant 1,098 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 220rpm.
During dynamic vulcanization can continuous tie rod pelletizing, tie rod appearance is more smooth.
Embodiment 5
The formula composition of rubber composition is shown in Table 1, and preparation process and comparative example 1 are identical.Each component is based on parts by weight in table 1.
Nitrile rubber 100
Nylon 6 66.7
2,5- dimethyl -2,5- di-t-butyl peroxy -3- hexin 1
TAIC 1
Stabilizer 701 0.2
Anti-aging agent 445 1.5
Antioxidant 245 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 200rpm.
During dynamic vulcanization can continuous tie rod pelletizing, tie rod appearance is more smooth.
Embodiment 6
The formula composition of rubber composition is shown in Table 1, and preparation process and comparative example 1 are identical.Each component is based on parts by weight in table 1.
Nitrile rubber 100
Nylon 6 66.7
2,5- dimethyl -2,5- di-t-butyl peroxy -3- hexin 1.5
TAIC 1
Stabilizer 701 0.5
Anti-aging agent 445 1.5
Antioxidant 245 1
Preparation process:
(1) rubber granulation: at room temperature, in room temperature mixer, nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxygen
Agent is uniformly mixed bottom sheet, carries out rubber granulation in rubber comminutor at room temperature.
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle and other antioxidant in high-speed mixer,
The rubber and nylon mixture mixed, which is put into, carries out dynamic vulcanization in double screw extruder, screw slenderness ratio 68, screw rod is straight
Diameter 40mm, 220 DEG C of extruder temperature, screw speed 220rpm.
During dynamic vulcanization can continuous tie rod pelletizing, tie rod appearance is more smooth.
The Technology of Dynamic Vulcanized and tie rod quality of comparative example and embodiment are listed in table 1.
1 comparative example of table and embodiment Technical expression and tie rod appearance
| Whether continuous tie rod pelletizing | Tie rod appearance | |
| Comparative example 1 | It is no | It swells coarse |
| Comparative example 2 | It is no | It swells coarse |
| Comparative example 3 | It is | It is coarse |
| Embodiment 1 | It is | It is more smooth |
| Embodiment 2 | It is | It is more smooth |
| Embodiment 3 | It is | It is more smooth |
| Embodiment 4 | It is | It is more smooth |
| Embodiment 5 | It is | It is more smooth |
| Embodiment 6 | It is | It is more smooth |
Claims (5)
1. a kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer, comprising following components is blended:
100 parts by weight of nitrile rubber
20 ~ 90 parts by weight of nylon
0.1~5 parts by weight of vulcanizing agent
0.1~5 parts by weight of vulcanization aid
0.01~3 parts by weight of stabilizer
0.1~3 parts by weight of anti-aging agent
0.1~3 parts by weight of antioxidant
Wherein its Mooney viscosity 30 ~ 60 of the nitrile rubber, acrylonitrile content 25 ~ 45%, preferably acrylonitrile content 30 ~ 42%, institute
Stating nylon is nylon 6.
2. a kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer according to claim 1, which is characterized in that institute
Stating vulcanizing agent is peroxide vulcanizing agent；Including the bis- butylperoxyisopropyl benzene of 1,3-, 1,4- dual-tert-butyl peroxy isopropyl
Base benzene, 2,5- dimethyl -2,5- two (t-butylperoxy) hexane, 2,5- dimethyl -2,5- di-t-butyl peroxy -3- oneself
Alkynes.
3. dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer according to claim 1, which is characterized in that the sulphur
Change auxiliary agent be TAIC, 0.1 ~ 5 part of dosage.
4. a kind of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer according to claim 1, which is characterized in that institute
State stabilizer be hindered amine, phosphite ester, free radical scavenger class processing stabilizers, 0.01 ~ 3 part of dosage.
5. a kind of prepare a kind of system of dynamic vulcanization nitrile rubber/nylon thermoplastic's elastomer described in one of Claims 1 to 4
Preparation Method, it is characterised in that the following steps are included:
(1) rubber granulation: first nitrile rubber and crosslinking agent, cross-linking aid, stabilizer and antioxidant are mixed in room temperature mixer
It closes uniformly, rubber granulation is carried out in rubber comminutor；
(2) dynamic vulcanization: stirring evenly rubber particles and nylon particle in high-speed mixer, the rubber and Buddhist nun mixed
Imperial mixture is put into and carries out dynamic vulcanization in double screw extruder, and 190 ~ 230 DEG C of extruder temperature, screw speed 150 ~
400rpm。
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Cited By (9)
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| CN110092954A (en) * | 2018-01-29 | 2019-08-06 | 中国石油化工股份有限公司 | Nitrile rubber/nylon thermoplastic's elastomer and preparation method thereof |
| CN111959069A (en) * | 2020-01-07 | 2020-11-20 | 中裕软管科技股份有限公司 | Heat-resistant water belt and preparation method thereof |
| CN112080052A (en) * | 2020-09-27 | 2020-12-15 | 烟台橡研材料科技有限公司 | Air suction noise reduction rubber and preparation method thereof |
| CN113549255A (en) * | 2021-08-18 | 2021-10-26 | 徐州工业职业技术学院 | Preparation method of anti-aging butyronitrile rubber powder-based PVC (polyvinyl chloride) thermoplastic elastomer and application of anti-aging butyronitrile rubber powder-based PVC thermoplastic elastomer in automobile parts |
| CN113831612A (en) * | 2020-06-24 | 2021-12-24 | 中国石油化工股份有限公司 | Oil-resistant TPV composition and preparation method thereof |
| CN114350042A (en) * | 2022-02-11 | 2022-04-15 | 道恩高材(北京)科技有限公司 | Oil-resistant and high-temperature-resistant thermoplastic vulcanized rubber of hydrogenated butyronitrile/polyamide system |
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| CN114437425A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Thermoplastic vulcanized rubber composition, thermoplastic vulcanized rubber, and preparation method and application thereof |
| CN114437426A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Thermoplastic vulcanized rubber composition, thermoplastic vulcanized rubber, and preparation method and application thereof |
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| CN110092954A (en) * | 2018-01-29 | 2019-08-06 | 中国石油化工股份有限公司 | Nitrile rubber/nylon thermoplastic's elastomer and preparation method thereof |
| CN110092954B (en) * | 2018-01-29 | 2021-07-02 | 中国石油化工股份有限公司 | Nitrile rubber/nylon thermoplastic elastomer and preparation method thereof |
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Application publication date: 20190726 |