CN105949697A - High-temperature-resisting acrylic rubber and preparation method thereof - Google Patents
High-temperature-resisting acrylic rubber and preparation method thereof Download PDFInfo
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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Abstract
The invention provides high-temperature-resisting acrylic rubber which is prepared from, by weight, 30-45 parts of hard monomer-methyl methacrylate, 10-15 parts of soft monomer n-butyl acrylate, 30-35 parts of functional monomers, 20-30 parts of filler, 10-15 parts of special core-shell microspheres, 2-4 parts of initiator, 1-3 parts of vulcanizing agent and 30-60 parts of solvent. The function monomers contain one or more of hydroxide radical, carboxyl, epoxy group, aryl and phosphate. Multiple ways for improving high temperature resistance are combined and matched, the acrylic rubber with the excellent high temperature resistance is obtained, and using requirements of the prior art can be met.
Description
Technical field
The present invention relates to a kind of acrylate rubber, be specifically related to a kind of high temperature resistant acrylate rubber.
Background technology
Acrylate rubber is the rubber made for main component with the polymer of acrylate, and it has the heat resistance the same with fluorubber as silicone rubber and has as fluorubber, oil resistivity that epichlorohydrin rubber is the same with nitrile rubber.It can be used for the automobile component of the heat-resisting and resistance to lubricating oil of requirement, such as close to the various sealing members of electromotor, packing ring, filler, turbine sebific duct etc..
Performance based on its excellence, its use field is increasingly wider, requires more and more higher to its properties, and the requirement of resistance to elevated temperatures is also stepped up by acrylate rubber, and in prior art, the resistance to elevated temperatures of acrylate rubber is difficult to meet requirement.Therefore, it is badly in need of the excellent acrylate rubber of a kind of resistance to elevated temperatures and meets the demand of prior art.
Summary of the invention
Goal of the invention: the present invention provides a kind of high temperature resistant acrylate rubber, it is intended to by selecting suitable monomer, filler, preparation technology etc. to prepare the acrylate rubber of resistance to elevated temperatures.By select specific function monomer, improve crosslink density, introduce fire-retardant heatproof group improve heat-resisting quantity；Select suitable filler and modification mode, improve heat transfer efficiency, make heat shed as early as possible；Select extraordinary core-shell structure copolymer microsphere, melt heat absorption by the physics of core metal, improve resistance to elevated temperatures.The means of the comprehensive multinomial raising resistance to elevated temperatures of the present invention, cooperate, and obtain the acrylate rubber with excellent high temperature resistance performance.
Present invention also offers the preparation method of a kind of high temperature resistant acrylate rubber, its each compositional selecting specific addition opportunity, obtain the high temperature resistant acrylate rubber of ad hoc structure.
The concrete technical scheme of the present invention: a kind of high temperature resistant acrylate rubber, its raw material consists of: hard monomer methyl methacrylate 30-45 weight portion, soft monomer n-butyl acrylate 10-15 weight portion, function monomer 30-35 weight portion, filler 20-30 weight portion, extraordinary core-shell structure copolymer microsphere 10-15 weight portion, initiator 2-4 weight portion, vulcanizing agent 1-3 weight portion, solvent 30-60 weight portion；Described function monomer contain hydroxyl, carboxyl, epoxy radicals, aromatic radical, phosphate-based in one or more.
Described function monomer improves crosslink density by introducing crosslinkable groups, crosslinked group, introduces aromatic group and phosphate-based raising resistance to elevated temperatures.
Optimal technical scheme as function monomer, described function monomer is made up of 2-(Acryloyloxy)ethanol, epoxy acrylate, benzyl methacrylate and 2-HEMA phosphate ester, and 2-(Acryloyloxy)ethanol, epoxy acrylate, benzyl methacrylate and 2-HEMA phosphate ester composition weight ratio are 1:1:2:1.The introducing of 2-(Acryloyloxy)ethanol and epoxy acrylate improves acrylate rubber later stage crosslinking degree, benzyl methacrylate introduces aromatic group, improve resistance to elevated temperatures, 2-HEMA phosphate ester not only introduces hydroxyl, also it is further introduced into bound phosphate groups, improves flame retardant type, temperature tolerance.By selecting the suitable amounts of four kinds of monomers, balancing crosslinking degree and the acrylate rubber pliability as elastomer, the acrylate rubber finally given also has good resistance to elevated temperatures.
Described filler is made up of modified graphene oxide and aluminium sesquioxide, and both mass ratioes are 1:2.Graphene oxide forms, with aluminium sesquioxide, the structure contacted, and effectively raises heat transfer efficiency, makes heat shed in a large number, improves the resistance to elevated temperatures of overall acrylate.
As optimal technical scheme, described modified graphene oxide is silane coupler modified graphene oxide.Graphene oxide is to use classical Hummers method to prepare, and it remains the big π bond structure of part class phenyl ring, has certain heat conductivility.Silane coupler can select kind common on market, can be KH-550, KH-560 etc., and coupling agent, by hydrolysis, carries out mix and blend overnight with graphene oxide, obtains silane coupler modified graphene oxide.It can improve the contact stabilization of graphene oxide and aluminium sesquioxide.
As optimal technical scheme, described aluminium sesquioxide is preferably dendroid aluminium sesquioxide, use dendritic aluminium sesquioxide can improve the contact probability of aluminium sesquioxide and graphene oxide, improve heat conductivility, as early as possible heat is derived from interior, improving its heat resistance, this is other unapproachable effects of structure aluminium sesquioxide.
Graphene oxide uses the silane coupler modified degree that is uniformly dispersed not only improving Graphene and substrate ring epoxy resins, simultaneously, the use of coupling agent improves the contact stabilization of graphene oxide and aluminium sesquioxide, improve acrylate rubber heat conductivity and thermostability.
Described extraordinary core-shell structure copolymer microsphere be silicon dioxide be shell, low-melting-point metal is core.In this area, the fusing point of silicon dioxide is at about 1700 DEG C, and low-melting-point metal is below 500 DEG C.When low-melting-point metal occurs fusing, silicon dioxide can also keep its micro-sphere structure, and melting is a process absorbed heat, can under the high temperature conditions, protection acrylate rubber in certain time.
As optimal technical scheme, described low-melting-point metal is lead, zinc, stannum.The fusing point of stannum 232 DEG C, the fusing point of lead 329 DEG C, zinc is 419 DEG C.Use different metal can realize absorbing heat under different temperatures as core, present invention preferably employs extraordinary core-shell structure copolymer microsphere prepared by different metal and be used in mixed way, it is possible to achieve gradient is absorbed heat, improve overall resistance to elevated temperatures.
Described vulcanizing agent is the mixing vulcanizing system of quaternary ammonium salt and sodium stearate, and the mass ratio of quaternary ammonium salt and sodium stearate is 1:1.This vulcanizing system is novel system, can effectively realize sulfuration, improves heat resistance.
Described initiator is azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide.
The preparation method of high temperature resistant acrylate rubber, method particularly includes: step (1): the solvent taking 15-30 weight portion adds reactor, it is heated to 80-110 DEG C, then by hard monomer methyl methacrylate 30-45 weight portion, soft monomer n-butyl acrylate 10-15 weight portion, function monomer 15-17.5 weight portion, extraordinary core-shell structure copolymer microsphere 10-15 weight portion and the initiator mix homogeneously of 0.8-1.6 weight portion, at the uniform velocity it is added dropwise in reactor, dropping process completes at 1-1.5h, continues reaction 1h；Step (2): function monomer 15-17.5 weight portion, remaining 1.2-2.4 weight portion initiator and the solvent mix homogeneously of 15-30 weight portion, at the uniform velocity adds in the reactor of step (1), and dropping process completes at 0.3-1h, continues reaction 0.5h；Step (3): being added by filler 20-30 weight portion in the reactor of step (2), cooling obtains high temperature resistant acrylate rubber solution, adds vulcanizing agent 1-3 weight portion further, adds heat cure and obtain high temperature resistant acrylate rubber.
Useful technique effect: the present invention is by selecting specific function monomer, improving crosslink density, introduce fire-retardant heatproof group and improve heat-resisting quantity, and further preferred four kinds of different modes improve the function monomer of thermostabilitys, collaborative improves thermostability；Use graphene oxide and the heat conduction of aluminium sesquioxide, heat-resisting system, the point-face contact of performance, the use of dendroid aluminium sesquioxide improves contact probability, and silane coupler modified graphene oxide improves resin dispersion and contact stabilization, improves heat conductivity and thermostability.When facing temperature and being the highest, surface of graphene oxide deoxidation, become Graphene, system heat conductivity, thermostability improve further.Select extraordinary core-shell structure copolymer microsphere, melt heat absorption by the physics of core metal, improve resistance to elevated temperatures, preferably different melting points metal combination and use, it is achieved gradient is absorbed heat.The means of the comprehensive multinomial raising resistance to elevated temperatures of the present invention, cooperate, and obtain the acrylate rubber with excellent high temperature resistance performance.
Detailed description of the invention:
Embodiment
1
:
The preparation method of high temperature resistant acrylate rubber, method particularly includes: step (1): take and the solvent of 25 weight portions is added reactor, it is heated to 100 DEG C, then by hard monomer methyl methacrylate 40 weight portion, soft monomer n-butyl acrylate 12 weight portion, 2-(Acryloyloxy)ethanol 3 weight portion, epoxy acrylate 3 weight portion, benzyl methacrylate 6 weight portion, 2-HEMA phosphate ester 3 weight portion, in core-shell structure copolymer microsphere, silicon dioxide is shell, lead zinc-tin is three each 4 weight portions of class microsphere and the initiator mix homogeneously of 1.2 weight portions of core, at the uniform velocity it is added dropwise in reactor, dropping process completes at 1.5h, continue reaction 1h；Step (2): 2-(Acryloyloxy)ethanol 3 weight portion, epoxy acrylate 3 weight portion, benzyl methacrylate 6 weight portion, 2-HEMA phosphate ester 3 weight portion, remaining initiator 1.8 weight portion and solvent 25 weight portion mix homogeneously, at the uniform velocity add in the reactor of step (1), dropping process completes at 0.3h, continues reaction 0.5h；Step (3): by silane coupler modified for filler graphene oxide 10 weight portion, dendroid aluminium sesquioxide 20 weight portion adds in the reactor of step (2), cooling obtains high temperature resistant acrylate rubber solution, add vulcanizing agent quaternary ammonium salt 1 weight portion, sodium stearate 1 weight portion further, add heat cure and obtain high temperature resistant acrylate rubber.
Embodiment
2-3
And comparative example
1-7
The preparation method of embodiment 2-3 and comparative example 1-6, with embodiment 1, differs only in the difference of component, consumption, referring specifically to following table.Being simultaneously introduced with core-shell particles for filler in comparative example 7 preparation method, component, consumption are same as in Example 1.
Claims (9)
1. a high temperature resistant acrylate rubber, it is characterized in that: raw material consists of: hard monomer methyl methacrylate 30-45 weight portion, soft monomer n-butyl acrylate 10-15 weight portion, function monomer 30-35 weight portion, filler 20-30 weight portion, extraordinary core-shell structure copolymer microsphere 10-15 weight portion, initiator 2-4 weight portion, vulcanizing agent 1-3 weight portion, solvent 30-60 weight portion；Described function monomer contain hydroxyl, carboxyl, epoxy radicals, aromatic radical, phosphate-based in one or more.
High temperature resistant acrylate rubber the most as claimed in claim 1, it is characterised in that: described filler is made up of modified graphene oxide and aluminium sesquioxide, and both mass ratioes are 1:2.
High temperature resistant acrylate rubber the most as claimed in claim 2, it is characterised in that: described modified graphene oxide is to be prepared by Hummers method, is modified by silane coupler；Described aluminium sesquioxide is dendroid aluminium sesquioxide.
High temperature resistant acrylate rubber the most as claimed in claim 1, it is characterized in that: described function monomer is made up of 2-(Acryloyloxy)ethanol, epoxy acrylate, benzyl methacrylate and 2-HEMA phosphate ester, 2-(Acryloyloxy)ethanol, epoxy acrylate, benzyl methacrylate and 2-HEMA phosphate ester composition weight ratio are 1:1:2:1.
High temperature resistant acrylate rubber the most as claimed in claim 1, it is characterised in that: described extraordinary core-shell structure copolymer microsphere be silicon dioxide be shell, low-melting-point metal is core.
High temperature resistant acrylate rubber the most as claimed in claim 5, it is characterised in that: described low-melting-point metal is lead, zinc, stannum.
High temperature resistant acrylate rubber the most as claimed in claim 1, it is characterised in that: described vulcanizing agent is the mixing vulcanizing system of quaternary ammonium salt and sodium stearate, and the mass ratio of quaternary ammonium salt and sodium stearate is 1:1.
High temperature resistant acrylate rubber the most as claimed in claim 1, it is characterised in that: described initiator is azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide.
9. the preparation method of the high temperature resistant acrylate rubber according to any one of claim 1-8, it is characterised in that:
Step (1): the solvent taking 15-30 weight portion adds reactor, it is heated to 80-110 DEG C, then by hard monomer methyl methacrylate 30-45 weight portion, soft monomer n-butyl acrylate 10-15 weight portion, function monomer 15-17.5 weight portion, extraordinary core-shell structure copolymer microsphere 10-15 weight portion and the initiator mix homogeneously of 0.8-1.6 weight portion, at the uniform velocity being added dropwise in reactor, dropping process completes at 1-1.5h, continues reaction 1h；
Step (2): function monomer 15-17.5 weight portion, the initiator of remaining 1.2-2.4 weight portion and the solvent mix homogeneously of 15-30 weight portion, at the uniform velocity adds in the reactor of step (1), and dropping process completes at 0.3-1h, continues reaction 0.5h；
Step (3): being added by filler 20-30 weight portion in the reactor of step (2), cooling obtains high temperature resistant acrylate rubber solution, adds vulcanizing agent 1-3 weight portion further, adds heat cure and obtain high temperature resistant acrylate rubber.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810339625.9A CN108641257B (en) | 2016-07-22 | 2016-07-22 | High-temperature-resistant acrylate rubber |
| CN201610579763.5A CN105949697B (en) | 2016-07-22 | 2016-07-22 | A kind of high temperature resistant acrylic rubber and preparation method thereof |
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| CN201610579763.5A CN105949697B (en) | 2016-07-22 | 2016-07-22 | A kind of high temperature resistant acrylic rubber and preparation method thereof |
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| CN201810339625.9A Division CN108641257B (en) | 2016-07-22 | 2016-07-22 | High-temperature-resistant acrylate rubber |
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| CN105949697B CN105949697B (en) | 2018-06-12 |
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| CN201810339625.9A Active CN108641257B (en) | 2016-07-22 | 2016-07-22 | High-temperature-resistant acrylate rubber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107868638A (en) * | 2017-12-06 | 2018-04-03 | 成都创客之家科技有限公司 | A kind of pressure sensitive adhesive binding agent for eye speculum bonding and preparation method thereof |
| CN107955563A (en) * | 2017-12-06 | 2018-04-24 | 成都创客之家科技有限公司 | A kind of preparation method of pressure sensitive adhesive binding agent for eye speculum bonding |
| CN108587027A (en) * | 2018-05-23 | 2018-09-28 | 董大樵 | A kind of negative ion type lactoprene and its preparation method and application |
| CN109207114A (en) * | 2018-07-03 | 2019-01-15 | 南宁珀源能源材料有限公司 | It is anti-to cut away single-component anaerobic glue of piece and preparation method thereof |
| CN109312137A (en) * | 2016-07-05 | 2019-02-05 | 电化株式会社 | Acrylic rubber composition |
| CN109537102A (en) * | 2018-12-03 | 2019-03-29 | 福建坤彩材料科技股份有限公司 | Polyester master particle and preparation method thereof |
| CN110218539A (en) * | 2019-07-10 | 2019-09-10 | 广东省科学院产业技术育成中心 | A kind of organosilicon modified acrylic ester high-temperature, high-temperature insulation pressure-sensitive |
| CN113563682A (en) * | 2021-08-25 | 2021-10-29 | 山东海益橡胶科技有限公司 | Modified carboxyl acrylate rubber without guanidine accelerator and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110303633A (en) * | 2019-05-14 | 2019-10-08 | 嘉兴济铭商贸有限公司 | A kind of butadiene-styrene rubber mobile phone shell |
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- 2016-07-22 CN CN201610579763.5A patent/CN105949697B/en not_active Expired - Fee Related
- 2016-07-22 CN CN201810339625.9A patent/CN108641257B/en active Active
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| US4618390A (en) * | 1983-06-13 | 1986-10-21 | Ashland Oil, Inc. | Method for preparing laminated articles |
| CN101275059A (en) * | 2007-03-28 | 2008-10-01 | 刘萍 | Heat-resistant strippable micro-viscous pressure-sensitive adhesive film and preparation thereof |
| CN101550208A (en) * | 2008-12-23 | 2009-10-07 | 上海高分子功能材料研究所 | Continuous extrusion method by bulk polymerization of acrylate rubber |
| CN101812180A (en) * | 2010-04-20 | 2010-08-25 | 北京化工大学 | Method for preparing vulcanizing-free acrylic ester rubber |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109312137A (en) * | 2016-07-05 | 2019-02-05 | 电化株式会社 | Acrylic rubber composition |
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| CN107868638A (en) * | 2017-12-06 | 2018-04-03 | 成都创客之家科技有限公司 | A kind of pressure sensitive adhesive binding agent for eye speculum bonding and preparation method thereof |
| CN107955563A (en) * | 2017-12-06 | 2018-04-24 | 成都创客之家科技有限公司 | A kind of preparation method of pressure sensitive adhesive binding agent for eye speculum bonding |
| CN108587027A (en) * | 2018-05-23 | 2018-09-28 | 董大樵 | A kind of negative ion type lactoprene and its preparation method and application |
| CN109207114A (en) * | 2018-07-03 | 2019-01-15 | 南宁珀源能源材料有限公司 | It is anti-to cut away single-component anaerobic glue of piece and preparation method thereof |
| CN109537102A (en) * | 2018-12-03 | 2019-03-29 | 福建坤彩材料科技股份有限公司 | Polyester master particle and preparation method thereof |
| CN110218539A (en) * | 2019-07-10 | 2019-09-10 | 广东省科学院产业技术育成中心 | A kind of organosilicon modified acrylic ester high-temperature, high-temperature insulation pressure-sensitive |
| CN113563682A (en) * | 2021-08-25 | 2021-10-29 | 山东海益橡胶科技有限公司 | Modified carboxyl acrylate rubber without guanidine accelerator and preparation method thereof |
| CN113563682B (en) * | 2021-08-25 | 2023-01-17 | 山东海益橡胶科技有限公司 | Modified carboxyl acrylate rubber without guanidine accelerator and preparation method thereof |
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| CN108641257B (en) | 2020-06-12 |
| CN105949697B (en) | 2018-06-12 |
| CN108641257A (en) | 2018-10-12 |
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