CN106832612A - A kind of attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization - Google Patents
A kind of attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization Download PDFInfo
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- CN106832612A CN106832612A CN201710079855.1A CN201710079855A CN106832612A CN 106832612 A CN106832612 A CN 106832612A CN 201710079855 A CN201710079855 A CN 201710079855A CN 106832612 A CN106832612 A CN 106832612A
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- attapulgite
- inorganic hybridization
- organic inorganic
- coupling agent
- ludox
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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
- 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
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization.The present invention have developed novel organosilicon coupling agent and coordinate Ludox, organic inorganic hybridization surface modified attapulgite soil, so as to be applied to the filling-modified of ethylene propylene diene rubber, obtain the attapulgite modified ternary ethlene propyene rubbercompound material of high performance organic inorganic hybridization.The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, it is made up of the raw material of following quality proportioning：Attapulgite modified 100~500 parts of 100 parts of ethylene propylene diene rubber, organic inorganic hybridization, 10~30 parts of paraffin oil, 0.5~4 part of sulphur, 0.5~4 part of auxiliary curing agent.
Description
Technical field
It is modified more specifically to a kind of organic inorganic hybridization the present invention relates to a kind of ternary ethlene propyene rubbercompound material
Attapulgite ternary ethlene propyene rubbercompound material.
Background technology
Resistance to ag(e)ing of the ethylene propylene diene rubber (ethylene propylene dien monomer, EPDM) with height,
Outstanding corrosion-resistant, water-fast, oil resistivity, and excellent insulating properties, are widely used in air locking, electric insulation product, outdoor
Sports equipment product etc..But because EPDM is noncrystalline rubber, need reinforcement to obtain preferable performance indications.Conventional
EPDM supporting materials are carbon blacks, filling number and the grain diameter influence of the carbon black performance of reinforced rubber.Although black-reinforced EPDM
Good physical property can be obtained, but the EPDM rubber composite product of black can only be produced.Nano inorganic mineral are as covered
The aboundresources such as de- soil, fine particle calcium carbonate, silica, potter's clay, cheap, species is various, is widely used in reinforcement EPDM, can produce
Light color or colour EPDM products.Modified montmorillonoid filling EPDM (Influence of clay modification on the
structure and mechanical properties of EPDM/montmorillonite nanocomposites
[J].Polym Test,2004,23:217-223.), although reducing the crosslink density of rubber, improve the stretching of material
Intensity.Using the bentonite of different proportion, calcium carbonate and silica-filled EPDM (Comparative study on the
effect of partial replacement of silica or calcium carbonate by bentonite on
the properties of EPDM composites[J].Polym Test,2012,31:199-208.), then can find with
The increase of bentonite ratio, cure time shortens.
Concave-convex clay rod (Attapulgite, palygorskite) is with concavo-convex referred to as " attapulgite " or " recessed soil "
Rod stone is a kind of porous type chain layered hydrous richness magnesium alumino metasilicate salt clay mineral (hereinafter referred to as " concave convex rod of main component
Soil "), belong to typical nanometer-sub-micron nonmetallic ore.The theoretical chemistry formula of attapulgite is Si8Mg5O20(OH)2(H2O)4·
4H2O.8 hydrones are contained within each crystal unit, wherein 4 are coordinated with magnesium ion, as the crystallization water；Another 4 moisture
Son exists with free state, is bound by structure pore；Also there is hydroxyl structure in inside configuration.The actual composition of attapulgite with
By the substitution of Al, Mg is varied from Si by the substitution (referred to as class matter is with mutually replacement) of the elements such as Al, Fe, with the place of production and ore bed
The difference of structure, composition also slightly has difference.
Attapulgite microstructure generally comprises three levels：(1) basic structural unit --- micro- bar-shaped or fibrous list
Crystal, abbreviation rod is brilliant, and unit layer has upper and lower two silicon-oxy tetrahedrons double-strand chip, centre 5 magnesium (or aluminium) oxygen octahedrals of folder
Body, each elementary layer connects into the crystal structure of duct formula by the oxygen atom for sharing each other, forms fibrous monocrystalline (many
In straight needle-like, bar-shaped or threadiness), the brilliant a diameter of 0.01 μm of order of magnitude of single rod, length is up to 0.1~1 μm；(2)
By the rod crystalline substance beam of rod crystalline substance aggregate parallel, the numerous Parallel Tunnel of self-assembling formation is empty between nano stick crystal fiber arranged in parallel
Gap, the internal void volume of micron level attapulgite accounts for more than the 30% of particle overall volume；(3) by brilliant beam (including rod is brilliant) phase
Mutually assemble the various aggregations piled up and formed, particle diameter is usually 0.01~0.1mm orders of magnitude.It is raw by itself hydrophily and tradition
The limitation of production. art, usual attapulgite products particle diameter is big, compound with polymer often to play filling incremental contribution.
Patent No. EP0221225 patents disclose a kind of surface modifying method of attapulgite, using quaternary ammonium salt low
Attapulgite is processed in polar solvent, the rheological property of attapulgite can be effectively improved.But desolvation is needed after treatment, is located
Science and engineering skill is more complicated.Attapulgite is processed through cetyl trimethylammonium bromide (CTAB), and nanometer is prepared using situ aggregation method
(situ aggregation method prepares nano-attapulgite/lactic acid composite material [J] composites to attapulgite/lactic acid composite material
Journal, 2010,27 (4):45-51.), the mechanical property and heat endurance of composite are improved.The but in-situ polymerization work
Skill industrialization is realized more difficult.Attapulgite is applied to ternary ethlene propyene rubbercompound material, current conventional surface process agent is
Silane coupler and titanate coupling agent are (such as：Influence [J] of modified synergic attapulgite to ternary ethylene-propylene rubber reinforced performance
Silicate journal, 2013,41 (1):71-75；The preparation of attapulgite/ethylene propylene diene rubber nano composite material and performance [J]
China Synthetic Rubber Industry, 2016,39 (1):15-19.), the selection of coupling agent and modified material but in above-mentioned method of modifying
Performance etc. all also has raising to be optimized.It is indicated above that the surface of attapulgite is modified and is applied to polymer matrix composite
It is crucial.Therefore, synthesizing new attapulgite's surface inorganic agent is designed, using rational surface treatment mode, for attapulgite
Ternary ethlene propyene rubbercompound material, is that exploitation novel tertiary EP rubbers is combined so as to solve problems of the prior art
One of key of material, is also the effective means rationally using attapulgite.
The content of the invention
Present invention aim to address problems of the prior art and deficiency, there is provided a kind of organic inorganic hybridization is modified
Attapulgite ternary ethlene propyene rubbercompound material.The present invention have developed novel organosilicon coupling agent and coordinate Ludox, You Jiwu
Machine hydridization surface modified attapulgite soil, so as to be applied to the filling-modified of ethylene propylene diene rubber, obtains high performance organic-inorganic
Hybrid modification attapulgite ternary ethlene propyene rubbercompound material.
The present invention also provides the preparation method of the attapulgite modified ternary ethlene propyene rubbercompound material of the organic inorganic hybridization,
Method is simple and easy to apply, wherein the loading in ethylene propylene diene rubber of the attapulgite after treatment is big, rubber rheology processability is good
Good, the EPDM composite after vulcanization shows good shock absorbing capability.
The present invention is achieved by the following technical solutions：
The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, it is matched somebody with somebody by following quality
The raw material of ratio is made：
The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, its further technical side
Case be described organic inorganic hybridization it is attapulgite modified be by modified concavo-convex of organo-silicon coupling agent and Ludox surface
Rod soil.
The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, its further technology
Scheme is that the attapulgite modified surface modification step of described organic inorganic hybridization is：Attapulgite is stirred in high-speed mixer
Mix and spray under state organo-silicon coupling agent, organo-silicon coupling agent quality consumption is 0.1~0.5%, 80~100 DEG C of attapulgite
Mixed at high speed 30 minutes or more；Then Ludox is sprayed, Ludox quality consumption is 2~8%, the 100~130 of attapulgite
DEG C mixed at high speed 90 minutes or more, obtains organic inorganic hybridization attapulgite modified.
The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, its further technology
Scheme is that described organo-silicon coupling agent structural formula is as follows：
[CH3(CH2)n]mSi(OR)4-m
Wherein R is methyl or ethyl；M=1,2 or 3；N=15~23.It is preferred that m=2, n=15~19.
The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, its further technology
Scheme can also be that described Ludox is acidic silicasol or alkaline silica sol, and the solid content of Ludox is 20~30%.Silicon
Colloidal sol is preferably alkaline silica sol.
The attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, its further technical side
Case can also be that described auxiliary curing agent is vulcanizing agent DZ, vulcanizing agent PZ, vulcanizing agent M, vulcanizing agent DM or its combination.
The preparation method of the attapulgite modified ternary ethlene propyene rubbercompound material of organic inorganic hybridization of the invention, it includes
Following steps：
By each component raw material, in the rubber internal mixer after normal temperature banburying 20~60 minutes, mill mill flakiness, and put
Put in flat plate mold, flat plate mold is vulcanized 10~25 minutes for 150~180 DEG C in vulcanizing press, obtain organic-inorganic
Hybrid modification attapulgite ternary ethlene propyene rubbercompound material.
Compared with prior art the invention has the advantages that：
Routine chain alkyl organo-silicon coupling agent is mainly DH-109 (C at present12H25CH3Si(OCH3)2), in fabric treating
It is used widely with rubber and plastic processing.Organo-silicon coupling agent in the present invention, more conventional alkyl organic coupling agent possesses more
Alkyl long, and relatively many chain alkyl functional groups.Through the attapulgite that organo-silicon coupling agent of the present invention is processed, that is, show
The compatibility good with ethylene propylene diene rubber, ratio that can be higher is filling-modified；Simultaneously more alkyl functional is rolled into a ball and more long
Alkyl segment stronger intermolecular force, the rubber after vulcanization can be produced to show with ethylene propylene diene rubber macromolecular chain
Good mechanical property, is embodied in good shock absorbing capability.In addition, the attapulgite processed by Ludox, recessed
Convex rod soil surface will adsorb nano-silicon dioxide particle.The nano-silicon dioxide particle of attapulgite particle surface, thus it is possible to vary
The surface polarity of attapulgite, and organo-silicon coupling agent of the invention forms cooperative effect, is not losing rubber composite power
Raising attapulgite loading under the premise of performance is learned, while the substantially processing rheological property of optimization EPDM.
The modified filling-modified EPDM composite of attapulgite of organic inorganic hybridization of the invention, it is recessed after treatment
Convex rod soil loading in ethylene propylene diene rubber is big, and rubber rheology processability is good, the EPDM composite after vulcanization
Show good shock absorbing capability；When the attapulgite modified consumption of organic inorganic hybridization for ethylene propylene diene rubber 100~
When 500%, EPDM composite co-mixing system still shows good rheology processability.Ethylene propylene diene rubber can be with
Using conventional vulcanizing system, the EPDM composite after vulcanization shows good shock absorbing capability.
Specific embodiment
Following examples are the preparations of composite flame-retardant agent organosilicon original position encapsulation.
Embodiment 1
Using coupling agent CH3(CH2)15Si(OCH3)3Treatment attapulgite, coupling agent consumption is the 0.3% of attapulgite；
Alkaline silica sol (solid content is 25%) is used to process attapulgite, the consumption of alkaline silica sol is the 3.5% of attapulgite.Tool
Body handling process is：Attapulgite sprays above-mentioned organo-silicon coupling agent under stirring in high-speed mixer, and 95 DEG C of high speeds are mixed
Close 30 minutes；Then Ludox is sprayed, 125 DEG C of mixed at high speed 90 minutes obtain organic inorganic hybridization attapulgite modified.
Ethylene-propylene diene copolymer material formula is：
The EPDM of above-mentioned formula, in the rubber internal mixer after normal temperature banburying 40 minutes, mill mill is into thin
Piece, cuts and is placed in flat plate mold on demand, and mold thickness is 10mm.Inside there is the flat plate mold of EPDM flat
165 DEG C vulcanize 15 minutes in plate vulcanizer, finally give the EPDM composite sheet that thickness is 10mm, and test impact is inhaled
Receipts amount is 28%.
Embodiment 2
Using coupling agent [CH3(CH2)17]2Si(OCH2CH3)2Treatment attapulgite, coupling agent consumption is attapulgite
0.4%；Alkaline silica sol (solid content is 28%) is used to process attapulgite, the consumption of alkaline silica sol is attapulgite
5.5%.Specifically handling process is：Attapulgite sprays above-mentioned organo-silicon coupling agent, 90 under stirring in high-speed mixer
DEG C mixed at high speed 30 minutes；Then spray Ludox, 115 DEG C of mixed at high speed 90 minutes, obtain organic inorganic hybridization be modified it is concavo-convex
Rod soil.
Ethylene-propylene diene copolymer material formula is：
The EPDM of above-mentioned formula, in the rubber internal mixer after normal temperature banburying 55 minutes, mill mill is into thin
Piece, cuts and is placed in flat plate mold on demand, and mold thickness is 12mm.Inside there is the flat plate mold of EPDM flat
175 DEG C vulcanize 19 minutes in plate vulcanizer, finally give the EPDM composite sheet that thickness is 12mm, and test impact is inhaled
Receipts amount is 38%.
Embodiment 3
Using coupling agent [CH3(CH2)19]3SiOCH2CH3Treatment attapulgite, coupling agent consumption is attapulgite
0.15%；Alkaline silica sol (solid content is 22%) is used to process attapulgite, the consumption of alkaline silica sol is attapulgite
7.5%.Specifically handling process is：Attapulgite sprays above-mentioned organo-silicon coupling agent, 90 under stirring in high-speed mixer
DEG C mixed at high speed 30 minutes；Then spray Ludox, 125 DEG C of mixed at high speed 90 minutes, obtain organic inorganic hybridization be modified it is concavo-convex
Rod soil.
Ethylene-propylene diene copolymer material formula is：
The EPDM of above-mentioned formula, in the rubber internal mixer after normal temperature banburying 38 minutes, mill mill is into thin
Piece, cuts and is placed in flat plate mold on demand, and mold thickness is 13mm.Inside there is the flat plate mold of EPDM flat
175 DEG C vulcanize 23 minutes in plate vulcanizer, finally give the EPDM composite sheet that thickness is 13mm, and test impact is inhaled
Receipts amount is 40%.
Embodiment 4
Using coupling agent [CH3(CH2)23]2Si(OCH3)2Treatment attapulgite, coupling agent consumption is attapulgite
0.42%；Acidic silicasol (solid content is 28%) is used to process attapulgite, the consumption of acidic silicasol is attapulgite
7.5%.Specifically handling process is：Attapulgite sprays above-mentioned organo-silicon coupling agent, 90 under stirring in high-speed mixer
DEG C mixed at high speed 30 minutes；Then spray Ludox, 115 DEG C of mixed at high speed 90 minutes, obtain organic inorganic hybridization be modified it is concavo-convex
Rod soil.
Ethylene-propylene diene copolymer material formula is：
The EPDM of above-mentioned formula, in the rubber internal mixer after normal temperature banburying 30 minutes, mill mill is into thin
Piece, cuts and is placed in flat plate mold on demand, and mold thickness is 8mm.Inside there is the flat plate mold of EPDM flat
155 DEG C vulcanize 21 minutes in plate vulcanizer, finally give the EPDM composite sheet that thickness is 8mm, and test impact is inhaled
Receipts amount is 22%.
Embodiment 5
Using coupling agent [CH3(CH2)19]2Si(OCH2CH3)2Treatment attapulgite, coupling agent consumption is attapulgite
0.34%；Alkaline silica sol (solid content is 28%) is used to process attapulgite, the consumption of alkaline silica sol is attapulgite
6.5%.Specifically handling process is：Attapulgite sprays above-mentioned organo-silicon coupling agent, 90 under stirring in high-speed mixer
DEG C mixed at high speed 30 minutes；Then spray Ludox, 125 DEG C of mixed at high speed 90 minutes, obtain organic inorganic hybridization be modified it is concavo-convex
Rod soil.
Ethylene-propylene diene copolymer material formula is：
The EPDM of above-mentioned formula, in the rubber internal mixer after normal temperature banburying 30 minutes, mill mill is into thin
Piece, cuts and is placed in flat plate mold on demand, and mold thickness is 12mm.Inside there is the flat plate mold of EPDM flat
170 DEG C vulcanize 13 minutes in plate vulcanizer, finally give the EPDM composite sheet that thickness is 12mm, and test impact is inhaled
Receipts amount is 41%.
Embodiment 6
Using coupling agent [CH3(CH2)15]2Si(OCH2CH3)2Treatment attapulgite, coupling agent consumption is attapulgite
0.38%；Alkaline silica sol (solid content is 22%) is used to process attapulgite, the consumption of alkaline silica sol is attapulgite
3.5%.Specifically handling process is：Attapulgite sprays above-mentioned organo-silicon coupling agent, 90 under stirring in high-speed mixer
DEG C mixed at high speed 30 minutes；Then spray Ludox, 105 DEG C of mixed at high speed 90 minutes, obtain organic inorganic hybridization be modified it is concavo-convex
Rod soil.
Ethylene-propylene diene copolymer material formula is：
The EPDM of above-mentioned formula, in the rubber internal mixer after normal temperature banburying 30 minutes, mill mill is into thin
Piece, cuts and is placed in flat plate mold on demand, and mold thickness is 12mm.Inside there is the flat plate mold of EPDM flat
158 DEG C vulcanize 23 minutes in plate vulcanizer, finally give the EPDM composite sheet that thickness is 12mm, and test impact is inhaled
Receipts amount is 42%.
Claims (9)
1. the attapulgite modified ternary ethlene propyene rubbercompound material of a kind of organic inorganic hybridization, it is characterised in that matched somebody with somebody by following quality
The raw material of ratio is made：
2. composite according to claim 1, it is characterised in that described organic inorganic hybridization is attapulgite modified to be
By the modified attapulgite of organo-silicon coupling agent and Ludox surface.
3. composite according to claim 2, it is characterised in that described organic inorganic hybridization is attapulgite modified
Surface modification step is：Attapulgite sprays organo-silicon coupling agent, organo-silicon coupling agent under stirring in high-speed mixer
Quality consumption is 0.1~0.5%, 80~100 DEG C of mixed at high speed 30 minutes or more of attapulgite；Then Ludox is sprayed,
Ludox quality consumption is 2~8%, 100~130 DEG C of mixed at high speed 90 minutes or more of attapulgite, obtains organic-inorganic
Hybrid modification attapulgite.
4. composite according to claim 3, it is characterised in that described organo-silicon coupling agent structural formula is as follows：
[CH3(CH2)n]mSi(OR)4-m
Wherein R is methyl or ethyl；M=1,2 or 3；N=15~23.
5. composite according to claim 4, it is characterised in that the m=2 described in organo-silicon coupling agent structural formula, n
=15~19.
6. composite according to claim 3, it is characterised in that described Ludox is acidic silicasol or alkaline silicon
Colloidal sol, the solid content of Ludox is 20~30%.
7. composite according to claim 6, it is characterised in that described Ludox is alkaline silica sol.
8. composite according to claim 1, it is characterised in that described auxiliary curing agent is vulcanizing agent DZ, vulcanizing agent
PZ, vulcanizing agent M, vulcanizing agent DM or its combination.
9. a kind of preparation method of composite as described in claim 1-8 is any, its feature is comprised the following steps：
By each component raw material, in the rubber internal mixer after normal temperature banburying 20~60 minutes, mill mill flakiness, and be placed on
In flat plate mold, flat plate mold is vulcanized 10~25 minutes for 150~180 DEG C in vulcanizing press, obtain organic inorganic hybridization
Attapulgite modified ternary ethlene propyene rubbercompound material.
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| CN108690233A (en) * | 2018-05-12 | 2018-10-23 | 南京工程学院 | A kind of butadiene-styrene rubber vulcanizate of resistance to organic media and preparation method thereof |
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Application publication date: 20170613 |