CN103351539A - Ethylene-propylene-diene monomer rubber/montmorillonite nanocomposite and preparation method thereof - Google Patents
Ethylene-propylene-diene monomer rubber/montmorillonite nanocomposite and preparation method thereof Download PDFInfo
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- CN103351539A CN103351539A CN2013103114993A CN201310311499A CN103351539A CN 103351539 A CN103351539 A CN 103351539A CN 2013103114993 A CN2013103114993 A CN 2013103114993A CN 201310311499 A CN201310311499 A CN 201310311499A CN 103351539 A CN103351539 A CN 103351539A
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Abstract
The invention discloses an ethylene-propylene-diene monomer rubber/montmorillonite nanocomposite and a preparation method thereof. The preparation method comprises the following steps: preparing modified montmorillonite: adding an intercalator into montmorillonite suspending liquid, stirring, reacting, and gaining intercalator modified montmorillonite through suction filtering, washing and drying; milling: adding the intercalator modified montmorillonite and an additive into the ethylene-propylene-diene monomer rubber to carry out dense milling, adding a vulcanizing agent after the gained glue material is cooled to carry out milling, and gaining milling glue; carrying out vulcanization on the milling glue, and gaining the ethylene-propylene-diene monomer rubber/montmorillonite nanocomposite. The preparation method brings long-chain organic intercalation molecular chain containing unsaturated double bond into montmorillonite layers through an ion-exchange reaction, realizes organic functionalization of the layered montmorillonite surface, has the characteristic of co-vulcanization with ethylene-propylene-diene monomer rubber substrate molecular chain, and realizes the chemical crosslinking of inorganic blocking agent and a rubber network structure, thereby improving the mechanical property and the gas barrier property of the composite.
Description
Technical field
The invention belongs to field of high polymer material processing, be specifically related to a kind of EPDM/montmorillonite nanocomposites and preparation method thereof.
Background technology
The resistance to air loss of rubber refers to rubber to the behavior that sees through of gas, and generally the rate of permeation with gas characterizes.Rubber is one of important physical properties of rubber item to gas permeability.Rubber is the macromolecular material of a class low Tg (Tg), and use temperature is always far above Tg.Therefore, compare with glassy polymers, its gas barrier property is very low.Development along with rubber industry, increasing occasion is at the air-tightness of application of rubber, as at tyre industry, resistance to air loss is the needed most important performance of tube glue or air retaining wall material, in nuclear power and national defense industry, for guaranteeing Security of the system and reliability, to having chemically active oxygen in the system, steam, and the less micro-molecular gas such as hydrogen of size have strict restriction, the elaxtic seal that excellent barrier properties need to be arranged micro-molecular gas in a large number, and nuclear power, the running environment of the systems such as weapon is to the ageing-resistant performance of material, especially radiation resistance proposes high requirement, the isoprene-isobutylene rubber radiation resistance is relatively poor preferably for resistance to air loss commonly used in the general industry, and the good airtight property of silicon rubber of radiation resistance is poor, all can not satisfy the demand of system.
Nano combined method can effectively reduce gas to the osmosis of macromolecular material.In the particle-filled macromolecular material of laminated clay nanometer, because the existence of sheet silicate has prolonged micro-molecular gas the evolving path in matrix, thereby improved the barrier of matrix material.Utilize in-situ inserted polymerization, melt intercalation, solution intercalation, emulsion intercalation method can prepare laminated clay nanometer composite material." preparation method of clay-rubber nm-class composite material " of the propositions such as Zhang Liqun (ZL98101496.8) patented technology adopts the standby matrix material of emulsion intercalation legal system exactly.Because disperse phase is the layered inorganic nanoparticle, the effects such as the surface-area effects that nanoparticle has, quantum size effect and macroscopic quantum tunneling can affect polymer segment motion, molecular chain interaction and phase structure, thereby it is little to make matrix material have density, the premium properties such as high-strength, high-ductility.Because the good over-all properties of nano composite material, and it is abundant to have a clay resource of natural nano structure, and cheap, composite nano polymer/clay material is various countries' research and industrialization focuses in recent years.The preparation of high molecule nano composite material mainly concentrates on: on polynite and PA, PET, PE, PP compound.
The barrier property of high molecule nano composite material and inorganic particulate dispersiveness and the distribution situation in the polymer body has direct relation.Only have Nano filling and polymer interface to have when being combined preferably, nanoparticle is just understood Uniform Dispersion in polymer body, and the solubleness of gas this moment in polymkeric substance increases and the straight line reduction with the packing volume mark; If it is bad that filler is combined with polymkeric substance, then can in polymkeric substance, form " cavity ", increased on the contrary the solubleness of gas in polymkeric substance, reduce the resistance to air loss of material.
Make at present clay intercalation or to peel off common method be that to adopt organic modifiers that the inorganic clay surface is carried out organically-modified in rubber, strengthen the affinity at inorganic clay and rubber molecule interface, be convenient to the intercalation of rubber macromolecule.Organo-clay and rubber matrix interface physical bond normally in this matrix material, when being subject to external force, slippage easily occurs and affects composite property in clay and rubber interface.Zhang Liqun etc. disclose a kind of method that improves clay and styrene-butadiene rubber composite material boundary strength and performance in patent " silane coupler modified clay and the preparation method of butadiene styrene rubber nanometer composite material " (application number 200610114731.4).Adopt silane coupler modified clay, clay/butadiene styrene rubber nanometer composite material that preparation has excellent mechanical property.But this method needs clay and rubber latex to process, and that is to say the kind that is only applicable to rubber latex, has certain limitation.
Rubber is important flexible sealing material, but owing to force of cohesion less between its molecular chain and larger free volume, not good to the barrier property of gas.Although adopt inorganic barrier agent can improve its barrier property, usually can't overcome the relatively poor problem of the barrier property of matrix own, can bring simultaneously inorganic/organic materials boundary defect.
Summary of the invention
The purpose of this invention is to provide all better EPDM/montmorillonite nanocomposites and preparation method thereof of a kind of resistance to air loss, mechanical property and radiation resistance, overcome the problem of organic/inorganic boundary defect.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
A kind of preparation method of EPDM/montmorillonite nanocomposites may further comprise the steps:
Step 1: the preparation of modified montmorillonoid: intercalator is joined in the montmorillonite suspension liquid, behind the stirring reaction, through suction filtration, washing, the dry intercalator modified montmorillonoid that gets; This step will contain the long-chain of unsaturated double-bond by ion exchange reaction intercalator molecular chain is introduced between cheating engaging layer, realizes the functional organic on stratiform polynite surface.
Step 2: mixing: the intercalator modified montmorillonoid of step 1 and auxiliary agent joined carry out internally mix in the terpolymer EP rubber, add vulcanizing agent after the sizing material that the obtains cooling and carry out mixingly, obtain rubber unvulcanizate;
Step 3: the rubber unvulcanizate of step 2 vulcanized namely get EPDM/montmorillonite nanocomposites.
Further: described intercalator is both to have contained unsaturated double-bond in the molecule, contains again the organic ammonium salt of chain alkyl.Need to contain the functional group that chemical reaction can occur with polynite and terpolymer EP rubber molecular chain respectively in the intercalator, can improve the interface affinity of polynite and terpolymer EP rubber matrix.Ammonium ion in the intercalator of the present invention and the Na between cheating engaging layer
+, Ca
2+Plasma will contain between the long-chain organic intercalation agent molecular chain introducing cheating engaging layer of the two keys of unsaturated C=C by cation exchange reaction in the aqueous solution, realize the functional organic on stratiform polynite surface; Crosslinking reaction can occur with rubber molecular chain in the C=C unsaturated double-bond in the intercalator in sulfidation, make intercalator enter the cross-linked network of rubber molecule.Therefore, intercalator has played " bridging " effect between polynite and rubber molecule, thereby has improved barrier property and the mechanical property of matrix material.
Further: the molecular formula of described intercalator is CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
nCH
3Cl, n 〉=10 wherein, in an embodiment of the present invention, intercalator can be CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
11CH
3Cl, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
13CH
3Cl, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
15CH
3Br, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
15CH
3Cl, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
17CH
3Br, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
17CH
3Cl.
Further: the mass ratio of described intercalator and polynite is (1.1～1.5): 1.
Further: described vulcanizing agent is superoxide, and in an embodiment of the present invention, vulcanizing agent can be dicumyl peroxide (DCP) or 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane (DBPH).
Further: described polynite median size≤25 microns, cation exchange capacity 〉=90mmol/100g.
Further: the mass ratio of the intercalator modified montmorillonoid described in the step 2 and terpolymer EP rubber is (1～20): 100.
Further: the curing temperature described in the step 3 is 160～180 ℃.
Further: the temperature of the drying described in the step 1 is 80 ℃, and this drying temperature is optimum temps, because excess Temperature can affect structure and the performance of product; Temperature is crossed low meeting and is prolonged the dry time, affects efficient.
A kind of EPDM/montmorillonite nanocomposites adopts the preparation of above-mentioned method and gets.
The present invention compared with prior art has following beneficial effect:
The method that the present invention prepares EPDM/montmorillonite nanocomposites at first will contain between the long-chain organic intercalation agent molecular chain introducing cheating engaging layer of unsaturated double-bond by ion exchange reaction, realize the functional organic on stratiform polynite surface.The design of the reactive functional groups by intercalator and vulcanization of rubber ligand system makes it have characteristics with terpolymer EP rubber substrate molecule chain covulcanization.The stratiform polynite is peeled off or partly peel off by melt blending technique, be assembled between the rubber matrix molecular chain with sheet, by this partial order dispersing mode, utilize polynite to have large face thickness rate laminate structure and to the barrier of gas excellence, significantly prolonged micro-molecular gas the evolving path in matrix, and because the chemically crosslinked of inorganic barrier agent and rubber network structure, overcome the problem of inorganic/organic interface defective, thereby improved mechanical property and the gas barrier property of matrix material.
Description of drawings
Fig. 1 is the electron-microscope scanning figure of MMT/EPDM matrix material, and wherein (A) is blank sample; (B) be 5phr DK2/EPDM; (C) be 5phr OMMT/EPDM; (D) be 5phr VMMT/EPDM; Phr is expressed as the content of additive in the rubber; DK2 is commercially available organic modification montmonrillonite; OMMT is the organo montmorillonite of CTAB modification; VMMT is the organo montmorillonite of intercalator modification.
Embodiment
The invention will be further elaborated and explanation below in conjunction with embodiments of the invention.
Embodiment 1:
50g polynite (MMT) speed with 1500r/min in the ultrapure water of 1000ml was stirred 3 hours, mix rear static spending the night, make montmorillonite suspension liquid.In montmorillonite suspension liquid, add the intercalator of 1.1 times of equivalents (for easy, to contain the intercalator of chain alkyl ammonium salt of vinyl referred to as VD), behind stirring reaction 6h under the normal temperature, suction filtration, washing 2 times, made sample 80 ℃ of dryings in vacuum chamber obtained intercalator modified montmorillonoid (for easy, the polynite that will contain the chain alkyl ammonium salt intercalator modification of vinyl is called for short VMMT) in 24 hours.
Get 100 parts of terpolymer EP rubbers (EPDM) and put banburying 2min to the Banbury mixer, the banburying Temperature Setting is 90 ℃, in Banbury mixer, add successively intercalator modified montmorillonoid VMMT1 part, 30 parts of white carbon blacks, 5 parts in zinc oxide, 1 part of stearic acid, 4 parts of paraffin oils, mixing 8min obtains rubber unvulcanizate.In two rod mills, above-mentioned rubber unvulcanizate is added vulcanizing agent DCP4 part, mixingly be pressed into thin slice after evenly.After at room temperature parking 24h, thin slice is put into mould, vulcanize at vulcanizing press, curing temperature is 170 ℃, and sulfide stress is 10MPa, and curing time is 8min, obtains intercalator modified montmorillonoid and EPDM matrix material.By the national standard test, the mechanical property of matrix material sees Table 2, and gas barrier property sees Table 3.
In the present embodiment, intercalator can be selected the chain alkyl ammonium salt that contains styryl, and can select particularly molecular formula is CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
11CH
3Cl.In other embodiments of the invention, intercalator can be selected the chain alkyl ammonium salt that contains styryl, and can select particularly molecular formula is CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
13CH
3Cl, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
15CH
3Br, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
15CH
3Cl, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
17CH
3Br, CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
17CH
3Cl.
In the above-described embodiment, vulcanizing agent is dicumyl peroxide (DCP).
In the above-described embodiment, polynite median size≤25 micron, cation exchange capacity 〉=90mmol/100g.
Embodiment 2:
As different from Example 1, polynite VMMT content is 3 parts among the EPDM, and all the other processing condition and operation steps are with embodiment 1, and the mechanical property of matrix material sees Table 2, and gas barrier property sees Table 3.
Embodiment 3:
As different from Example 1, polynite VMMT content is 5 parts among the EPDM, and all the other processing condition and operation steps are with embodiment 1, and the mechanical property of matrix material sees Table 2, and gas barrier property sees Table 3.
Embodiment 4:
As different from Example 1, polynite VMMT content is 7 parts among the EPDM, and all the other processing condition and operation steps are with embodiment 1, and the mechanical property of matrix material sees Table 2, and gas barrier property sees Table 3.
Embodiment 5:
As different from Example 1, polynite VMMT content is 9 parts among the EPDM, and all the other processing condition and operation steps are with embodiment 1, and the mechanical property of matrix material sees Table 2, and gas barrier property sees Table 3.
Embodiment 6:
As different from Example 1, add the intercalator VD of 1.3 times of equivalents in montmorillonite suspension liquid, intercalator modified montmorillonoid VMMT consumption is 3 parts, and all the other processing condition and operation steps are with embodiment 1.
Embodiment 7:
As different from Example 1, intercalator modified montmorillonoid VMMT consumption is 3 parts, and vulcanizing agent changes 2 into, 5-dimethyl-2,5-bis(t-butylperoxy) hexane (being called for short DBPH), 175 ℃ of curing temperatures, curing time is 10 minutes, and all the other processing condition and operation steps are with embodiment 1.
The comparative example 1:
As different from Example 1, polynite VMMT content is 0 part among the EPDM, and all the other processing condition and operation steps are with embodiment 1, and the mechanical property of material sees Table 2, and gas barrier property sees Table 3.
The comparative example 2:
5gMMT is stirred formation suspension with an amount of pure water, add 2.1g cetyl trimethylammonium bromide (CTAB) in suspension, be warming up to 85 ℃, suction filtration behind the mechanical stirring mixed solution 2h, and with the ultrapure water cleaning for several times.Product is put into the organo montmorillonite (OMMT) that obtains the CTAB modification after the vacuum drying oven drying.
As different from Example 1, used 3 parts of the organo montmorillonites (OMMT) of CTAB modification among the EPDM, all the other processing condition and operation steps are with embodiment 1, and the mechanical property of material sees Table 2, and gas barrier property sees Table 3.
The comparative example 3:
Different from comparative example 2 is: used 7 parts of the organo montmorillonites (OMMT) of CTAB modification among the EPDM, all the other processing condition and operation steps are with embodiment 1, and the mechanical property of material sees Table 2, and gas barrier property sees Table 3.
Table 1: the component add-on of comparative example 1-3 and embodiment 1-7
| ? | The intercalator modification is covered | Intercalator | Intercalator and illiteracy are taken off | Vulcanizing agent | Rubber consumption |
| ? | Take off soil (umber) | ? | The weight ratio of soil | ? | (umber) |
| Comparative Examples 1 | 0 | 0 | -- | DCP | 100 |
| Comparative Examples 2 | 3 | CTAB | -- | DCP | 100 |
| Comparative Examples 3 | 7 | CTAB | -- | DCP | 100 |
| Embodiment 1 | 1 | VD | 1.1 | DCP | 100 |
| Embodiment 2 | 3 | VD | 1.1 | DCP | 100 |
| Embodiment 3 | 5 | VD | 1.1 | DCP | 100 |
| Embodiment 4 | 7 | VD | 1.1 | DCP | 100 |
| Embodiment 5 | 9 | VD | 1.1 | DCP | 100 |
| Embodiment 6 | 3 | VD | 1.3 | DCP | 100 |
| Embodiment 7 | 3 | VD | 1.1 | DBPH | 100 |
Table 2: the mechanical property of comparative example 1-3 and embodiment 1-5
Table 3: the gas barrier property of comparative example 1-3 and embodiment 1-5
Although invention has been described with reference to explanatory embodiment of the present invention here, above-described embodiment only is the better embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and embodiment will drop within the disclosed principle scope and spirit of the application.
Claims (10)
1. the preparation method of an EPDM/montmorillonite nanocomposites is characterized in that may further comprise the steps:
Step 1: the preparation of modified montmorillonoid: intercalator is joined in the montmorillonite suspension liquid, behind the stirring reaction, through suction filtration, washing, the dry intercalator modified montmorillonoid that gets;
Step 2: mixing: the intercalator modified montmorillonoid of step 1 and auxiliary agent joined carry out internally mix in the terpolymer EP rubber, add vulcanizing agent after the sizing material that the obtains cooling and carry out mixingly, obtain rubber unvulcanizate;
Step 3: the rubber unvulcanizate of step 2 vulcanized namely get EPDM/montmorillonite nanocomposites.
2. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1 is characterized in that described intercalator is both to have contained the two keys of C=C in the molecule, contains again the organic ammonium salt of chain alkyl.
3. the preparation method of EPDM/montmorillonite nanocomposites according to claim 2, the molecular formula that it is characterized in that described intercalator is CH
2CHC
6H
4CH
2N (CH
3)
2(CH
2)
nCH
3Cl, wherein n 〉=10.
4. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1 is characterized in that the mass ratio of described intercalator and polynite is (1.1～1.5): 1.
5. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1 is characterized in that described vulcanizing agent is superoxide.
6. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1 is characterized in that described polynite median size≤25 microns, cation exchange capacity 〉=90mmol/100g.
7. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1 is characterized in that the mass ratio of the intercalator modified montmorillonoid described in the step 2 and terpolymer EP rubber is (1～20): 100.
8. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1 is characterized in that the curing temperature described in the step 3 is 160～180 ℃.
9. the preparation method of EPDM/montmorillonite nanocomposites according to claim 1, the temperature that it is characterized in that the drying described in the step 1 is 80 ℃.
10. EPDM/montmorillonite nanocomposites is characterized in that adopting each described method preparation of claim 1～9 and gets.
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| CN106046566A (en) * | 2016-07-19 | 2016-10-26 | 合肥毅创钣金科技有限公司 | EPDM (ethylene-propylene-diene monomer) rubber sealing strip with gas tightness enhanced by graphite and butyl rubber powder |
| CN115678171A (en) * | 2022-11-11 | 2023-02-03 | 国网新疆电力有限公司电力科学研究院 | Preparation method of ultralow cold-resistant ethylene propylene diene monomer rubber sealing ring |
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Application publication date: 20131016 |