CN108129253A - A kind of analysis method of EPDM - Google Patents
A kind of analysis method of EPDM Download PDFInfo
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- CN108129253A CN108129253A CN201711390740.0A CN201711390740A CN108129253A CN 108129253 A CN108129253 A CN 108129253A CN 201711390740 A CN201711390740 A CN 201711390740A CN 108129253 A CN108129253 A CN 108129253A
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- analysis
- microwave heating
- alkane
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- 238000004458 analytical method Methods 0.000 title claims abstract description 60
- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 52
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000003851 corona treatment Methods 0.000 claims abstract description 22
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 21
- 239000002510 pyrogen Substances 0.000 claims abstract description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 33
- 239000012188 paraffin wax Substances 0.000 claims description 22
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 16
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical class CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 11
- 229920002554 vinyl polymer Polymers 0.000 claims description 11
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- GXDHCNNESPLIKD-UHFFFAOYSA-N 2-methylhexane Chemical class CCCCC(C)C GXDHCNNESPLIKD-UHFFFAOYSA-N 0.000 claims description 5
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 5
- JVSWJIKNEAIKJW-UHFFFAOYSA-N 2-Methylheptane Chemical class CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 3
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 claims 1
- 239000000470 constituent Substances 0.000 abstract description 2
- 229920001971 elastomer Polymers 0.000 description 45
- 239000005060 rubber Substances 0.000 description 45
- 238000000034 method Methods 0.000 description 14
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical group C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 13
- 239000005977 Ethylene Substances 0.000 description 13
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 13
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 12
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 6
- 239000003292 glue Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000000178 monomer Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- 238000004073 vulcanization Methods 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- OJOWICOBYCXEKR-KRXBUXKQSA-N (5e)-5-ethylidenebicyclo[2.2.1]hept-2-ene Chemical compound C1C2C(=C/C)/CC1C=C2 OJOWICOBYCXEKR-KRXBUXKQSA-N 0.000 description 2
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000006259 organic additive Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010059 sulfur vulcanization Methods 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 239000005061 synthetic rubber Substances 0.000 description 2
- INYHZQLKOKTDAI-UHFFFAOYSA-N 5-ethenylbicyclo[2.2.1]hept-2-ene Chemical compound C1C2C(C=C)CC1C=C2 INYHZQLKOKTDAI-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000003811 acetone extraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- OAIVIYSBZFEOIU-UHFFFAOYSA-N chloroform;propan-2-one Chemical compound CC(C)=O.ClC(Cl)Cl OAIVIYSBZFEOIU-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229920003020 cross-linked polyethylene Polymers 0.000 description 1
- 239000004703 cross-linked polyethylene Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- MAHNFPMIPQKPPI-UHFFFAOYSA-N disulfur Chemical compound S=S MAHNFPMIPQKPPI-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005442 electron-positron pair Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- PRBHEGAFLDMLAL-UHFFFAOYSA-N hexa-1,4-diene Chemical class CC=CCC=C PRBHEGAFLDMLAL-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 229920002681 hypalon Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C4/00—Preparation of hydrocarbons from hydrocarbons containing a larger number of carbon atoms
- C07C4/02—Preparation of hydrocarbons from hydrocarbons containing a larger number of carbon atoms by cracking a single hydrocarbon or a mixture of individually defined hydrocarbons or a normally gaseous hydrocarbon fraction
- C07C4/04—Thermal processes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to constituent analysis field more particularly to a kind of analysis methods of EPDM.A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, microwave heating is pyrolyzed, with infrared analysis pyrogen.
Description
Technical field
The invention belongs to constituent analysis field more particularly to a kind of analysis methods of EPDM.
Background technology
Rubber plays more next due to having the characteristics such as elasticity is high, air-tightness is good in fields such as aviation, transport and industrial productions
More important role.Rubber complicated component, containing rubber, compounding agent and additive etc. be a variety of organic and inorganic component, respectively
Kind component all has a certain impact to its performance, but heat resistance, oil resistance performance of the main rubber glue kind to rubber
It influences maximum.Ethylene propylene diene rubber is also referred to as EPDM, is a kind of important rubber, the wherein content of ethylene unit and propylene units
Performance for EPDM is highly important.
In the prior art, EPDM analyze and mainly use pyrolysis method and membrane process, there is dissolving to make again in membrane process
Embrane method and cracking film method, rubber is due to highly cross-linked, it is difficult to dissolve and melting, preparation method are more complicated.Infrared light
The method of spectrum analysis most convenient is cracking sample preparation method.But in experiment, the organic additive in sample can interfere glue kind to analyze, one
As with acetone or chloroform-acetone extraction major part organic additive crack sample preparation again, this process takes longer.Therefore, how quickly
Accurately and conveniently EPDM is analyzed, still belongs to blank at present.
Invention content
In order to solve prior art problem, the present invention provides a kind of analysis method of EPDM, includes the following steps：By EPDM
Sided corona treatment is carried out, adds in alkane, microwave heating is pyrolyzed, with infrared analysis pyrogen.
In some embodiments, the voltage of the sided corona treatment is 8000-12000V/m2。
In some embodiments, the alkane is linear paraffin and the mixture of branched paraffin.
In some embodiments, the one kind of the linear paraffin in pentane, hexane, heptane, octane.
In some embodiments, the branched paraffin is selected from 2- methybutanes, 2- methylpentanes, 2- methyl hexanes, 2-
One kind in methyl heptane.
In some embodiments, the weight ratio of the linear paraffin and branched paraffin is (2-3)：1.
In some embodiments, the time of the microwave heating is 25-45s.
In some embodiments, the power of the microwave heating is 700-800W.
In some embodiments, the infrared analysis uses pressing potassium bromide troche.
In some embodiments, the infrared analysis is analyzed according to the absorption peak of methyl on spectrogram and vinyl.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to following detailed description.
Specific embodiment
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with fields of the present invention
The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but can include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element do not pointed out, step or component.If in claim, this
Phrase will make claim be closed, it be made not include the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to the element described in the clause；Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value limits, this, which should be understood as, specifically discloses by any range limit or preferred value and any range
All ranges that any pairing of lower limit or preferred value is formed, regardless of whether the range separately discloses.For example, when open
During range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise range intention includes its end
Value and all integers and score in the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " arbitrary
It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, represents specific the present invention is not limited to this
Quantity further includes the modified part of the acceptable change without lead to related basic function close to the quantity.Phase
It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, it is approximate
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, range limits can be with
It combines and/or exchanges, these ranges include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article " one kind " before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. occurrence number) unrestriction.Therefore "one" or " one kind " should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the apparent purport of the quantity refers to singulative.
EP rubbers is one of seven big synthetic rubber kinds.EP rubbers is compared with general synthetic rubber, difference
It is, the raw rubber trade mark type that each major company in the whole world is provided is various, and the specific aim of product is very strong, more multiple using processing technology
It is miscellaneous various.
The raw rubber of EP rubbers is a kind of translucent white-amber solid.When not removing residual catalyst metal,
Light green is often presented in air.The cold flow properties of EPM are unfavorable for storing and be molded compared with EPDM high in physical aspect, easy when depositing long
Flowing occurs or is bonded to one another.The other all rubber of density ratio of EP rubbers are all small, therefore the cost of unit volume is low.
In addition to currently used ethylidene norbornene (ENB), dicyclopentadiene (DCPD) and 1,4- hexadienes (1,4-
) etc. HD as outside Third monomer, some new other olefinic monomers such as 5- vinyl -2- norbornene (VNB), 1,7- pungent two
Alkene, 7- methyl-1-6- octadienes etc. are also progressed into EP rubbers polymer.These olefin(e) compounds are as third or
Four monomers participate in the copolyreaction of ethylene and propylene, prepare such as ethylene-octene bipolymer (EOC), ethylene-propylene-VNB
The new products such as terpolymer, ethylene-propylene-ENBVNB quadripolymers, so as to assign Ethylene-propylene Elastomer new function, make second
The performance of third rubber is with more specialization, more improvement.
EP rubbers is in random arrangement because of the ethylene on molecular backbone and propylene monomer units.So as to lose polyethylene or
The regularity of polypropylene molecule structure becomes impalpable structure and noncrystalline elastic rubber.The alkadiene third of EPDM
Monomer is located on side chain.Main chain is still the straight chain type backbone structure of saturation, therefore not only maintains two as bibasic ethylene propylene rubber
The excellent performance of first EP rubbers.And it can be vulcanized with Sulfur.
For the EPDM of differing ethylene and propylene content, performance differs, it is therefore desirable to which EPDM is analyzed.
The present invention provides a kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane
Hydrocarbon, microwave heating are pyrolyzed, with infrared analysis pyrogen.
The heat-resisting and heatproof air aging performance of EP rubbers is better than other general purpose rubbers, and the Long-term service temperature of product can
Up to 120 DEG C, maximum operating temperature is 150 DEG C.Its raw rubber starts slowly to decompose during higher than 150 DEG C, its vulcanizate at 200 DEG C
Physical property decrease speed is also slow.Therefore EP rubbers remains to protect within considerable time in 180-260 DEG C of temperature range
Hold the stability of physical property.Usual EP rubbers can only short-period used or interval use at 150 DEG C or more.Use peroxide
The EP rubbers of vulcanization can then work under the conditions of more stringent.But bibasic ethylene propylene rubber belongs to softening (degradation) type aging.
And ethylene propylene diene rubber is then structuring (crosslinking) aging, EP rubbers can be hardened due to elongation reduces after heat ageing.
The electrical isolation and corona-resistance property of EP rubbers are extremely superior, and volume resistivity is up to 1016-l017Ω cm,
Breakdown voltage and dielectric constant are higher, and corona-resistant performance and resistance to electricity cracking performance are better than IIR, chlorosulfonated polyethylene, poly- second
Alkene and crosslinked polyethylene.The water absorbing properties very little of EP rubbers, electrical property changes also very little after immersion, after long-term immersion, in water
In electric property it is also very stable.
The heat-proof water and steam performance of EP rubbers are excellent, can long period of soaking in natural water area or high-temperature-hot-water, inhale
It is aqueous very poor, performance change after immersion also very little.But its resistance to superheated water performance is influenced by vulcanizing system.Using peroxide and
Efficient vulcanization system superheated water superior performance more resistance to than vulcanizate with sulfur sulfide system.When using sulfur vulcanization, the third rubber of second
The resistance to superheated water performance of glue is even good not as good as the butyl rubber of sulfur vulcanization.The resistance to steam performance of EP rubbers is than its heat resistance
Can be also superior, high pressure resistant steam performance is better than other general purpose rubbers.
EP rubbers belongs to amorphism rubber, and the tensile strength of pure glue vulcanizate is very low, and use value is little, therefore must
Filler must be added in and carry out reinforcement.Sizing material after filler reinforcement, the mechanical property and use value of vulcanizate significantly carry
Height, EPR can largely fill oils and filler (up to 200 parts), and high Mooney viscosity EPR is not only reduced into after height is filled
This, and the influence to physical property is little.But the degree that elasticity is caused to reduce is more somewhat larger than NR.
In some embodiments, the voltage of the sided corona treatment is 8000-12000V/m2。
Its principle of sided corona treatment is to make body surface in processed body surface corona discharge using high-frequency high voltage
It generates radical reaction and crosslinks polymer.Surface it is roughening and increase its wetability to polar solvent-these from
Processed surface molecular is aoxidized and polarized by shocking by electricity and penetrating into surface breakdown its molecular structure by daughter.
In some embodiments, the alkane is linear paraffin and the mixture of branched paraffin.
In some embodiments, the one kind of the linear paraffin in pentane, hexane, heptane, octane.
In some embodiments, the branched paraffin is selected from 2- methybutanes, 2- methylpentanes, 2- methyl hexanes, 2-
One kind in methyl heptane.
In some embodiments, the weight ratio of the linear paraffin and branched paraffin is (2-3)：1.
EP rubbers is mainly used for automobile component, tire, waterproof roll, electric wire, oil modifier, polyolefin modified
The fields such as agent, part of washing machine, solar thermal collector.Auto industry is the main application fields of China's EP rubbers product, main
It is used to produce automobile heat-resistor hose, automobile sealed adhesive tape, automobile rubber pad, spark plug boot, tire white sidewall
Glue, protective cover etc..EP rubbers and polypropylene modified material for manufacture vehicle steering wheel, bumper, instrument board, mud guard,
Air conduit, automobile fan, heat dissipation grid and various pipe fittings etc..In terms of waterproof roll, EP rubbers is current performance
One of most excellent coiled material compared with traditional asphalt, has that long lifespan, intensity are big, elasticity is good, waterproof is reliable, easy for construction etc.
Feature is widely used in the waterproofing work of house, bridge, tunnel, reservoir, dykes and dams etc..
In terms of electric wire, EP rubbers have it is excellent be electrically insulated, resistance to ozone, fire resisting, weather-proof, anti ageing property,
It is widely used as power cable, mine cable, the electric wire of the ship of war, X ray DC voltage cable, atomic energy apparatus electricity consumption
The heat-resisting and high pressure resistant field such as line cable.In addition, EP rubbers has higher filler and oils fillibility, conduction can be filled
Conductive or semi-conductive rubber is made in carbon black or other materials.
In some embodiments, the time of the microwave heating is 25-45s.
In some embodiments, the power of the microwave heating is 700-800W.
Microwave heating is to utilize the energy feature of microwave, the process heated to object.General heating means rely on
The environment of circumference makes the surface of object first be heated, then in a manner of the radiation of heat or by hot-air convection
Pass through the inside of heat transfer conductive object.This method efficiency is low, and heating time is long.
The maximum feature of microwave heating is that microwave generates inside heating object, and heat source comes from interior of articles, heating
Uniformly, be conducive to improve product quality, simultaneously because " inside and outside heating simultaneously " substantially reduces heating time, the efficiency of heating surface is high,
Be conducive to improve product yield.The inertia very little of microwave heating can realize the quick control of gradient of temperature, be conducive to continuous life
Place of production volume automatically controls.
The characteristic of microwave heating is mainly reflected in：Dielectric substance heating effect.Cation and neighbouring negative electricity in dielectric substance
Son is existing in pairs, these electronics closely combine, and do not work mutually, and the whole electric field strength for the external world of medium is
Zero.If it can be rearranged immediately plus very highfield, electron-positron pair to dielectric substance.If electric field is alternation and is high
Frequency, then can vibrate will be because generating heat during friction to frequently rotating for intermolecular electronics.The penetration depth of microwave.Microwave
Into in dielectric substance since dielectric substance loss absorbs microwave energy, microwave intensity will gradually weaken.Microwave energy will be by certain
Rule attenuation.The selection of microwave heating.The absorption and heating of microwave are related with loss factor.
In some embodiments, the infrared analysis uses pressing potassium bromide troche.
In some embodiments, the infrared analysis is analyzed according to the absorption peak of methyl on spectrogram and vinyl.
Vulcanization rubber is build molecule, and due to the constraint of mesh node, only swelling is insoluble in organic solvent.Vulcanize rubber
After glue is contacted with solvent, situation is similar to being compared into unvulcanised, and solvent molecule is absorbed, into the three-dimensional network of macromolecular
Among structure, and rapidly to the interstitial diffusion of rubber macromolecule, then gradually strut macromolecular tangle net but unlike, it is molten
Vulcanization net can not be disintegrated or be destroyed to agent molecule, can only lead to volume expansion or resistance to weightening at most.
Inventor has found that technical solution using the present invention allows EPDM first to carry out in the research process for completing the present invention
Sided corona treatment then by the dissolving of the linear paraffin of special ratios and branched paraffin, can be such that EPDM is fully pyrolyzed, processing side
Just it is quick, using infrared analysis using pressing potassium bromide troche, preferable result can be obtained.It has been recognised by the inventors that after sided corona treatment,
The configuration of surface of EPDM produces activation, under the action of branched paraffin, it is easier to dissociate, linear paraffin is also easier to enter body
Gap between type molecule.Under microwave heating, molecule prompt activation enables EPDM to be fully pyrolyzed.
On infrared spectrum, 2925cm-1And 2854cm-1The peak at place is the absorption of vibrations of methylene.1376cm-1Locate as first
Base absorption peak, 1459cm-1Locate the bending vibration absorption for methyl.1640cm-1And 722cm-1Locate the characteristic absorption for vinyl.
According to the intensity and peak area of these characteristic absorption peaks on infrared absorption spectra, those skilled in the art can be in EPDM
The content of ethylene and propylene carries out qualitative and quantitative analysis.
With reference to specific embodiment, the present invention is further explained.
EPDM samples are the EPDM samples containing 34% propylene and 40% ethylene.
Embodiment 1
A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, microwave heating,
It is pyrolyzed, with infrared analysis pyrogen.
The voltage of the sided corona treatment is 8000V/m2.The alkane is pentane and the mixture of 2- methybutanes.Pentane
Weight ratio with 2- methybutanes is 2.5：1.The time of the microwave heating is 25s.The power of the microwave heating is 800W.
The infrared analysis uses pressing potassium bromide troche.The infrared analysis is divided according to the absorption peak of methyl on spectrogram and vinyl
Analysis.
Obtain propylene content 32%, ethylene contents 42%.
Embodiment 2
A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, microwave heating,
It is pyrolyzed, with infrared analysis pyrogen.
The voltage of the sided corona treatment is 10000V/m2.The alkane is hexane and the mixture of 2- methylpentanes.Hexane
Weight ratio with 2- methylpentanes is 3：1.The time of the microwave heating is 30s.The power of the microwave heating is 780W.Institute
Infrared analysis is stated using pressing potassium bromide troche.The infrared analysis is analyzed according to the absorption peak of methyl on spectrogram and vinyl.
Obtain propylene content 34%, ethylene contents 40%.
Embodiment 3
A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, microwave heating,
It is pyrolyzed, with infrared analysis pyrogen.
The voltage of the sided corona treatment is 12000V/m2.The alkane is octane and the mixture of 2- methylpentanes.Octane
Weight ratio with 2- methylpentanes is 2：1.The time of the microwave heating is 30s.The power of the microwave heating is 780W.Institute
Infrared analysis is stated using pressing potassium bromide troche.The infrared analysis is analyzed according to the absorption peak of methyl on spectrogram and vinyl.
Obtain propylene content 36%, ethylene contents 38%.
Embodiment 4
A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, microwave heating,
It is pyrolyzed, with infrared analysis pyrogen.
The voltage of the sided corona treatment is 9000V/m2.The alkane is heptane and the mixture of 2- methybutanes.Heptane
Weight ratio with 2- methybutanes is 3：1.The time of the microwave heating is 45s.The power of the microwave heating is 700W.Institute
Infrared analysis is stated using pressing potassium bromide troche.The infrared analysis is analyzed according to the absorption peak of methyl on spectrogram and vinyl.
Obtain propylene content 34%, ethylene contents 38%.
Embodiment 5
A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, microwave heating,
It is pyrolyzed, with infrared analysis pyrogen.
The voltage of the sided corona treatment is 11000V/m2.The alkane is hexane and the mixture of 2- methyl hexanes.Hexane
Weight ratio with 2- methyl hexanes is 2：1.The time of the microwave heating is 25s.The power of the microwave heating is 75000W.
The infrared analysis uses pressing potassium bromide troche.The infrared analysis is divided according to the absorption peak of methyl on spectrogram and vinyl
Analysis.
Obtain propylene content 33%, ethylene contents 40%.
Comparative example 1
A kind of analysis method of EPDM, includes the following steps：EPDM is added in into alkane, microwave heating is pyrolyzed, and use is red
Outer analysis pyrogen.
The alkane is hexane and the mixture of 2- methylpentanes.The weight ratio of hexane and 2- methylpentanes is 3：1.It is described
The time of microwave heating is 30s.The power of the microwave heating is 780W.The infrared analysis uses pressing potassium bromide troche.It is described
Infrared analysis is analyzed according to the absorption peak of methyl on spectrogram and vinyl.
Obtain propylene content 20%, ethylene contents 24%.
Comparative example 2
A kind of analysis method of EPDM, includes the following steps：EPDM is subjected to sided corona treatment, adds in alkane, oil bath heating,
It is pyrolyzed, with infrared analysis pyrogen.
The voltage of the sided corona treatment is 10000V/m2.The alkane is hexane and the mixture of 2- methylpentanes.Hexane
Weight ratio with 2- methylpentanes is 3：1.The infrared analysis uses pressing potassium bromide troche.The infrared analysis is according to first on spectrogram
The absorption peak of base and vinyl is analyzed.
Obtain propylene content 25%, ethylene contents 30%.
Aforementioned example is merely illustrative, for explaining some features of the method for the invention.Appended right will
It asks and is intended to the range as wide as possible that requirement is contemplated that, and embodiments as presented herein is only according to all possible implementation
The explanation of the embodiment of the selection of the combination of example.Therefore, the purpose of applicant is that appended claim is not illustrated this hair
The exemplary selectional restriction of bright feature.Some numberical ranges used also include sub- model in the claims
It encloses, the variation in these ranges should be also construed in the conceived case by appended claim covering.
Claims (10)
1. a kind of analysis method of EPDM, which is characterized in that include the following steps：EPDM is subjected to sided corona treatment, adds in alkane,
Microwave heating is pyrolyzed, with infrared analysis pyrogen.
2. the analysis method of EPDM as described in claim 1, which is characterized in that the voltage of the sided corona treatment is 8000-
12000V/m2。
3. the analysis method of EPDM as described in claim 1, which is characterized in that the alkane is linear paraffin and branched paraffin
Mixture.
4. the analysis method of EPDM as claimed in claim 3, which is characterized in that the linear paraffin is selected from pentane, hexane, heptan
One kind in alkane, octane.
5. the analysis method of EPDM as claimed in claim 3, which is characterized in that the branched paraffin be selected from 2- methybutanes,
One kind in 2- methylpentanes, 2- methyl hexanes, 2- methyl heptanes.
6. the analysis method of EPDM as claimed in claim 3, which is characterized in that the weight of the linear paraffin and branched paraffin
Than for (2-3)：1.
7. the analysis method of EPDM as described in claim 1, which is characterized in that the time of the microwave heating is 25-45s.
8. the analysis method of EPDM as described in claim 1, which is characterized in that the power of the microwave heating is 700-
800W。
9. the analysis method of EPDM as described in claim 1, which is characterized in that the infrared analysis uses pressing potassium bromide troche.
10. the analysis method of EPDM as described in claim 1, which is characterized in that the infrared analysis is according to methyl on spectrogram
It is analyzed with the absorption peak of vinyl.
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| CN1192224A (en) * | 1995-06-30 | 1998-09-02 | 联邦科学及工业研究组织 | Improved surface treatment of polymers |
| JP2001242078A (en) * | 2000-03-01 | 2001-09-07 | Ngk Insulators Ltd | Method and device for diagnosing deterioration |
| CN1398248A (en) * | 2000-02-10 | 2003-02-19 | 南非核能源有限公司 | Treatment of fluorocarbon feedstocks |
| CN102216246A (en) * | 2008-10-01 | 2011-10-12 | 3M创新有限公司 | Process of making fluoroolefins by thermal decomposition of fluorinated materials |
| CN103278752A (en) * | 2013-04-28 | 2013-09-04 | 西安交通大学 | Device and method for corona accelerated aging of polymer insulating material |
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2017
- 2017-12-21 CN CN201711390740.0A patent/CN108129253B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1192224A (en) * | 1995-06-30 | 1998-09-02 | 联邦科学及工业研究组织 | Improved surface treatment of polymers |
| CN1398248A (en) * | 2000-02-10 | 2003-02-19 | 南非核能源有限公司 | Treatment of fluorocarbon feedstocks |
| JP2001242078A (en) * | 2000-03-01 | 2001-09-07 | Ngk Insulators Ltd | Method and device for diagnosing deterioration |
| CN102216246A (en) * | 2008-10-01 | 2011-10-12 | 3M创新有限公司 | Process of making fluoroolefins by thermal decomposition of fluorinated materials |
| CN103278752A (en) * | 2013-04-28 | 2013-09-04 | 西安交通大学 | Device and method for corona accelerated aging of polymer insulating material |
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