CN108129253B - EPDM analysis method - Google Patents
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- CN108129253B CN108129253B CN201711390740.0A CN201711390740A CN108129253B CN 108129253 B CN108129253 B CN 108129253B CN 201711390740 A CN201711390740 A CN 201711390740A CN 108129253 B CN108129253 B CN 108129253B
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- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 49
- 238000004458 analytical method Methods 0.000 title claims abstract description 43
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 43
- CVSVTCORWBXHQV-UHFFFAOYSA-N creatine Chemical compound NC(=[NH2+])N(C)CC([O-])=O CVSVTCORWBXHQV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 35
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 33
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 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 18
- 238000000034 method Methods 0.000 claims description 17
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 14
- 238000003851 corona treatment Methods 0.000 claims description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 11
- GXDHCNNESPLIKD-UHFFFAOYSA-N 2-methylhexane Chemical compound CCCCC(C)C GXDHCNNESPLIKD-UHFFFAOYSA-N 0.000 claims description 10
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 10
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 10
- JVSWJIKNEAIKJW-UHFFFAOYSA-N 2-Methylheptane Chemical compound CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 6
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 34
- 229920001971 elastomer Polymers 0.000 description 22
- 239000005060 rubber Substances 0.000 description 22
- 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
- 239000004636 vulcanized rubber Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000008188 pellet Substances 0.000 description 7
- 229920002554 vinyl polymer Polymers 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 239000003921 oil Substances 0.000 description 5
- -1 olefin compounds Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 229920002521 macromolecule Polymers 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
- XWJBRBSPAODJER-UHFFFAOYSA-N 1,7-octadiene Chemical compound C=CCCCCC=C XWJBRBSPAODJER-UHFFFAOYSA-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
- INYHZQLKOKTDAI-UHFFFAOYSA-N 5-ethenylbicyclo[2.2.1]hept-2-ene Chemical compound C1C2C(C=C)CC1C=C2 INYHZQLKOKTDAI-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002791 soaking Methods 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
- 238000004073 vulcanization Methods 0.000 description 2
- PRBHEGAFLDMLAL-GQCTYLIASA-N (4e)-hexa-1,4-diene Chemical compound C\C=C\CC=C PRBHEGAFLDMLAL-GQCTYLIASA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 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
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001336 alkenes Chemical class 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
- 239000003795 chemical substances by application Substances 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
- 238000010924 continuous production Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction 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
- 150000001993 dienes Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920002681 hypalon Polymers 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
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 229920006029 tetra-polymer Polymers 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 238000005406 washing 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
Abstract
The invention belongs to the field of component analysis, and particularly relates to an EPDM analysis method. An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
Description
Technical Field
The invention belongs to the field of component analysis, and particularly relates to an EPDM analysis method.
Background
The rubber has the characteristics of high elasticity, good air tightness and the like, and plays an increasingly important role in the fields of aviation, transportation, industrial production and the like. The rubber product has complex components, contains various organic and inorganic components such as rubber, compounding agents, additives and the like, and various components have certain influence on the performance of the rubber product, but the main rubber species has the greatest influence on the temperature resistance and the oil resistance of the rubber product. Ethylene propylene diene monomer, also known as EPDM, is an important rubber in that the content of ethylene units and propylene units is important for the properties of EPDM.
In the prior art, the EPDM is mainly analyzed by a thermal cracking method and a film method, wherein the film method comprises a dissolving film-making method and a cracking film-making method, and a rubber product is difficult to dissolve and melt due to high crosslinking, so that the preparation method is complex. The most convenient method for infrared spectroscopy is the cracking sample preparation method. However, in the experiment, the organic auxiliary agent in the sample can interfere with the gel seed analysis, most of the organic auxiliary agent is generally extracted by acetone or chloroform-acetone and then cracked to prepare the sample, and the process is long in time consumption. Therefore, how to analyze EPDM rapidly, accurately and conveniently is still blank at present.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides an EPDM analysis method, which comprises the following steps: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
In some embodiments, the voltage of the corona treatment is 8000-2。
In some embodiments, the alkane is a mixture of a linear alkane and a branched alkane.
In some embodiments, the linear alkane is selected from one of pentane, hexane, heptane, octane.
In some embodiments, the branched alkane is selected from one of 2-methylbutane, 2-methylpentane, 2-methylhexane, 2-methylheptane.
In some embodiments, the weight ratio of linear alkane to branched alkane is (2-3): 1.
in some embodiments, the microwave heating is for a time period of 25 to 45 seconds.
In some embodiments, the microwave heating power is 700-.
In some embodiments, the infrared analysis employs potassium bromide tableting.
In some embodiments, the infrared analysis is performed according to absorption peaks of methyl and vinyl groups on a spectrum.
The above-described and other features, aspects, and advantages of the present application will become more apparent with reference to the following detailed description.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
Ethylene propylene rubber is one of seven kinds of synthetic rubber. Compared with common synthetic rubber, the ethylene propylene rubber has the difference that various raw rubber grades provided by various large companies all over the world are various, the product pertinence is strong, and the application and processing technology is more complex and diversified.
The raw rubber of the ethylene-propylene rubber is a semitransparent white-amber solid. When the residual catalyst metal is not removed, the catalyst is usually light green in air. EPM has a physically higher cold flow property than EPDM, is not storage and molding friendly, and tends to flow or stick to each other over time. The density of ethylene propylene rubber is lower than that of all other rubbers, so the cost per unit volume is low.
In addition to the currently used Ethylidene Norbornene (ENB), dicyclopentadiene (DCPD) and 1, 4-hexadiene (1,4-HD) as third monomers, some new olefin monomers such as 5-vinyl-2-norbornene (VNB), 1, 7-octadiene, 7-methyl-1-6-octadiene and the like are gradually introduced into ethylene-propylene rubber polymers. The olefin compounds are used as a third monomer or a fourth monomer to participate in the copolymerization reaction of ethylene and propylene to prepare new products such as ethylene-octene binary copolymer (EOC), ethylene-propylene-VNB terpolymer, ethylene-propylene-ENBVNB tetrapolymer and the like, thereby endowing the ethylene-propylene elastomer with new functions and enabling the performance of the ethylene-propylene rubber to be more specialized and more complete.
The ethylene-propylene rubber has ethylene and propylene monomer units in the main molecular chain in random arrangement. Thereby losing the regularity of the polyethylene or polypropylene molecular structure and becoming an amorphous structure and an amorphous elastic rubber. The diene third monomer of the EPDM is pendant. The main chain is still in a saturated straight chain type main chain structure like the ethylene propylene rubber, so that the excellent performance of the ethylene propylene rubber is maintained. And may be sulfurized with sulfur.
The properties are different for different ethylene and propylene contents of EPDM and analysis of EPDM is therefore required.
The invention provides an EPDM analysis method, which comprises the following steps: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
The heat resistance and thermo-oxidative aging resistance of the ethylene propylene rubber are superior to those of other general rubbers, and the long-term working temperature of the product can reach 120 ℃, and the maximum working temperature is 150 ℃. When the temperature is higher than 150 ℃, the crude rubber begins to be slowly decomposed, and the physical property of the vulcanized rubber is slowly reduced at 200 ℃. Therefore, the ethylene propylene rubber can still keep the stability of physical properties for a long time within the temperature range of 180-260 ℃. Ethylene-propylene rubber is generally used only for a short time or intermittently at temperatures above 150 ℃. Ethylene-propylene rubber vulcanized by peroxide can work under more severe conditions. However, ethylene propylene rubber is subject to softening (degradation) type aging. Ethylene propylene diene monomer is subjected to structured (cross-linked) aging, and ethylene propylene rubber becomes hard due to the reduction of elongation after thermal aging.
The ethylene propylene rubber has extremely excellent electrical insulation and corona resistance, and the volume resistivity of the ethylene propylene rubber is as high as 1016-l017Omega cm, high breakdown voltage and dielectric constant, and better corona discharge resistance and electric crack resistance than IIR, chlorosulfonated polyethylene, polyethylene and crosslinked polyethylene. The ethylene propylene rubber has small water absorption performance, small electrical property change after soaking, and stable electrical property in water after long-term soaking.
The ethylene propylene rubber has excellent heat-resistant water and steam resistance, can be soaked in natural water areas or high-temperature hot water for a long time, has poor water absorption, and has small performance change after being soaked. But its resistance to superheated water is affected by the vulcanization system. The superheated water resistance of the vulcanized rubber adopting the peroxide and the effective vulcanization system is superior to that of the vulcanized rubber adopting a sulfur vulcanization system. When sulfur vulcanization is used, the resistance to hot water of ethylene-propylene rubber is even less good than that of sulfur-vulcanized butyl rubber. The ethylene propylene rubber has steam resistance superior to heat resistance, and high pressure steam resistance superior to other general purpose rubbers.
The ethylene propylene rubber belongs to non-crystalline rubber, and the pure vulcanized rubber has low tensile strength and low use value, so that the ethylene propylene rubber needs to be reinforced by adding a filler. The mechanical property and the use value of the vulcanized rubber of the rubber compound after filling and reinforcing are greatly improved, the EPR can be filled with a large amount of oil and filler (up to 200 parts), and the high-Mooney-viscosity EPR is filled highly, so that the cost is reduced, and the influence on the physical property is small. But the degree of reduction in elasticity is slightly greater than NR.
In some embodiments, the voltage of the corona treatment is 8000-2。
The principle of corona treatment is that corona discharge is carried out on the surface of an object to be treated by using high frequency and high voltage, so that free radical reaction is generated on the surface of the object, and the polymer is crosslinked. The surface becomes rough and increases its wettability to polar solvents-these plasmons break down their molecular structure by electric shock and penetration into the surface, thereby oxidizing and polarizing the surface molecules being treated.
In some embodiments, the alkane is a mixture of a linear alkane and a branched alkane.
In some embodiments, the linear alkane is selected from one of pentane, hexane, heptane, octane.
In some embodiments, the branched alkane is selected from one of 2-methylbutane, 2-methylpentane, 2-methylhexane, 2-methylheptane.
In some embodiments, the weight ratio of linear alkane to branched alkane is (2-3): 1.
the ethylene propylene rubber is mainly used in the fields of automobile parts, tires, waterproof coiled materials, wires and cables, oil modifiers, polyolefin modifiers, washing machine parts, solar heat collectors and the like. The automobile industry is the main application field of ethylene propylene rubber products in China, and is mainly used for producing heat-resistant device hoses for automobiles, automobile sealing rubber strips, automobile rubber pads, spark plug sheaths, white tire sidewall rubber of tires, protective covers and the like. The modified ethylene propylene rubber and polypropylene material is used in making steering wheel, bumper, instrument panel, mudguard, air duct, automobile fan, heat dissipating grille, various pipe fittings, etc. In the aspect of waterproof coiled materials, ethylene propylene rubber is one of the coiled materials with the most excellent service performance at present, and compared with the traditional asphalt, the ethylene propylene rubber has the characteristics of long service life, high strength, good elasticity, reliable waterproof performance, convenient construction and the like, and is widely applied to waterproof engineering of houses, bridges, tunnels, reservoirs, dams and the like.
In the aspect of wires and cables, the ethylene propylene rubber has excellent electrical insulation, ozone resistance, fire resistance, weather resistance and anti-aging performance, and can be widely used in the heat-resistant and high-voltage-resistant fields of power cables, mining cables, wires and cables of military naval vessels, X-ray direct-current voltage cables, wires and cables for atomic energy devices and the like. In addition, the ethylene propylene rubber has higher filling property of fillers and oils, and can be filled with conductive carbon black or other materials to prepare conductive or semiconductive rubber.
In some embodiments, the microwave heating is for a time period of 25 to 45 seconds.
In some embodiments, the microwave heating power is 700-.
Microwave heating is a process of heating an object by using the energy characteristics of microwaves. A general heating method is to heat the surface of an object by heating the surrounding environment, radiating heat or by convection of hot air, and then conducting the inside of the object by heat conduction. This method is inefficient and requires long heating times.
The microwave heating has the biggest characteristic that the microwave is generated inside a heated object, a heat source comes from the inside of the object, the heating is uniform, the product quality is improved, meanwhile, the heating time is greatly shortened due to the 'simultaneous heating inside and outside', the heating efficiency is high, and the product yield is improved. The inertia of microwave heating is very small, the rapid control of temperature rise and fall can be realized, and the automatic control of continuous production land is facilitated.
The characteristics of microwave heating are mainly represented as follows: dielectric heating effect. The positive ions and the nearby negative electrons in the dielectric are present in pairs, and these electrons are tightly combined and do not act on each other, and the electric field strength of the whole dielectric to the outside is zero. If a very strong electric field is applied to the dielectric, the positive and negative electron pairs immediately rearrange. If the electric field is alternating and high frequency, the frequent rotation of the pairs of electrons between the molecules will vibrate and heat will be generated by friction. Penetration depth of the microwaves. Microwave energy is absorbed by the dielectric losses as the microwaves enter the dielectric, and the microwave intensity will gradually decrease. The microwave energy will decay according to a certain law. And (4) selecting a microwave heating mode. Both microwave absorption and heating are related to the loss factor.
In some embodiments, the infrared analysis employs potassium bromide tableting.
In some embodiments, the infrared analysis is performed according to absorption peaks of methyl and vinyl groups on a spectrum.
Vulcanized rubber is a molecular type, and only swells and does not dissolve in an organic solvent due to the constraint of grid nodes. After the vulcanized rubber is contacted with the solvent, the situation is similar to that of the vulcanized rubber entering non-vulcanized state, solvent molecules are absorbed, enter a three-dimensional network structure of macromolecules, rapidly diffuse to gaps among the rubber macromolecules, and gradually open a macromolecule entanglement net.
The inventor finds that through the technical scheme of the invention, the EPDM is subjected to corona treatment, and then the EPDM can be fully pyrolyzed through dissolving straight-chain alkane and branched-chain alkane in a specific ratio, the treatment is convenient and quick, and a better result can be obtained by using potassium bromide tabletting through infrared analysis. The inventors considered that the surface morphology of EPDM was activated by the corona treatment, and that the EPDM was more easily dissociated by the action of the branched alkane, and that the linear alkane was more easily taken into the gap between the molecules of the bodily form. Under microwave heating, the molecules are rapidly activated, enabling sufficient pyrolysis of the EPDM.
On the infrared spectrum, 2925cm-1And 2854cm-1The peak at (a) is the vibration absorption of the methylene group. 1376cm-1Is at 1459cm of methyl absorption peak-1Bending vibration absorption of the methyl group. 1640cm-1And 722cm-1Characteristic absorption of the vinyl group. From the intensities of these characteristic absorption peaks and the peak areas on the ir absorption spectra, one skilled in the art can perform qualitative and quantitative analysis of the ethylene and propylene content in EPDM.
The invention is further illustrated by the following specific examples.
The EPDM sample was an EPDM sample containing 34% propylene and 40% ethylene.
Example 1
An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
The voltage of the corona treatment is 8000V/m2. The alkane is a mixture of pentane and 2-methylbutane. The weight ratio of pentane to 2-methylbutane was 2.5: 1. the microwave heating time is 25 s. The power of the microwave heating is 800W. The infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 32% and the ethylene content was 42%.
Example 2
An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
The voltage of the corona treatment is 10000V/m2. The alkane is a mixture of hexane and 2-methylpentane. The weight ratio of hexane to 2-methylpentane was 3: 1. the microwave heating time is 30 s. The power of the microwave heating is 780W. The infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 34% and the ethylene content was 40%.
Example 3
An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
The voltage of the corona treatment is 12000V/m2. The alkane is a mixture of octane and 2-methylpentane. The weight ratio of octane to 2-methylpentane is 2: 1. the microwave heating time is 30 s. The power of the microwave heating is 780W. The infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 36% and the ethylene content was 38%.
Example 4
An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
The voltage of the corona treatment is 9000V/m2. The alkane is a mixture of heptane and 2-methylbutane. The weight ratio of heptane to 2-methylbutane was 3: 1. the microwave heating time is 45 s. The power of the microwave heating is 700W. The infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 34% and the ethylene content was 38%.
Example 5
An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, microwave heated, pyrolyzed, and the pyrolysate was analyzed with infrared.
The voltage of the corona treatment is 11000V/m2. The alkane is a mixture of hexane and 2-methylhexane. The weight ratio of hexane to 2-methylhexane is 2: 1. the microwave heating time is 25 s. The power of the microwave heating is 75000W. The infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 33% and the ethylene content 40% were obtained.
Comparative example 1
An analytical method for EPDM comprising the steps of: EPDM was added to the alkane, heated by microwave, pyrolyzed, and the pyrolysate was analyzed by infrared.
The alkane is a mixture of hexane and 2-methylpentane. The weight ratio of hexane to 2-methylpentane was 3: 1. the microwave heating time is 30 s. The power of the microwave heating is 780W. The infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 20% and the ethylene content 24%.
Comparative example 2
An analytical method for EPDM comprising the steps of: EPDM was corona treated, alkane was added, heated in an oil bath, pyrolyzed, and the pyrolysates were analyzed by infrared.
The voltage of the corona treatment is 10000V/m2. The alkane is a mixture of hexane and 2-methylpentane. The weight ratio of hexane to 2-methylpentane was 3: 1. the infrared analysis was performed using potassium bromide pellets. The infrared analysis is carried out according to absorption peaks of methyl and vinyl on a spectrogram.
The propylene content was 25% and the ethylene content 30%.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (6)
1. An analytical method for EPDM, comprising the steps of: performing corona treatment on EPDM, adding alkane, performing microwave heating, performing pyrolysis, and analyzing a pyrolysate by infrared;
the alkane is a mixture of straight-chain alkane and branched-chain alkane; the weight ratio of the straight-chain alkane to the branched-chain alkane is (2-3): 1;
the straight-chain alkane is selected from one of pentane, hexane, heptane and octane;
the branched alkane is selected from one of 2-methylbutane, 2-methylpentane, 2-methylhexane and 2-methylheptane.
2. The EPDM method of claim 1 wherein the voltage of the corona treatment is 8000-2。
3. The analytical method for EPDM of claim 1 wherein the microwave heating time is from 25 to 45 seconds.
4. The EPDM analytical method of claim 1 wherein the microwave heating power is 700-800W.
5. The method of analyzing EPDM of claim 1 wherein said infrared analysis uses potassium bromide sheeting.
6. The analytical method for EPDM of claim 1, wherein the infrared analysis is performed based on absorption peaks of methyl group and vinyl group on the spectrum.
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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 | Corona aging acceleration device and method for polymer insulating material |
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| 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 | Corona aging acceleration device and method for polymer insulating material |
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