CN106750491A - CM/EPDM blended rubber single-phase etching method and method for improving resolution in representing microstructure of rubber blend - Google Patents
CM/EPDM blended rubber single-phase etching method and method for improving resolution in representing microstructure of rubber blend Download PDFInfo
- Publication number
- CN106750491A CN106750491A CN201710043142.XA CN201710043142A CN106750491A CN 106750491 A CN106750491 A CN 106750491A CN 201710043142 A CN201710043142 A CN 201710043142A CN 106750491 A CN106750491 A CN 106750491A
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- China
- Prior art keywords
- epdm
- blend
- rubber
- etching
- glue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 64
- 239000005060 rubber Substances 0.000 title claims abstract description 64
- 239000000203 mixture Substances 0.000 title claims abstract description 61
- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000005530 etching Methods 0.000 title claims abstract description 37
- 239000003292 glue Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000002389 environmental scanning electron microscopy Methods 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 claims description 4
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 4
- 229960002447 thiram Drugs 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 2
- 150000004867 thiadiazoles Chemical group 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 description 5
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920006235 chlorinated polyethylene elastomer Polymers 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 229910000489 osmium tetroxide Inorganic materials 0.000 description 1
- 239000012285 osmium tetroxide Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/042—Elimination of an organic solid phase
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/046—Elimination of a polymeric phase
- C08J2201/0462—Elimination of a polymeric phase using organic solvents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
- C08J2323/28—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a CM/EPDM blended rubber single-phase etching method and a method for improving the resolution when representing the microstructure of a rubber blend, wherein a CM phase in the CM/EPDM blended rubber is vulcanized through a vulcanization system, and an EPDM phase is kept in an unvulcanized state; and etching the EPDM phase in the CM/EPDM blended glue from the blended system by using an etchant to form holes, leaving the unetched CM phase, extracting the redundant etchant from the blended glue by using a volatile solvent, and drying. One phase in the blended rubber is vulcanized to form a network structure, so that the network structure is kept stable in the etching process and is not corroded by a solvent, and an unvulcanized phase is etched to form an observable surface appearance.
Description
Technical field
Rubber blend microstructure is characterized the present invention relates to a kind of method of single-phase etching of CM/EPDM Blend rubbers and raising
When resolution ratio method.
Background technology
Characterizing two kinds of methods of rubber blend microstructure generally has ESEM, transmission electron microscope, AFM
With the mode such as phase contrast microscope, using it is most be ESEM and transmission electron microscope.Compared to ESEM, transmission electron microscope requirement
Two-phase in blend has sufficiently large contrast difference to observe, and needs to use ultra-thin section, sample preparation for solid sample
Level directly affects test result.
During decoration method is generally used when being observed micro structure using transmission electron microscope to blend one is mutually carried out
Dyeing, so as to improve title degree to improve resolution ratio, conventional coloring agent has osmium tetroxide and ruthenium tetroxide.Due to both dyeing
There are larger operational hazards when being exerted a gradual, corrupting influence on and greatly limit the use of this method in agent.
, it is necessary to be produced compared with macrorelief when material interface is broken, two during using scanning electron microscopic observation blend micro structure
Exist between phase and be clearly separated.The transmission electron microscope phase of chlorinated polyethylene rubber (CM) and ethylene propylene diene rubber (EPDM) blend
Not substantially, surface is unfavorable for the observation of ESEM to difference without substantially fluctuating after brittle failure.
The content of the invention
The present invention is intended to provide a kind of method of single-phase etching of CM/EPDM Blend rubbers and raising sign rubber blend are microcosmic
The method of resolution ratio during structure, in two phase structure is mutually etched formation cavity by the method for etching, beneficial to ESEM
Observation microstructure.
During two kinds of plastic blends, a wherein phase is etched, or rubber phase, the plastics phase not being etched are etched during rubber plastic blend
Remain to keep space structure to be easy to scanning electron microscopic observation.During two kinds of blend rubbers, after carrying out single-phase etching to uncured rubber, not by
The rubber of etching blocks the hole being etched due to still having preferable mobility.And the Blend rubber of complete cure is due to network
The formation of structure can only can not be etched by swelling.
In three kinds of conventional vulcanizing systems of chlorinated polyethylene rubber, only peroxide vulcanizing system can vulcanize EPDM.Base
In above-mentioned consideration, the present invention proposes a kind of method of the single-phase etching of CM/EPDM Blend rubbers.
The method of the single-phase etching of CM/EPDM Blend rubbers of the present invention, is mutually carried out by CM/EPDM Blend rubbers first
Vulcanization forms network structure, makes it that rock-steady structure is kept in etching process without being corroded by solvent, by unvulcanized phase etching, shape
Into observable surface topography.
The method of the single-phase etching of CM/EPDM Blend rubbers of the present invention, by using in vulcanizing system vulcanization CM/EPDM Blend rubbers
CM phases, and keep EPDM phases be in unvulcanized state；Followed by etching agent by the EPDM phases in CM/EPDM Blend rubbers from altogether
Etch away to form hole in mixed system, leave the CM phases not being etched, recycle volatile solvent by unnecessary etching agent from
Extracted in Blend rubber, after drying.
CM glue and the blending mass ratio of EPDM glue are 10 in the CM/EPDM Blend rubbers：90~90：10, blending method is
Mill is blended or banburying blending.
The vulcanizing system is Thiadiazole Curing System or thiourea curing system.
The Thiadiazole Curing System includes crosslinking agent and accelerator；
The crosslinking agent is selected from ECHOA, ECHOS, Vanax 189 or Rhenogran TDD, the addition of crosslinking agent
It is 0.5~5phr；The accelerator is selected from Vanax 808 or Rhenogran NC, and the addition of accelerator is 0.5~5phr.
The thiourea curing system is vulcanizing agent NA-22, and addition is 0.5~5phr.
At 150~190 DEG C, cure time is 3~60 minutes for curing temperature control.
The etching agent is dimethylbenzene, chloroform or gasoline etc., and quality and the CM/EPDM Blend rubber mass ratios of etching agent are
5~20：1；At 20~80 DEG C, etch period is 5~240 hours for etching temperature control.
The volatile solvent including ethanol, isopropanol or petroleum ether etc., the quality of the solvent and CM/EPDM Blend rubbers
Mass ratio be 5~20：1.
The present invention improve characterize rubber blend microstructure when resolution ratio method, be first by rubber blend according to
The above method carries out single-phase etching, and liquid nitrogen treatment recycles ESEM to see the microstructure of Blend rubber after obtaining section
Examine.
The rubber blend is CM/EPDM Blend rubbers, the blending matter of CM glue and EPDM glue in the CM/EPDM Blend rubbers
Amount is than being 10：90~90：10.
Compared with the prior art, beneficial effects of the present invention are embodied in：
The present invention can effectively change the microscopic appearance of Blend rubber using lithographic technique, so as to reflect in Blend rubber altogether
The micro structure of mixed component.Blend rubber material is effectively improved to be difficult to etch and be difficult intuitively to be observed altogether by existing means
The present situation of mixed system micro structure.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the single-phase lithographic method of CM/EPDM Blend rubbers of the present invention.
Fig. 2 is the stereoscan photograph after the single-phase etching of CM/EPDM Blend rubbers.As can be seen from Figure 2 Blend rubber surface
There is continuous hole, illustrate that solvent xylene, by the EPDM components dissolving in Blend rubber, leaves CM components.By lithographic technique,
The micro structure of CM components and EPDM components in Blend rubber can clearly be differentiated.
Fig. 3 is stereoscan photograph of the CM/EPDM Blend rubbers without etching processing.
Specific embodiment
Embodiment 1：
The method of the single-phase etching of CM/EPDM Blend rubbers is as follows in the present embodiment：
1st, CM glue and EPDM glue in mass ratio 50：50 ratio is blended, blending method mill, roll spacing 2mm, roller temperature 40
DEG C, mill time 5min；
2nd, the CM phases in CM/EPDM Blend rubbers are vulcanized by Thiadiazole Curing System, and it is unvulcanized to keep EPDM phases to be in
State；Crosslinking agent is ECHOA in Thiadiazole Curing System, and consumption 1phr, accelerator is Vanax 808, and consumption is 1phr；Sulphur
It is 170 DEG C, cure time 10 minutes to change temperature.
3rd, the EPDM phases in CM/EPDM Blend rubbers are etched away to form hole from co-mixing system using etching agent dimethylbenzene
Hole, leaves the CM phases not being etched, and recycles etoh solvent that unnecessary etching agent is extracted from Blend rubber, after drying i.e.
Can；
The quality of etching agent is 10 with CM/EPDM Blend rubbers mass ratio:1；Etching temperature is controlled in 50 DEG C, etch period
It is 48 hours；The quality of etoh solvent is 10 with the mass ratio of CM/EPDM Blend rubbers:1.
4th, liquid nitrogen treatment recycles ESEM to observe the microstructure of Blend rubber after obtaining section, as a result sees figure
2.Stereoscan photograph of the CM/EPDM Blend rubbers without etching processing is shown in Fig. 3.Contrasted from Fig. 2, Fig. 3 as can be seen that through over etching
Technology, can clearly differentiate the micro structure of CM components and EPDM components in Blend rubber.
Claims (10)
1. a kind of method of the single-phase etching of CM/EPDM Blend rubbers, it is characterised in that：Vulcanize CM/EPDM by vulcanizing system to be blended
CM phases in glue, and keep EPDM phases to be in unvulcanized state；Followed by etching agent by the EPDM phases in CM/EPDM Blend rubbers
Etch away to form hole from co-mixing system, leave the CM phases not being etched, recycle volatile solvent by unnecessary etching
Agent is extracted from Blend rubber, after drying.
2. method according to claim 1, it is characterised in that：
CM glue and the blending mass ratio of EPDM glue are 10 in the CM/EPDM Blend rubbers：90~90：10, blending method is mill
Blending or banburying blending.
3. method according to claim 1, it is characterised in that：
The vulcanizing system is Thiadiazole Curing System or thiourea curing system.
4. method according to claim 3, it is characterised in that：
The Thiadiazole Curing System includes crosslinking agent and accelerator；The crosslinking agent is selected from ECHOA, ECHOS, Vanax
189 or Rhenogran TDD, the addition of crosslinking agent is 0.5~5phr；The accelerator be selected from Vanax 808 or
Rhenogran NC, the addition of accelerator is 0.5~5phr.
5. method according to claim 3, it is characterised in that：
The thiourea curing system is vulcanizing agent NA-22, and addition is 0.5~5phr.
6. method according to claim 1, it is characterised in that：
At 150~190 DEG C, cure time is 3~60 minutes for curing temperature control.
7. method according to claim 1, it is characterised in that：
The etching agent is dimethylbenzene, chloroform or gasoline, and quality and the CM/EPDM Blend rubbers mass ratio of etching agent are 5~20：
1；At 20~80 DEG C, etch period is 5~240 hours for etching temperature control.
8. method according to claim 1, it is characterised in that：
The volatile solvent includes ethanol, isopropanol or petroleum ether, the quality of the solvent and the quality of CM/EPDM Blend rubbers
Than being 5~20：1.
9. a kind of method of resolution ratio when raising characterizes rubber blend microstructure, it is characterised in that：First by blend rubber
Thing carries out single-phase etching in accordance with the method for claim 1, and liquid nitrogen treatment recycles ESEM to blending after obtaining section
The microstructure of glue is observed；The rubber blend is CM/EPDM Blend rubbers.
10. method according to claim 9, it is characterised in that：
CM glue and the blending mass ratio of EPDM glue are 10 in the CM/EPDM Blend rubbers：90~90：10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043142.XA CN106750491B (en) | 2017-01-19 | 2017-01-19 | CM/EPDM blended rubber single-phase etching method and method for improving resolution in representing microstructure of rubber blend |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043142.XA CN106750491B (en) | 2017-01-19 | 2017-01-19 | CM/EPDM blended rubber single-phase etching method and method for improving resolution in representing microstructure of rubber blend |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106750491A true CN106750491A (en) | 2017-05-31 |
| CN106750491B CN106750491B (en) | 2019-09-10 |
Family
ID=58945123
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710043142.XA Active CN106750491B (en) | 2017-01-19 | 2017-01-19 | CM/EPDM blended rubber single-phase etching method and method for improving resolution in representing microstructure of rubber blend |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280280A (en) * | 2018-09-21 | 2019-01-29 | 佛山皖和新能源科技有限公司 | A kind of preparation method of high thermal conductivity type rubber-metal composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396639A (en) * | 2013-07-19 | 2013-11-20 | 华南理工大学 | Dynamic vulcanized fluoroplastic/fluororubber/silicone rubber thermoplastic elastomer and preparation method thereof |
| CN104530613A (en) * | 2015-01-09 | 2015-04-22 | 华南理工大学 | Rubber-phase fluorinated polysiloxane thermoplastic elastomer with core-shell structure and preparation method of rubber-phase fluorinated polysiloxane thermoplastic elastomer |
-
2017
- 2017-01-19 CN CN201710043142.XA patent/CN106750491B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396639A (en) * | 2013-07-19 | 2013-11-20 | 华南理工大学 | Dynamic vulcanized fluoroplastic/fluororubber/silicone rubber thermoplastic elastomer and preparation method thereof |
| CN104530613A (en) * | 2015-01-09 | 2015-04-22 | 华南理工大学 | Rubber-phase fluorinated polysiloxane thermoplastic elastomer with core-shell structure and preparation method of rubber-phase fluorinated polysiloxane thermoplastic elastomer |
Non-Patent Citations (1)
| Title |
|---|
| 王启丰等: ""低压橡皮电缆用CM/EPDM绝缘配方研究"", 《电线电缆》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280280A (en) * | 2018-09-21 | 2019-01-29 | 佛山皖和新能源科技有限公司 | A kind of preparation method of high thermal conductivity type rubber-metal composite material |
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