CN103709529B - A kind of RIIR/REPDM elastomer and preparation method thereof - Google Patents
A kind of RIIR/REPDM elastomer and preparation method thereof Download PDFInfo
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- CN103709529B CN103709529B CN201310611395.4A CN201310611395A CN103709529B CN 103709529 B CN103709529 B CN 103709529B CN 201310611395 A CN201310611395 A CN 201310611395A CN 103709529 B CN103709529 B CN 103709529B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
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Abstract
A kind of RIIR/REPDM elastomer and preparation method thereof, relates to a kind of isobutene-diene rubber regeneration and preparation method thereof, this waterproof material RIIR and REPDM be 100 parts by total amount, sulfur 1～2 part, accelerator 0.9～2 part, vulcanizing activator 2.5～8 parts, white carbon black 0～20 part。Both RIIR and REPDM have good process compatibility, and in RIIR, adding portion REPDM both can obtain good combination property, can improve again the machining property of RIIR。The two blend compounds can adopt identical vulcanizing system, and its rate of cure is closer to, and is easily formed co-vulcanization material。The present invention adopts RIIR, REPDM all to replace EPDM, IIR, reduce the cost of waterproof material, improve the cohesive of waterproof material and matrix, make the excellent properties such as the RIIR/REPDM waterproof material that final research prepares has resistance to ozone, weatherability, low temperature resistant, resistant to chemical media, hot air are aging。
Description
Technical field
The present invention relates to a kind of reclaimed rubber and preparation method thereof, particularly relate to a kind of RIIR/REPDM elastomer and preparation method thereof。
Background technology
Leakage of buildings is always up a big problem of puzzlement China building trade。At present, China's building leakage rate is significantly high, and main cause is that waterproof material is of low grade, of poor quality, and fake products is prevailing。Therefore, very big in the demand of China's high performance water proof material, but owing to Cost Problems is difficult to spread in building trade high performance waterproof material。In recent years along with the fast development of China's automobile industry, the yield of RIIR also strengthens therewith, and RIIR has the features such as heat-resisting, ageing-resistant, water-fast。In order to avoid wasting the rubber sources of preciousness, the application for RIIR becomes particularly important。RIIR is applied in waterproof material, and basic unit's flexible cracking suitability is strong, may be used for adopting cold construction to base material, saves the energy, reduces environmental pollution。It it is the excellent raw material of research waterproof material。
But itself processing characteristics of RIIR is poor, in mixed refining process process, easy roll banding, adds the REPDM that structural behaviour is similar with it in RIIR, and the two is with there being good process compatibility, can improve the processing characteristics of RIIR。RIIR/REPDM waterproof material have weather-proof, hot air is aging, resistance to ozone, resistant to chemical media, the excellent combination property such as water-fast, low temperature resistant, the preparation of RIIR/REPDM waterproof material, both reduced the cost of waterproof material, achieved again the utilization of reclaimed rubber。And introduction about RIIR/REPDM waterproof material this respect does not appear in the newspapers in document and patent。
Summary of the invention
It is an object of the invention to provide a kind of RIIR/REPDM elastomer and preparation method thereof, the present invention adopts RIIR, REPDM all to replace EPDM, IIR, reduce the cost of waterproof material, improve the cohesive of waterproof material and matrix, make the excellent properties such as the RIIR/REPDM waterproof material that final research prepares has resistance to ozone, weatherability, low temperature resistant, resistant to chemical media, hot air are aging。
It is an object of the invention to be achieved through the following technical solutions:
A kind of RIIR/REPDM elastomer, described elastomer is made up of the mass parts of consisting of thing: RIIR and REPDM be 100 parts by total amount, sulfur 1～2 part, accelerator 0.9～2 part, vulcanizing activator 2.5～8 parts, white carbon black 0～20 part。
A kind of RIIR/REPDM elastomers method, its preparation process of described method is:
A. first that RIIR and REPDM is thin logical for several times so as to mix homogeneously on a mill until, be then sequentially added into zinc oxide, stearic acid, mixing uniformly after add white carbon black, add accelerator after mix homogeneously, be eventually adding vulcanizing agent；Afterwards by elastomeric compound pack 10 times, mix homogeneously bottom sheet, park 24 hours stand-by；
B. will park the film back mixing bottom sheet again of 24 hours, stay with stand-by；
C. the back mixing glue in step b being put on vulcanizing press and vulcanized, temperature controls at 160 DEG C, measures t with rubber without rotor vulcameter during sulfuration10And t90, MLAnd MH；After the time of advent, take out vulcanizate, by its natural cooling, namely obtain RIIR/REPDM elastomer, be used for measuring mechanical property。
Advantages of the present invention and effect be:
1, a kind of RIIR/REPDM elastomer of the present invention, the excellent properties such as this elastomer can be used for waterproofing work aspect, and this waterproof material has resistance to ozone, weatherability, low temperature resistant, resistant to chemical media, hot air are aging。
2, a kind of RIIR/REPDM elastomers method of the present invention is simple, and this elastomer can be used as waterproof material, and this waterproof material is with low cost and improves the cohesive between waterproof material and base material。
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described。
One RIIR/REPDM elastomer of the present invention, is made up of the mass parts of consisting of thing: RIIR and REPDM be 100 parts by total amount, sulfur 1～2 part, accelerator 0.9～2 part, vulcanizing activator 2.5～8 parts, white carbon black 0～20 part。Medium super abrasion furnace black (N220), high abrasion furnace black (N330) or the fast extruding furnace black (N550) that its white carbon black can produce for Qingdao Kai Bote rubber and plastics auxiliaries company limited。Its vulcanization accelerator can be that N cyclohexyl 2 benzothiazole sulfenamide (CZ), PZ (BZ), zinc dibutyl dithiocarbamate (PZ), tetramethylthiuram disulfide (TMTD), benzothiazolyl mercaptan (M) or benzothiazole disulfide (DM) that Shijiazhuang City Mao Feng Chemical Co., Ltd. produces are used alone, or combination more than these several accelerator two kinds or both uses。Its vulcanizing activator be Shenyang three prestige prosperity Chemical Co., Ltd. produce stearic acid, Huludao Zinc Industry Co., Ltd. produce zinc oxide in combination with use。
A kind of RIIR/REPDM elastomer, its preparation process:
A. first that RIIR and REPDM is thin logical for several times so as to mix homogeneously on a mill until, be then sequentially added into zinc oxide, stearic acid, mixing uniformly after add white carbon black, add accelerator after mix homogeneously, be eventually adding vulcanizing agent；Afterwards by elastomeric compound pack 10 times, mix homogeneously bottom sheet, park 24 hours stand-by；
B. will park the film back mixing bottom sheet again of 24 hours, stay with stand-by；
C. the back mixing glue in step b being put on vulcanizing press and vulcanized, temperature controls at 160 DEG C, measures t with rubber without rotor vulcameter during sulfuration10And t90, MLAnd MH(each embodiment test result is in Table 1)；After the time of advent, take out vulcanizate, by its natural cooling, namely obtain RIIR/REPDM elastomer, be used for measuring mechanical property。
Opening rubber mixing machine used in experiment is that Huanqiu Machinery Co., Ltd., Qingdao produces, and model is XK-160；Rubber is that Taiwan high ferro Science and Technology Co., Ltd. produces without rotor vulcameter, and model is GT-M2000-A；Vulcanizing press is that Huanqiu Machinery Co., Ltd., Qingdao produces, and model is XLB-DQ400 × 400 × 2E；Electronic tensile test machine is that Rui Geer Instrument Ltd. of Shenzhen produces, and model is RGL-30A；Shao Er hardness is calculated as Yingkou Material Test Maching Factory and produces, and model is XHS；Sheet-punching machine is that Shanghai chemical machinery four factory produces, and model is CP-25。
Embodiment 1:
In the present embodiment, the vulcanizing system of employing is sulfur, TMTD, DM composition, and vulcanizing activator is zinc oxide with stearic acid with the use of, concrete formula: RIIR90 part, REPDM10 part, TMTD1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。
RIIR/REPDM elastomer described in the present embodiment, its preparation process:
A. first lead to thin on a mill until for RIIR and REPDM for several times so as to mix homogeneously, be subsequently adding zinc oxide, stearic acid, add accelerator after mix homogeneously, be eventually adding sulfur；Afterwards by elastomeric compound pack 10 times, mix homogeneously bottom sheet, park 24 hours stand-by；
B. will park the film back mixing bottom sheet again of 24 hours, stay with stand-by；
C. the back mixing glue in step b being put on vulcanizing press and vulcanized, temperature controls at 160 DEG C, measures t with rubber without rotor vulcameter during sulfuration10And t90, MLAnd MH(each embodiment test result is in Table 1)；After the time of advent, take out vulcanizate, by its natural cooling, namely obtain RIIR/REPDM elastomer, be used for measuring mechanical property。
RIIR/REPDM elastomer described in the present embodiment, performance test is divided into tensile property to test, and is undertaken by GB/T528 2009；Tear resistance is tested, and is undertaken by GB/T529-2008；Shao Er hardness test, is undertaken by GB/T531.1 2008。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 2:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, TMTD1.5 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 3:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, BZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 4:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, BZ1.5 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 5:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, PZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 6:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, PZ1.5 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 7:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, PZ0.5 part, TMTD1 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 8:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, PZ0.5 part, TMTD1 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 9:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, BZ0.5 part, TMTD1 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 10:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, BZ0.5 part, TMTD1 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 11:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula RIIR90 part, REPDM10 part, BZ0.3 part, PZ0.2 part, TMTD1 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 12:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, BZ0.3 part, PZ0.2 part, TMTD1 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 13:
The present embodiment and embodiment 1 are distinctive in that, change the kind of accelerator, concrete formula: RIIR90 part, REPDM10 part, BZ0.5 part, PZ0.5 part, TMTD0.5 part, M0.3 part, DM0.2 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 14:
The present embodiment and embodiment 1 are distinctive in that, the vulcanizing system that elastomeric compound part adopts is sulfur, PZ, DM composition, additionally adds N330, and sulfurationization activating agent is stearic acid and zinc oxide and uses。Concrete formula: RIIR90 part, REPDM10 part, PZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, N3305 part, sulfur 1.5 parts。
RIIR/REPDM elastomer described in the present embodiment, its preparation process:
A. first lead to thin on a mill until for RIIR and REPDM for several times so as to mix homogeneously, be subsequently adding zinc oxide, stearic acid, add accelerator after mix homogeneously, be eventually adding sulfur；Afterwards by elastomeric compound pack 10 times, mix homogeneously bottom sheet, park 24 hours stand-by；
B. will park the film back mixing bottom sheet again of 24 hours, stay with stand-by；
C. the back mixing glue in step b being put on vulcanizing press and vulcanized, temperature controls at 160 DEG C, measures t with rubber without rotor vulcameter during sulfuration10And t90, MLAnd MH(each embodiment test result is in Table 1)；After the time of advent, take out vulcanizate, by its natural cooling, namely obtain RIIR/REPDM elastomer, be used for measuring mechanical property。
RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 15:
The present embodiment and embodiment 14 are distinctive in that, only change the quality of N330。Concrete formula: RIIR90 part, REPDM10 part, PZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, N33010 part, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 16:
The present embodiment and embodiment 14 are distinctive in that, only change the quality of N330。Concrete formula: RIIR90 part, REPDM10 part, PZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, N33015 part, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 17:
The present embodiment and embodiment 14 are distinctive in that, only change the quality of N330。Concrete formula: RIIR90 part, REPDM10 part, PZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, N33020 part, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 18:
The present embodiment and embodiment 1 are distinctive in that, change RIIR and REPDM mass parts ratio, and the vulcanizing system of employing is sulfur, TMTD, M composition, and sulfurationization activating agent is stearic acid and zinc oxide and uses。Concrete formula: RIIR80 part, REPDM20 part, TMTD1.5 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 19:
The present embodiment and embodiment 18 are distinctive in that, only change RIIR and REPDM mass parts ratio。Concrete formula: RIIR70 part, REPDM30 part, TMTD1.5 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
Embodiment 20:
The present embodiment and embodiment 18 are distinctive in that, only change RIIR and REPDM mass parts ratio。Concrete formula: RIIR60 part, REPDM40 part, TMTD1.5 part, M0.5 part, zinc oxide 5 parts, stearic acid 3 parts, sulfur 1.5 parts。RIIR/REPDM elastomer described in the present embodiment, its mechanical experimental results is shown in Table 2。
The each embodiment cure data of table 1
| Test event | MH/(dN·m) | ML/(dN·m) | t10/min | t90/min |
| Embodiment 1 | 3 | 0 | 4:31 | 22:26 |
| Embodiment 2 | 2 | 0 | 3: 39 | 21:59 |
| Embodiment 3 | 2 | 0 | 3:22 | 32:51 |
| Embodiment 4 | 2 | 0 | 2:12 | 29:59 |
| Embodiment 5 | 3 | 0 | 2:33 | 32:38 |
| Embodiment 6 | 3 | 0 | 1:55 | 31:30 |
| Embodiment 7 | 3 | 0 | 3:31 | 26:38 |
| Embodiment 8 | 2 | 0 | 3:09 | 26:59 |
| Embodiment 9 | 3 | 0 | 3:30 | 22:38 |
| Embodiment 10 | 2 | 0 | 3:24 | 23:01 |
| Embodiment 11 | 2 | 0 | 1:55 | 15:46 |
| Embodiment 12 | 2 | 0 | 2:34 | 22:42 |
| Embodiment 13 | 3 | 0 | 3:16 | 26:21 |
| Embodiment 14 | 3 | 0 | 2:18 | 11;45 |
| Embodiment 15 | 4 | 1 | 2:09 | 10:10 |
| Embodiment 16 | 5 | 1 | 1:54 | 9:12 |
| Embodiment 17 | 5 | 1 | 1:32 | 8:21 |
| Embodiment 18 | 2 | 0 | 315 | 15:47 |
| Embodiment 19 | 2 | 0 | 0:41 | 10:43 |
| Embodiment 20 | 3 | 0 | 2:38 | 15:35 |
The each embodiment mechanical property of table 2
| Test event | Tensile strength/MPa | Elongation at break/% | Tearing strength/KN/m | Hardness/degree |
| Embodiment 1 | 4.4 | 537 | 24 | 61 |
| Embodiment 2 | 5.0 | 575 | 24 | 60 |
| Embodiment 3 | 4.6 | 511 | 21 | 55 |
| Embodiment 4 | 4.4 | 583 | 23 | 53 |
| Embodiment 5 | 6.5 | 578 | 26 | 63 |
| Embodiment 6 | 5.8 | 493 | 25 | 62 |
| Embodiment 7 | 5.0 | 527 | 24 | 63 |
| Embodiment 8 | 4.5 | 508 | 25 | 60 |
| Embodiment 9 | 4.4 | 532 | 24 | 62 |
| Embodiment 10 | 4.8 | 540 | 26 | 61 |
| Embodiment 11 | 5.5 | 511 | 25 | 67 |
| Embodiment 12 | 4.7 | 513 | 25 | 60 |
| Embodiment 13 | 5.1 | 520 | 26 | 60 |
| Embodiment 14 | 8.1 | 359 | 20 | 61 |
| Embodiment 15 | 8.5 | 338 | 22 | 62 |
| Embodiment 16 | 8.7 | 366 | 21 | 64 |
| Embodiment 17 | 8.8 | 325 | 23 | 65 |
| Embodiment 18 | 4.9 | 412 | 28 | 64 |
| Embodiment 19 | 6.8 | 420 | 27 | 63 |
| Embodiment 20 | 6.6 | 387 | 28 | 62 |
Claims (1)
1. a RIIR/REPDM elastomer, it is characterised in that described elastomer is made up of the mass parts of consisting of thing: RIIR90 part, REPDM10 part, PZ1.5 part, DM0.5 part, zinc oxide 5 parts, stearic acid 3 parts, N33020 part, 1.5 parts of sulfur。
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| Title |
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| IIR/EPDM 共混硫化胶拉伸断裂行为的研究;何顺雄等;《特种橡胶制品》;20050630;第26卷(第3期);1-5 * |
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