Methods of forming vulcanizable elastomeric formulations and vulcanized elastomeric articles
A technology of vulcanized elastomers and formulations, applied in the field of forming vulcanized elastomer products, which can solve the problems of slowing down manufacturing speed and reducing manufacturer's yield
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Embodiment 1
[0066] Example 1 - Preparation of (TMEDA)ZnS 6 complex
[0067] Tetramethylethylenediamine (TMEDA) (408 g) and methanol (72 g) were added to a mixture equipped with a mechanical stirrer (close to the vessel wall), thermocouple, N 2 Bubbler, water condenser, and electric heating mantle in a 3-liter three-neck glass flask. The system was purged with nitrogen and the temperature of the mixture was adjusted to 35°C. Freshly ground cyclooctasulfide (powder) was added over 5 minutes while maintaining agitation at 425-450 rpm. The temperature was increased to 45°C, at which point 40 grams of metallic zinc powder (98% purity) was added over 5 minutes while maintaining agitation at 425-450 rpm. The grey-green-yellow reactor contents were then slowly heated to 86°C and stirred for 4 hours, or until yellow. Once yellow, the mixture was kept at this temperature with stirring for an additional 2 hours. At the end of the reaction time, the flask was cooled to room temperature, the s...
Embodiment 2
[0068] Example 2 - From (TMEDA)ZnS 6 The complex prepares the cyclododecyl sulfide of the present invention (S 12 ）
[0069] Dichloromethane (750 mL) was added to a device equipped with a mechanical stirrer, thermocouple, N 2 Bubbler and stopper in a 2 L four-neck glass flask. Bromine (16.7 g, 104.5 mmol, 1.0 equiv) was weighed to contain 50 mL CH 2 Cl 2 bottle and add the mixture to the flask. The solution was cooled to 4°C. The zinc complex from Example 1, (TMEDA)ZnS was added in one portion 6 (97.5% pure) (40 g, 104.3 mmol, 1.0 equiv) and mixed with 50 mL CH 2 Cl 2 washing. There was an immediate exotherm to 11 °C. The solution was stirred for 15 min, filtered, washed with cold CH 2 Cl 2 Wash and suction dry. The solid was slurried in THF (250 mL), filtered and suction dried. Place the resulting solid in cold CS 2 (155 mL), filtered and suction dried to provide 10.2 g of a pale yellow solid (50.8% yield based on sulfur in zinc complex). Evaluation using...
Embodiment 3
[0071] Example 3 - Comparison of melting points of cyclododecylsulfide materials
[0072] Several batches of purified cyclododecylsulfide of the present invention were prepared following the procedures exemplified in Examples 1 and 2. Each final purified material is passed through Raman, Uniquat ® or ICP for analysis and the melting point onset temperature was measured using DSC as described above. The results are given in Table 1 below together with the melting point of "control" cyclododecyl sulfide by Steudel, R.; Eckert, B., "Solid Sulfur Allotropes", Topics in CurrentChemistry ( 2003) were extrapolated from data measured at DSC heating rates of 10°C / min, 5°C / min and 2.5°C / min.
[0073] Table 1
[0074] sample Melting point, °C Inventive batch 1 166.0 Inventive batch 2 156.0 Inventive batch 3 159.3 Inventive batch 4 158.6 Inventive batch 5 162.4 Inventive batch 6 164.0 Inventive batch 7 161.5 control 153.5 ...
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