Aminomethyl-containing hydrogenated nitrile rubber and its production method
A technology of nitrile rubber and aminomethyl, applied in the field of nitrile rubber, can solve the problems of small scorch tolerance, no knowledge, low processing safety, etc.
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[0111] Characterization method
[0112] The aminomethyl content can be determined by determining the decrease in the extinction of the nitrile band indirectly in the IR spectrum. For this purpose, 200 mg of partially or fully hydrogenated nitrile rubber are dissolved in 10 ml of chlorobenzene and the degree of mattness is determined before the hydrogenation. After the hydrogenation, exactly 200 mg of the aminomethyl-containing nitrile rubber was dissolved in 10 ml of chlorobenzene and the extinction was determined again. From the difference in extinction, it is possible to determine the conversion of the nitrile groups and thus the aminomethyl content in % by weight given the known content of bound α,β-unsaturated nitriles.
[0113] Exemplary calculation of aminomethyl content:
[0114] 200mg of 3406 was dissolved in 10 ml chlorobenzene and the extinction of the nitrile band was measured by IR spectroscopy. The extinction degree is 0.2451. 200 mg of the aminomethyl-c...
example A1
[0143] Example A1: with 50 bar H 2 Hydrogenation without special catalyst pretreatment:
[0144] 21g of 3406 was dissolved in a dry flask in a mixture made from 150 g dry THF and 150 g dry dioxane in a 500 ml flask at 60°C for 1 to 2 hours. The polymer solution and 21 g (dry mass) of the THF-wetted Raney cobalt catalyst spin-washed as above were transferred under protective gas into a dry autoclave (700 ml). For the transfer, an additional 50 g of THF was provided to completely flush the catalyst storage vial. The autoclave was closed and inertized with nitrogen. 20 g of ammonia are added and then pressurized with hydrogen up to a pressure of 50 bar. It was then heated to 130° C. and the reaction was carried out isobarically at this temperature for 24 hours. Stirring is performed here with 1200 UpM. After cooling, the autoclave was flushed with nitrogen, then opened and the reaction solution / suspension was filled into a storage vessel. The solvent / suspension is then ...
example A2
[0145] Example A2: 50 bar H with addition of n-dodecyl sulfide 2 without special catalyst pretreatment Hydrogenation of:
[0146] 21g of 3406 was dissolved in a dry flask in a mixture made from 150 g dry THF and 150 g dry dioxane in a 500 ml flask at 60°C for 1 to 2 hours. The polymer solution, 21 g (dry mass) of the Raney cobalt catalyst wetted with THF and 21 mg of n-dodecyl sulfide (0.1 wt. Transfer to a dry autoclave (700ml). For the transfer, an additional 50 g of THF was provided to completely flush the catalyst storage vial. The autoclave was closed and inertized with nitrogen. 20 g of ammonia are added and then pressurized with hydrogen up to a pressure of 50 bar. It was then heated to 130° C. and the reaction was carried out isobarically at this temperature for 24 hours. Stirring is performed here with 1200 UpM. After cooling, the autoclave was flushed with nitrogen, then opened and the reaction solution / suspension was filled into a storage vessel. The so...
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