A kind of hydrogenation method of ternary nitrile latex
A technology of ternary nitrile and nitrile rubber, which is applied in the field of hydrogenation of ternary nitrile latex, can solve the problems of the degree of hydrogenation of hydrogenation products to be improved, the reactivity of hydrogenation catalysts, and the high gel content of products. Effects of shortened reaction time, short reaction time, and easy operation
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[0041] The following examples will further illustrate the present invention, but do not limit the present invention thereby.
[0042] In the following examples and comparative examples, the method for determining the degree of hydrogenation is the bromine-iodide method (for details, refer to the bromine-iodide method for determining the degree of hydrogenation of hydrogenated nitrile rubber. Journal of Beijing University of Chemical Technology, 2002, 29(3), 46-48).
[0043] In the following examples and comparative examples, the molecular weight and molecular weight distribution are measured by a gel permeation chromatograph of HLC-8320 commercially available from TOSOH, with THF as the mobile phase and narrow distribution polystyrene as the standard sample at a temperature of 40°C.
[0044] Determination method of gel content: Weigh w1 gram of dry glue, add chlorobenzene to make a solution of 1g / 100mL, after dissolving for 24 hours, pour the solution into a filter screen with...
preparation example 1
[0048] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x m L n The preparation method of (C2), wherein, M 1 for rhodium, M 2 is ruthenium, X is chlorine, L is triphenylphosphine, a:b:m:n is 2:1:4:9.
[0049] 4.5 g PPh 3 Dissolve in hot ethanol solution at 70°C under the protection of argon, and add the dissolved solution into the reaction flask; weigh 0.5 g of RhCl 3 .H 2 O and 0.23 g RuCl 3 .H 2 O was dissolved in ethanol solution under the protection of argon, heated to reflux at 78°C, and RhCl 3 .H 2 O and RuCl 3 .H 2 The ethanol solution of O was added dropwise into the reaction flask to react for 2.5 hours, cooled to 25°C, filtered with suction, washed with ether to obtain a powdered hydrogenation catalyst with Rh:Ru=2:1, denoted as C2.
preparation example 2
[0051] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x m L n The preparation method of (C3), wherein, M 1 for rhodium, M 2 is ruthenium, X is chlorine, L is triphenylphosphine, a:b:m:n is 3:1:5:12.
[0052] 6 g PPh 3 Dissolve in hot ethanol solution at 70°C under the protection of argon, and add the dissolved solution into the reaction flask; weigh 0.75 g of RhCl 3 .H 2 O and 0.23 g RuCl 3 .H 2 O was dissolved in ethanol solution under the protection of argon, heated to reflux at 78°C, and RhCl 3 .H 2 O and RuCl 3 .H 2 The ethanol solution of O was added dropwise into the reaction flask to react for 2.5 hours, cooled to 25°C, filtered with suction, and washed with ether to obtain a powdered hydrogenation catalyst with Rh:Ru=3:1, denoted as C3.
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