A kind of hydrogenation method of nitrile latex
A technology for nitrile rubber and hydrogenation reaction is applied in the field of hydrogenation of nitrile latex, which can solve the problems that the hydrogenation degree of the hydrogenation product needs to be improved, the reaction activity of the hydrogenation catalyst is low, and the gel content of the product is high, and the reaction is shortened. Time, short response time, simple operation effect
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[0040] The following examples will further illustrate the present invention, but do not limit the present invention.
[0041] In the following examples and comparative examples, the method for determining the degree of hydrogenation is tested according to the method in the literature (Nuclear Magnetic Analysis Method for Hydrogenated Nitrile Rubber Microstructure and Degree of Hydrogenation. Petrochemical Industry, 2014, 43, 403).
[0042] Gel content determination method: Weigh w1 gram of dry glue, add chlorobenzene to make a solution of 1g / 100mL, dissolve for 24 hours, pour the solution into a filter with constant weight (w2g) and filter, then add The filter with insoluble matter is dried to constant weight, and the weight is recorded as w3 grams, then the gel content is: (w3-w2) / w1*10 6 ppm.
[0043] Hydrogenation catalyst (PPh 3 ) 3 RhCl was purchased from Acros Company and was designated as C1.
[0044] RhCl 3 .H 2 O, RuCl 3 .H 2 O were purchased from Kunming Polar Metal Material...
preparation example 1
[0047] This preparation example is used to illustrate the hydrogenation catalyst M 1 a M 2 b X m L n (C2) The preparation method, wherein M 1 For rhodium, M 2 Is ruthenium, X is chlorine, L is triphenylphosphine, and a:b:m:n is 2:1:4:9.
[0048] Put 4.5 grams of PPh 3 Dissolve in 70℃ hot ethanol solution under argon protection, 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 is dissolved in ethanol solution under the protection of argon, heated to reflux at 78℃, and the RhCl 3 .H 2 O and RuCl 3 .H 2 The ethanol solution of O was added dropwise to the reaction flask to react for 2.5 hours, the temperature was lowered to 25°C, filtered with suction, and washed with ether to obtain a powdered hydrogenation catalyst of Rh:Ru=2:1, denoted as C2.
preparation example 2
[0050] This preparation example is used to illustrate the hydrogenation catalyst M 1 a M 2 b X m L n (C3) The preparation method, wherein M 1 For rhodium, M 2 Is ruthenium, X is chlorine, L is triphenylphosphine, and a:b:m:n is 3:1:5:12.
[0051] Put 6 grams of PPh 3 Dissolve in 70℃ hot ethanol solution under argon protection, and add the dissolved solution to the reaction flask; weigh 0.75 g of RhCl 3 .H 2 O and 0.23 g RuCl 3 .H 2 O is dissolved in ethanol solution under the protection of argon, heated to reflux at 78℃, and the RhCl 3 .H 2 O and RuCl 3 .H 2 The ethanol solution of O was added dropwise to the reaction flask to react for 2.5 hours, the temperature was lowered to 25°C, filtered with suction, and washed with ether to obtain a powdered hydrogenation catalyst of Rh:Ru=3:1, denoted as C3.
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