Chelating resin, pretreatment method, noble metal removal method, and method of removing noble metal catalyst from unsaturated copolymer hydrogenation liquid
A technology of chelating resin and pretreatment liquid, applied in the field of unsaturated copolymer hydrogenation, can solve the problems of secondary pollution of products, long time required to remove precious metal catalyst, etc., and achieve the effect of reducing removal time
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preparation example 1-1
[0107] This preparation example is used to illustrate the hydrogenation catalyst M p X m L n (P1) The preparation method, wherein M is rhodium, X is chlorine, L is triphenylphosphine, p is 1, m is 1, and n is 3.
[0108] Put 4.5 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 is dissolved in ethanol solution under the protection of argon, heated to reflux at 78℃, and the RhCl 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.
preparation example 1-2
[0110] This preparation example is used to illustrate the hydrogenation catalyst M 1 a M 2 b X c L d (P2) The preparation method, wherein M 1 For rhodium, M 2 Is ruthenium, X is chlorine, L is triphenylphosphine, a:b:c:d=2:1:4:9.
[0111] Put 4.5 grams of PPh 3 Dissolve in 70℃ hot ethanol solution under the protection of argon, and add the dissolved solution to 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 catalyst for hydrogenation with Rh:Ru=2:1.
[0112] The physical parameters of the chelating resin styrene-divinylbenzene copolymer used in Examples 1-21 are shown in Table 1.
[0113] Table 1
[0114]
[0115]
[0116] The hydrogenated bu...
Embodiment 1-19
[0127] (1) Soak the chelating resin styrene-divinylbenzene copolymer in the pretreatment liquid I at a'℃ for b'hours, and then filter to obtain the chelate treated by the pretreatment liquid I Resin, and then soak the obtained chelating resin in pretreatment liquid II, soaking at i'℃ for c'hours, and filter to obtain the pretreated chelating resin, wherein, pretreatment liquid I, pretreatment liquid The volume ratio of II to the chelating resin styrene-divinylbenzene copolymer is d', and the specific surface area of the chelating resin after pretreatment was measured. The results are shown in Table 4;
[0128] (2) In the catalyst removal unit, the pretreated chelating resin is arranged in a packed tower, and the hydrogenated butadiene-acrylonitrile copolymer solution A prepared above is adjusted to f'g / at e'℃. The flow rate of min passes through the packed tower to remove the precious metal catalyst. The volume ratio of the hydrogenated butadiene-acrylonitrile copolymer solutio...
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