Chelating resin, pretreatment method, precious metal removal method, and precious metal catalyst removal method in unsaturated copolymer hydrogenation liquid
A technology of precious metal catalysts and chelating resins, which is applied in the pretreatment field of removing precious metal catalysts and chelating resins, can solve the problems of secondary pollution of products, long time required for removing precious metal catalysts, etc., and achieve short removal time Effect
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preparation example 1-1
[0099] This preparation example is used to illustrate hydrogenation catalyst M p x m L n The production method of (P1), wherein M is rhodium, X is chlorine, L is triphenylphosphine, p is 1, m is 1, and n is 3.
[0100] 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 0.75 g of RhCl 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 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 powder catalyst for hydrogenation.
preparation example 1-2
[0102] This preparation example is used to illustrate hydrogenation catalyst M 1 a m 2 b x c L d (P2) 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.
[0103] 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, and washed with ether to obtain a powdered Rh:Ru=2:1 catalyst for hydrogenation.
[0104] The physical parameters of the chelating resin styrene-divinylbenzene copolymer that adopts among the embodiment 1-15 are shown in Table 1.
[0105] Table 1
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[0108] The hydroge...
Embodiment
[0119] (1) Soak the chelating resin styrene-divinylbenzene copolymer in the pretreatment liquid at a'°C, the soaking time continues b'hour, then filter to obtain the pretreated chelating resin, wherein the pretreatment Liquid and the volume ratio of chelating resin styrene-divinylbenzene copolymer are c ', measure the specific surface area of chelating resin after pretreatment, the results are shown in Table 4;
[0120] (2) In the catalyst removal unit, the pretreated chelating resin B is arranged in the packed tower, and at e'°C, the above-mentioned hydrogenated butadiene-acrylonitrile copolymer solution A prepared by f'g The flow rate of / min passes through the packed tower to remove the precious metal catalyst, wherein the volume ratio of the hydrogenated butadiene-acrylonitrile copolymer solution to the chelating resin is g', and after h' hours, a small amount of hydrogenated butadiene that has been removed is taken For the diene-acrylonitrile copolymer solution, the con...
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