Preparation method of methacrylonitrile catalyst
A technology of methacrylonitrile catalyst and dispersant, which is applied in the field of preparation of methacrylonitrile catalyst, can solve the problems of easily broken carrier, affecting the long-term use effect of the catalyst, and easy clogging, and achieves overcoming easy breakage, increasing yield, The effect of high catalytic activity
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Embodiment 1
[0016] 1) In the reactor, add 100 parts by weight of macroporous polystyrene cation exchange resin, 5 parts of manganese tricarbonylcyclopentadiene, 3 parts of potassium pentamethylcyclopentadiene, 700 parts of water, 3 parts Hydroxypropyl methylcellulose, 1 part of benzoyl peroxide, reacted at 83°C for 8 hours, filtered, and dried to obtain intermediate product 1;
[0017] 2) In parts by weight, disperse 100 parts of intermediate product 1 in 15,000 parts of dichloroethane, add 2.1 parts of trimethylantimony, 2.3 parts of trimethylbismuth, 2.8 parts of diethylzinc, and 1.7 parts of n-butyllithium , 700 parts of tetramethylethylenediamine, reacted at 62°C for 4h, filtered and washed with methanol after the reaction, and intermediate product 2 was obtained.
[0018] 3) In parts by weight, add 3 parts of 1-5 dimethyl diselenide and 20 parts of toluene to 100 parts of intermediate product 2, react at 10°C for 2 hours, filter, and dry to obtain the catalyst product. Numbered M-1....
Embodiment 2
[0020] 1) In the reactor, add 100 parts by weight of macroporous polystyrene cation exchange resin, 1 part of manganese tricarbonylcyclopentadiene, 1 part of potassium pentamethylcyclopentadiene, 500 parts of water, 1 part Hydroxypropyl methylcellulose, 0.5 parts of benzoyl peroxide, reacted at 80°C for 12h, filtered, and dried to obtain intermediate product 1;
[0021] 2) By weight, disperse 100 parts of intermediate product 1 in 1000 parts of dichloroethane, add 1 part of trimethylantimony, 1 part of trimethylbismuth, 1 part of diethylzinc, 1 part of n-butyllithium , 500 parts of tetramethylethylenediamine, reacted at 50°C for 8h, filtered and washed with methanol after the reaction, and intermediate product 2 was obtained.
[0022] 3) In parts by weight, add 1 part of dimethyl diselenide and 10 parts of toluene to 100 parts of intermediate product 2, react at 0°C for 5 hours, filter, and dry to obtain the catalyst product. Numbered M-2.
Embodiment 3
[0024] 1) In the reactor, add 100 parts by weight of macroporous polystyrene cation exchange resin, 10 parts of manganese tricarbonylcyclopentadiene, 10 parts of potassium pentamethylcyclopentadiene, 1000 parts of water, 4 parts Hydroxypropyl methylcellulose, 2 parts of benzoyl peroxide, reacted at 95°C for 5 hours, filtered, and dried to obtain intermediate product 1;
[0025] 2) In parts by weight, disperse 100 parts of intermediate product 1 in 2000 parts of dichloroethane, add 5 parts of trimethyl antimony, 5 parts of trimethyl bismuth, 5 parts of diethyl zinc, and 5 parts of n-butyllithium , 1000 parts of tetramethylethylenediamine, reacted at 80°C for 2h, filtered and washed with methanol after the reaction, and intermediate product 2 was obtained.
[0026] 3) In parts by weight, add 10 parts of 5-dimethyldiselenide and 30 parts of toluene to 100 parts of intermediate product 2, react at 30°C for 1 hour, filter, and dry to obtain the catalyst product. Numbered M-3.
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