Solid heterogeneous catalyst used for preparation method using ethylene oxide, carbon dioxide and methanol to prepare dimethyl carbonate and ethylene glycol and preparation method of solid heterogeneous catalyst
A heterogeneous catalyst, the technology of dimethyl carbonate, is applied in the preparation of carbon dioxide or inorganic carbonate, the preparation of oxygenated compounds, chemical instruments and methods, etc. Problems such as poor product selectivity, to achieve the effects of high conversion rate and product selectivity, high product quality, and short reaction process
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[0034] The present invention is used for the preparation method of the solid heterogeneous catalyst of ethylene oxide, carbon dioxide and methyl alcohol preparation dimethyl carbonate and ethylene glycol, comprises the steps:
[0035] Step 1. Carrier pretreatment
[0036] The carrier material, that is, the modified resin material (chlorinated polyethylene, chlorinated polypropylene or chloromethylated polystyrene) is vacuum-dried at 20-200°C for 0.5-48h.
[0037] Step 2, active component 1 is immobilized
[0038] Mix the carrier obtained in step 1 and the active component imidazole at a mass ratio of 1.0:(0.1-0.7), react at 20-200°C for 0.5-48h, filter, wash and dry.
[0039] Step 3, active component 2 is immobilized
[0040] Mix the solid and active component 2 halogen-containing organic matter (2-bromoethanol or 1,2-dibromoethane) obtained in step 2 at a mass ratio of 1.0: (0.5-1.5), and react at 20-200°C for 0.5 -48h, the obtained solid is filtered, washed with ethyl ace...
Embodiment 1
[0044] Step 1. Carrier chloromethylated polystyrene is vacuum-dried at 80° C. for 12 hours;
[0045] Step 2. Take 10 g of the solid obtained in step 1, mix it with 3.6 g of imidazole and react at 80°C for 8 hours;
[0046] Step 3, the solid obtained in step 2 is filtered, washed with ethyl acetate, water, and methanol, and then vacuum-dried at 80°C;
[0047] Step 4, reacting 10 g of the solid obtained in step 3 and 7 g of 2-bromoethanol at 80° C. for 8 h;
[0048] Step 5. The solid obtained in Step 4 is filtered, washed with ethyl acetate and methanol, and then vacuum-dried at 80° C. to obtain a solid heterogeneous catalyst.
[0049] Put 0.5 g of the solid heterogeneous catalyst material obtained in step 5 into a 200 ml autoclave, and close the autoclave. Add 80g of ethylene oxide / methanol solution with a mixing ratio of 1:4 into the reactor, then fill it with 1MPa carbon dioxide, heat up to 170°C to start the reaction, and after 2 hours, the conversion rate of ethylene oxid...
Embodiment 2
[0051] Step 1. The carrier chlorinated polyethylene is vacuum-dried at 100° C. for 8 hours;
[0052] Step 2. Take 10g of the solid obtained in step 1, mix it with 7g of imidazole and react at 120°C for 6h;
[0053] Step 3, the solid obtained in step 2 is filtered, washed with ethyl acetate, water, and methanol, and then vacuum-dried at 80°C;
[0054] Step 4. React 10 g of the solid obtained in step 3 and 15 g of 2-bromoethanol at 120° C. for 6 h;
[0055] Step 5. The solid obtained in step 4 is filtered, washed with ethyl acetate and methanol, and then vacuum-dried at 120° C. to obtain a solid heterogeneous catalyst.
[0056] Put 0.5 g of the solid heterogeneous catalyst material obtained in step 5 into a 200 ml autoclave, and close the autoclave. Add 80g of ethylene oxide / methanol solution with a mixing ratio of 1:4 into the reactor, then fill it with 1MPa carbon dioxide, heat up to 170°C to start the reaction, and after 2 hours, the conversion rate of ethylene oxide is 100...
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