A kind of method utilizing sulfone solvent to process polystyrene sulfonic acid resin catalyst
A technology of polystyrene sulfonic acid and catalyst, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., which can solve the difficulties in the preparation of methyl chloroacetate and sodium methoxide , Not suitable for large-scale production and other issues, to achieve the best reactivity effect
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Embodiment 1
[0035] Put 10 grams of D-006 sulfonic acid resin catalyst into 100 mL of insoluble sulfone solvent (dimethyl sulfone, methyl vinyl sulfone, sulfolene, sulfolane, diethyl sulfone, allyl sulfone, etc.) In the reactor, treat the sulfonic acid resin catalyst in the temperature range of 100-150 °C for 2-6 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: Weigh 30 mL of DMM, 30 mL of 1,4-dioxane solvent, and 1 g of the modified sulfonic acid resin catalyst, and add them to the reaction kettle respectively, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1 %, pass in 3.0 MPa CO, let it stand for 30 minutes, and use it for leak detection of the reactor to ensure that the device is airtight and then emptied Gas in the kettle. The stirring speed of the reactor was 500 rpm, 3.0 MPa CO was int...
Embodiment 2
[0040] Put 10 grams of different types of polystyrene sulfonic acid resin catalysts (D-009B, DA-330, D-006, D-072, Amberlyst-15, NKC-9) into a 100mL reaction kettle containing diethylsulfone solvent , at 100-150°C, 5.0 MPa, and CO atmosphere for 6 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: Weigh 30 mL of DMM, 30 mL of 1,4-dioxane solvent, and 1 g of the modified sulfonic acid resin catalyst, and add them to the reaction kettle respectively, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1 %, pass in 3.0 MPa CO, let it stand for 30 minutes, and use it for leak detection of the reactor to ensure that the device is airtight and then emptied Gas in the kettle. The stirring speed of the reactor was 500 rpm, 3.0 MPa CO was introduced, the reaction temperature was controlled at 11...
Embodiment 3
[0045] Put 10 grams of NKC-9 catalyst into a 100 mL reaction kettle containing diethyl sulfone solvent, and treat it at 150 °C, 5.0 MPa, and CO atmosphere for 0.5-20 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: Weigh 30 mL of DMM, 30 mL of 1,4-dioxane solvent, and 1 g of the modified sulfonic acid resin catalyst, and add them to the reaction kettle respectively, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1 %, pass in 3.0 MPa CO, let it stand for 30 minutes, and use it for leak detection of the reactor to ensure that the device is airtight and then emptied Gas in the kettle. The stirring speed of the reactor was 500 rpm, 3.0 MPa CO was introduced, the reaction temperature was controlled at 110 °C, and the reaction was carried out for 6 hours. Cool down to room temperature ...
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