A kind of method for efficiently synthesizing the sulfonic acid resin catalyst of synthesizing polyoxymethylene dimethyl ether
A polymethoxydimethyl ether and sulfonic acid resin technology, which is applied in the directions of organic compound/hydride/coordination complex catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the difficulty of liquid acid catalysts and products Separation, can not be recycled, reduce yield and other issues
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Embodiment 1
[0027] Put 3 grams of NKC-9 sulfonic acid tree catalyst into 100 mL containing insoluble alcohol solvent (methanol, ethanol, propanol, ethylene glycol, 1,3-propanediol, 2-propanol, n-butanol, n-pentanol , Isoamyl alcohol, n-hexanol, cyclohexanol, benzyl alcohol, etc.) in the reaction kettle, treat the sulfonic acid resin catalyst in the temperature range of 70-140 ℃ for 1-8h. 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: 60 mL of DMM, 20 g of paraformaldehyde, and 3 g of the modified sulfonic acid resin catalyst were weighed and added to the reaction kettle respectively. 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 lower than 0.1%. Into 2.0 MPa of N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in th...
Embodiment 2
[0032] The polystyrene sulfonic acid resin catalyst (D-009B, DA-330, D-006, D-072, Amberlyst-15, NKC-9) of 3g different models is packed in the reactor containing benzyl alcohol solvent of 100mL, in 100-150 ℃, 5.0 MPa, CO atmosphere for 1 h. The treated catalyst was filtered and dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: 60 mL of DMM, 20 g of paraformaldehyde, and 3 g of the modified sulfonic acid resin catalyst were weighed and added to the reaction kettle respectively. 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 lower than 0.1%. N passing through 2.0 MPa 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Pass again 2.0 MPaN 2 , the stirring speed of the reactor was 500 rpm, the reaction temperature was controlled at 90 °C, and t...
Embodiment 3
[0037] Put 3g of NKC-9 catalyst into a 100ml reaction kettle containing benzyl alcohol solvent, and treat it at 130°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: 60 mL of DMM, 20 g of paraformaldehyde, and 3 g of the modified sulfonic acid resin catalyst were weighed and added to the reaction kettle respectively. 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 lower than 0.1%. Into 2.0 MPa of N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Pass again 2.0 MPa N 2 , the stirring speed of the reactor was 500 rpm, the reaction temperature was controlled at 90 °C, and the reaction time was 3 h.
[0038] Table 3. The effect of different catalyst tr...
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