Method for synthesizing polyformaldehyde dimethyl ether by taking methanol and methanal as raw materials
A polyoxymethylene dimethyl ether and methanol technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult separation, high equipment requirements, and large environmental pollution, and achieve high reaction conversion rate, The effect of good technical effect and high product yield
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[0015] Example 1
[0016] Add 2 g of catalyst SO into a 300 ml tank reactor 4 2- / Fe 2 O 3 , 100ml methanol and 300ml formaldehyde, in 130 oC Reacted with 0.8MPa autogenous pressure for 4h, and the sample was centrifuged and analyzed by gas chromatography. The product contains polyoxymethylene dimethyl ether (CH 3 O(CH 2 O) n CH 3 ) And unreacted raw materials methanol and formaldehyde, the composition distribution is as follows (expressed in weight %): methanol 3.1%; methylal 22.5%; formaldehyde 4.7%; n=2, 25.8%; n=3, 24.2%; n =4, 11.3%; n=5~10, 8.2%; n> 10. Margin.
[0017] Solid super acid SO used 4 2- / Fe 2 O 3 Catalyst preparation method:
[0018] 0.5mol / L FeCl in 200ml 3 Add 12.5% by mass of NH to the solution 3 ·H 2 O, adjust pH=9, let stand for 24h, filter and wash until no Cl - Check out. 100 o C drying and grinding. The powder is added to 1mol / L (NH 4 ) 2 SO 4 Soak in solution for 14h, dry, 600 o C roasting.
Example Embodiment
[0019] Example 2
[0020] Add 2 g of catalyst Cl in a 300 ml tank reactor - / TiO 2 , 100ml of methanol and 150ml of formaldehyde, reacted at 130oC and 0.6 MPa autogenous pressure for 4h, and the sample was centrifuged and analyzed by gas chromatography. The product contains polyoxymethylene dimethyl ether (CH 3 O(CH 2 O) n CH 3 ) And unreacted raw materials methanol and formaldehyde, the composition distribution is as follows (expressed in weight %): methanol 38.5%; methylal 32.1%; formaldehyde 0%; n=2, 17.1%; n=3, 10.2%; n =4, 0%; n=5~10, 0%; n> 10. Margin.
[0021] The solid super acid used Cl - / TiO 2 Catalyst preparation method:
[0022] Measure 100ml TiCl 4 The solution was quickly added 12.5% by mass NH in a 200 ml beaker 3 ·H 2 O until no white smoke is emitted, filter and wash 100 o C dry. The powder is added to 2mol / L hydrochloric acid solution, soaked for 2h, dried, 600 o C roasting.
Example Embodiment
[0023] Example 3
[0024] Add 2 g of catalyst SO into a 300 ml tank reactor 4 2- / ZrO 2 , 100ml methanol and 300ml formaldehyde, in 80 o C reacted for 4h, and the sample was centrifuged and analyzed by gas chromatography. The product contains polyoxymethylene dimethyl ether (CH 3 O(CH 2 O) n CH 3 ) And unreacted raw materials methanol and formaldehyde, the composition distribution is as follows (expressed in weight %): methanol 14.3%; methylal 42.2%; formaldehyde 3.2%; n=2, 11.2%; n=3, 8.7%; n =4, 5.5%; n=5~10, 14.4%; n> 10. Margin.
[0025] Solid super acid SO used 4 2- / ZrO 2 Catalyst preparation method:
[0026] Weigh 100 grams of ZrOCl 2 Place it in a 400 ml beaker, make a 15% by mass aqueous solution, and add 12.5% by mass NH dropwise 3 ·H 2 O, adjust pH=9, age for 3h, filter by suction, and wash until no Cl - Check out. The above filter cake 100 o C drying and grinding. Add 10 g of the above powder to 150 ml of 0.5 mol / L H 2 SO 4 Soak in the solution for 2h, dry, 600 o C r...
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