A kind of method for preparing 1,3-propanediol
A technology for propylene glycol and propanol, which is used in hydrolysis preparation, chemical instruments and methods, catalyst activation/preparation, etc., can solve problems such as poor stability of intermediate products, low yield of 1,3-propanediol, etc., and achieve mild and stable reaction conditions. The effect of good performance and remarkable technical effect
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Embodiment 1
[0029] Preparation of hydrogenation catalyst:
[0030] Among them, the content of active components is: CuO, 40wt%; ZnO, 12wt%; ZrO 2 , 5wt%; P 2 o 5 , 0.3wt%.
[0031] Weigh copper nitrate, zinc nitrate, zirconium nitrate and ammonium hydrogen phosphate according to the proportion and dissolve them in pure water to make a mixed solution with a concentration of 1mol / L; weigh the silica sol according to the proportion, and add the prepared mixed solution while stirring, After uniform stirring, it was dried at 90° C. for 4 hours, calcined at 550° C. for 5 hours, and pressed into tablets to obtain the hydrogenation catalyst.
[0032] Preparation of 1,3-propanediol:
[0033] Step (1): Put 2.5 ml of the hydrogenation catalyst prepared into a fixed-bed reactor, and reduce it for 20 h at 280° C. in the presence of a mixed gas of hydrogen and nitrogen with a hydrogen volume concentration of 5v%. Then at 200°C, 5MPa, hydrogen / ester molar ratio 30:1, volume space velocity 2h -1 Un...
Embodiment 2
[0036] Preparation of hydrogenation catalyst:
[0037] Among them, the content of active components is: CuO, 30wt%; ZnO, 12wt%; ZrO 2 , 5wt%; P 2 o 5 , 0.3wt%.
[0038] Dissolve copper nitrate, zinc nitrate, zirconium nitrate and ammonium hydrogen phosphate in pure water according to the ratio to make a mixed solution with a concentration of 1mol / L, and weigh SiO with a particle size of 80-150 microns according to the ratio 2 The microsphere carrier was mixed and impregnated at 60°C for 5 hours, dried at 90°C for 4 hours, and calcined at 550°C for 5 hours to obtain the hydrogenation catalyst.
[0039] Preparation of 1,3-propanediol:
[0040]Step (1): Using the same reaction conditions as step (1) in Example 1 to evaluate the hydrogenation catalyst, the hydrogenation reaction result is: the conversion rate of methyl 3-methoxypropionate is 99.74%, and the conversion rate of 3-methoxy The selectivity to 1-propanol was 98.52%.
[0041] Step (2): using the same reaction condi...
Embodiment 3
[0043] Preparation of hydrogenation catalyst:
[0044] Among them, the content of active components is: CuO, 25wt%; ZnO, 12wt%; ZrO 2 , 5wt%; P 2 o 5 , 0.3wt%.
[0045] Using the same catalyst preparation method as in Example 2, the hydrogenation catalyst was obtained.
[0046] Preparation of 1,3-propanediol:
[0047] Step (1): Using the same reaction conditions as step (1) in Example 1 to evaluate the hydrogenation catalyst, the hydrogenation reaction result is: the conversion rate of methyl 3-methoxypropionate is 96.51%, and the conversion rate of 3-methoxypropionate is 96.51%. The selectivity to 1-propanol was 98.26%.
[0048] Step (2): using the same reaction conditions as step (2) in Example 1 to carry out the hydrolysis experiment. The product was isolated and analyzed, and the yield of 1,3-propanediol was calculated to be 83.65%.
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