Method for preparing 1,10-decanediol through supercritical dimethyl sebacate hydrogenation
A technology of dimethyl sebacate and decanediol, which is applied in the field of supercritical hydrogenation of dimethyl sebacate to prepare 1,10-decanediol, which can solve the problems of high pressure and large amount of hydrogen recycling
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Embodiment 1
[0019] (1), methyl alcohol and dimethyl sebacate are mixed homogeneously with mass ratio 2:3; (2), the raw material in hydrogen and step (1) is mixed with certain hydrogen-ester ratio and sent into the fixed-bed reactor Pre-mixer; (3), the uniformly mixed raw materials in step (2) are continuously fed into a 10ml 20~40 mesh Cu / ZnO / Al 2 o 3 Catalyst (Cu50%wt, ZnO40%wt, Al 2 o 3 10%wt) fixed-bed reactor for hydrogenation reaction under certain conditions. (see Table 1 for specific conditions); (4), the product enters the separator and separates to obtain 1,10-decanediol. The reaction results are shown in Table 1.
[0020] Table 1 embodiment 1 reaction conditions and reaction result
[0021] Reaction temperature / ℃ air speed / h -1 hydrogen ester ratio Reaction pressure / MPa X / % S / % 240 0.3 80:1 8.5 98.69 97.99 245 0.4 50:1 8 99.05 95.48 250 0.5 35:1 9 99.85 94.23
[0022] Note: X , the conversion rate of dimethyl sebacate; ...
Embodiment 2
[0026] (1), methyl alcohol and dimethyl sebacate are mixed homogeneously with 1:3 mass ratio; (2), hydrogen and the raw material in the step (1) are mixed with certain hydrogen-ester ratio and sent to the fixed-bed reactor Pre-mixer; (3), the uniformly mixed raw materials in step (2) are continuously fed into a 10ml 20~40 mesh Cu / ZnO / Al 2 o 3 Catalyst (Cu50%wt, ZnO30%wt, Al 2 o 3 20%wt) fixed-bed reactor, hydrogenation reaction is carried out under certain conditions. (see Table 2 for specific conditions); (4), the product enters the separator and separates to obtain 1,10-decanediol. The reaction results are shown in Table 2.
[0027] Table 2 embodiment 2 reaction conditions and reaction result
[0028] Reaction temperature / ℃ air speed / h -1 hydrogen ester ratio Reaction pressure / MPa X / % S / % 240 0.3 90:1 9 95.46 98.99 250 0.4 75:1 8.5 98.45 92.48 260 0.5 45:1 8 99.15 91.23
[0029] Note: X , the conversion rate of dime...
Embodiment 3
[0031] (1), methyl alcohol and dimethyl sebacate are mixed homogeneously with 1:1 mass ratio; (2), hydrogen is mixed with the raw material in step (1) and sent to fixed-bed reactor with certain hydrogen-ester ratio Pre-mixer; (3), the uniformly mixed raw materials in step (2) are continuously fed into a 10ml 20~40 mesh Cu / ZnO / Al 2 o 3 Catalyst (Cu40%wt, ZnO40%wt, Al 2 o 3 20%wt) fixed-bed reactor, hydrogenation reaction is carried out under certain conditions. (see Table 3 for the specific conditions); (4), the product enters the separator and separates to obtain 1,10-decanediol. The reaction results are shown in Table 3.
[0032] Table 3 embodiment 3 reaction conditions and reaction result
[0033] Reaction temperature / ℃ air speed / h -1 hydrogen ester ratio Reaction pressure / MPa X / % S / % 240 0.3 90:1 9 93.46 98.89 250 0.4 75:1 8.5 94.45 93.48 260 0.5 45:1 8 96.15 90.23
[0034] Note: X , the conversion rate of dimethyl...
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