Preparation method of sandaler
The technology of a kind of sandalwood ether and catalyst is applied in the field of preparation of sandalwood ether, and can solve the problems of low utilization rate of raw materials, large amount of peroxide used, and high energy consumption
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[0100] The present invention provides a kind of preparation method of santalyl ether, described method comprises steps:
[0101] (i) in an organic solvent, under the action of a hydration catalyst, methoxydihydromyrcene and water undergo a hydration reaction to generate santalyl ether;
[0102]
[0103] Wherein, the hydration catalyst includes a first catalyst and a second catalyst;
[0104] The first catalyst is a solid acid catalyst, the solid acid catalyst includes a solid acid and a first metal active component, the first metal active component is loaded on the solid acid, the first metal The active component is selected from the group consisting of platinum, nickel, molybdenum, or combinations thereof;
[0105] The second catalyst includes a modified cation exchange resin loaded with a second metal active component, and the modified cation exchange resin is a cation exchange resin soaked in a strong acid;
[0106] The second metal active component is selected from th...
Embodiment 1
[0174] Beta zeolite (ID: NKF-6-25YY, Cation Type H, Crystallinity 95%, SiO 2 / Al 2 o 3 (Molar ratio)=25, the wt.% of sodium oxide is 0.05%, specific surface area=640m 2 / g, Nankai University Catalyst Co., Ltd).
[0175] D72 macroporous strongly acidic cation exchange resin from Anhui Sanxing Resin Technology Co., Ltd.
[0176] alcohol catalyst
[0177] Alcoholation catalyst is the D72 macroporous strongly acidic cation exchange resin modified by strong acid, which is prepared by the following method:
[0178] (b) Soak commercially available D72 macroporous strongly acidic cation exchange resin with hydrochloric acid, make it ion-exchange and carry out modification treatment, dry, obtain the D72 macroporous strongly acidic cation exchange resin modified by strong acid, i.e. alcohol catalyst, Wherein, the concentration of hydrochloric acid used is 2 mol / L, the dosage of hydrochloric acid is 10 times of the resin weight, the soaking time is 12 hours, and the soaking temperat...
Embodiment 2-18
[0195] The preparation method of santalyl ether, described method comprises steps:
[0196] (1) Preparation of Methoxydihydromyrcene
[0197]
[0198] Dihydromyrcene, methanol and the alcoholization catalyst prepared in Example 1 were uniformly mixed, wherein the ratio of the amount of dihydromyrcene to methanol was 1:4, and the amount of the alcoholization catalyst was 35g per mole Dihydromyrcene was reacted with stirring at a reaction temperature of 40° C. for 36 hours. After the reaction reached equilibrium, it was naturally cooled, filtered, and the filtrate was collected. The filtrate was washed successively with saturated sodium bicarbonate solution, distilled water, and saturated sodium chloride, dried over anhydrous magnesium sulfate, and filtered through the dried solution. The fraction at 83°C / 12mmHg yielded methoxydihydromyrcene with a yield of 86.3%.
[0199] (2) preparation of santalyl ether
[0200]
[0201] The hydration catalyst of embodiment 1 is pack...
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Abstract
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