Preparation method of lyral
A technology of lyral and catalyst, which is applied in the field of preparation of lyral, can solve the problems of large environmental pollution, polymerization or yield decline, low yield, etc.
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[0078] The invention provides a kind of preparation method of lyral, and described method comprises steps:
[0079] (1) in an organic solvent, under the effect of a hydration catalyst, citrus aldehyde and water undergo a hydration reaction to generate neoliral;
[0080]
[0081] Wherein, the hydration catalyst includes a first catalyst and a second catalyst;
[0082] 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, or a combination thereof;
[0083] The second catalyst is a modified cation exchange resin loaded with a second metal active component, the modified cation exchange resin is a cation exchange resin soaked in a strong acid, and the second metal active component is selected from the following Groups: Zinc chloride, aluminum chlorid...
Embodiment 1
[0146] 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).
[0147] D72 macroporous strongly acidic cation exchange resin from Anhui Sanxing Resin Technology Co., Ltd.
[0148] Preparation of the first catalyst
[0149] The first catalyst is a solid acid catalyst supporting the first metal active component, which is prepared by the following method:
[0150] Using solid acid β zeolite as a carrier, impregnate β zeolite with one or more of the aqueous solutions containing different amounts of chloroplatinic acid and nickel nitrate hexahydrate, dry at 130°C after impregnation, and roast and reduce at 480°C. Obtain the solid acid catalyst supporting the first metal active component, i.e. the first catalyst, and the different first catalysts are as shown in Table 1:
[0151] The first catalyst of different components of table 1 ...
Embodiment 2-17
[0161] Hydration catalyst
[0162] The hydration catalyst is the beta zeolite of Example 1, the first catalyst, the second catalyst or a mixture of the first catalyst and the second catalyst.
[0163] The preparation method of lyral
[0164] Add isopropanol, citrus aldehyde and water into the stirring mixing tank according to the molar ratio of 1:0.5:1, add different hydration catalysts according to 2wt% of the amount of citrus aldehyde added, mix and pump into the reaction tower, Reaction at 80°C for 8h, after the completion of the reaction, successively layered with a continuous stratifier, solvent removed through a solvent removal tower, and rectified to obtain the product Neoliral, under different hydration catalyst conditions, HPLC (high performance liquid The selectivity (the lyral that the reaction generates accounts for the percentage of the amount of substance of the product generated by the reaction), the conversion rate of citrus aldehyde are as shown in table 3: ...
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Abstract
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