Method for synthesizing tricyclic decane unsaturated monoaldehyde

A tricyclodecane and unsaturated technology, which is applied in the field of synthesizing tricyclodecane unsaturated monoaldehyde, can solve the problems of low monoaldehyde selectivity, complex reaction system, and high reaction temperature, and achieve simple reaction system and high preparation process. The effect of simplicity and mild reaction conditions

Inactive Publication Date: 2012-08-01
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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Problems solved by technology

[0004] In conclusion, the main problems in the synthesis of tricyclodecane unsaturated monoaldehydes are that the reaction system is complicated, a large amount of solvents, phase transfer agents or surfactants are needed, the reaction temperature is relatively high, and the selectivity of monoaldehydes is relatively low.

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  • Method for synthesizing tricyclic decane unsaturated monoaldehyde

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Embodiment 1

[0029] Preparation of Ferromagnetic Oxide Iron Tetroxide Directly Supporting Metal

[0030] a, under strong stirring, 50mmol (20.2g) Fe(NO 3 ) 3 9H 2 O and (0.1 g) RhCl 3 ·3H 2 O was dissolved in 100mL distilled water, then added dropwise to 330mL (0.47mol / L) Na 2 CO 3 In the aqueous solution, the precipitation temperature is 20°C, and the whole process takes about 1 hour. The precipitate is vacuum filtered and centrifuged, and the precipitate is washed with distilled water to neutrality. The metal hydroxide supported by iron hydroxide formed by precipitation is in the Dry at 120°C for 16 hours to obtain a brown solid;

[0031] b. Roasting the brown solid in step a at a temperature of 400° C., the roasting time is 4 hours, and the roasting atmosphere is air;

[0032] c. Reducing and activating the roasted solid in step b with hydrogen as a reductant at a temperature of 400° C. for 1 hour to obtain about 4 g of rhodium metal supported by ferromagnetic oxide ferric oxide;...

Embodiment 2

[0038] Preparation of Ferromagnetic Oxide Iron Tetroxide Directly Supporting Metal

[0039] Under vigorous stirring, 50mmol (20.2g) Fe(NO 3 ) 3 9H 2 O and (0.1 g) RhCl 3 ·3H 2 O was dissolved in 100mL of distilled water, and then added dropwise to 330mL (0.47mol / L) NaOH aqueous solution. The precipitation temperature was 40°C. The whole process took about 1 hour. The precipitate was vacuum filtered and centrifuged, and the precipitate was washed with distilled water. To neutrality, the metal hydroxide supported by iron hydroxide formed by precipitation was dried at a temperature of 80 ° C for 6 hours to obtain a brown solid;

[0040] b. Roasting the brown solid in step a at a temperature of 200° C., the roasting time is 4 hours, and the roasting atmosphere is nitrogen;

[0041] c. Reducing and activating the roasted solid in step b with hydrogen as a reductant at a temperature of 200° C. for 6 hours to obtain about 4 g of rhodium metal supported by ferromagnetic oxide tri...

Embodiment 3

[0047] Preparation of Ferromagnetic Oxide Iron Tetroxide Directly Supporting Metal

[0048] Under vigorous stirring, 50mmol (20.2g) Fe(NO 3 ) 3 9H 2 O and (0.1 g) RhCl 3 ·3H 2 O, 0.1g of cobalt nitrate was dissolved in 100mL of distilled water, and then added dropwise to 330mL (0.47mol / L) of ammonia solution, the precipitation temperature was 20°C, and the whole process took about 1 hour, and the precipitate was vacuum filtered and centrifuged. The precipitate was washed with distilled water to neutrality, and the iron hydroxide-supported metal hydroxide formed by precipitation was dried at a temperature of 100° C. for 8 hours to obtain a brown solid;

[0049] b. Roasting the brown solid in step a at a temperature of 300° C., the roasting time is 5 hours, and the roasting atmosphere is air;

[0050] c. The solid roasted in step b is activated by hydrogen reduction with a reducing agent at a temperature of 300° C. for 2 hours to obtain about 4 g of cobalt-rhodium bimetal s...

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Abstract

The invention relates to a method for synthesizing a tricyclic decane unsaturated monoaldehyde. According to the method, a dicylopentadiene is catalyzed under the action of a catalyst at the low temperature and pressure without using a solvent to synthesize a tricyclic unsaturated monoaldehyde, the catalyst is a metal phosphonic complex catalyst which is carried by a ferromagnetic oxide, and an impregnation method and a coprecipitation method are used to prepare the tricyclic decane unsaturated monoaldehyde. By means of the method, the conversion rate of the dicylopentadiene (DCPD) can reach to above 99%, and the selectivity of the tricyclic decane unsaturated monoaldehyde can reach to above 98%.

Description

Technical field: [0001] The invention relates to a method for synthesizing tricyclodecane unsaturated monoaldehyde. technical background: [0002] Dicyclopentadiene (DCPD) mainly comes from ethylene by-product C5 fraction and coal coking light benzene fraction. After hydroformylation, it can synthesize high value-added fine chemicals tricyclodecane unsaturated monoaldehyde and tricyclodecane dicarbaldehyde , Tricyclodecane dimethanol, etc. Alcohol produced by hydrogenation of the product aldehyde is not only a raw material for pesticides, lubricating oils and plasticizers, but also an intermediate for synthesizing fragrances and medicines. Among them, monoaldehydes can be directly used as spices with a fresh and delicate aroma, and the monoalcohols formed by hydrogenation of monoaldehydes are important intermediates for the synthesis of strong antiviral drugs with a helical structure. [0003] For the synthesis of tricyclodecane unsaturated monoaldehyde, the traditional sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/445C07C45/50B01J31/28
Inventor 吾满江·艾力马昱博高志贤
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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