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Method for selective catalytic hydrogenation for 9,9-bi(methoxymethylated) fluorine (BMMF)

A methoxymethyl, catalytic hydrogenation technology, applied in 9 fields, achieves the effects of good repeatability, simple operation and high product stereoselectivity

Inactive Publication Date: 2011-01-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But for its highly selective hydrogenation product cis-1,2,3,4,4a,9a-hexahydro-9,9-di(methoxymethyl)(cis-H 6 BMMF) fluorene has not been reported yet

Method used

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  • Method for selective catalytic hydrogenation for 9,9-bi(methoxymethylated) fluorine (BMMF)
  • Method for selective catalytic hydrogenation for 9,9-bi(methoxymethylated) fluorine (BMMF)
  • Method for selective catalytic hydrogenation for 9,9-bi(methoxymethylated) fluorine (BMMF)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In an autoclave with a volume of 75 milliliters, 2.03 grams of BMMF, 20 milliliters of cyclohexane, and 0.25 grams of activated modified skeleton nickel catalyst were put into the autoclave. MPa of hydrogen, put it into an oil bath and slowly heat up to 120°C, adjust the hydrogen valve to make the system pressure reach 2.0MPa, react for 320min, analyze it by gas chromatography after cooling, the conversion rate of raw materials is 100%, and the product cis-H 6 The selectivity of BMMF was 96.6%.

Embodiment 2

[0023] In an autoclave with a volume of 75 milliliters, 2.03 grams of BMMF, 20 milliliters of tetrahydrofuran, and 0.25 grams of activated modified skeleton nickel catalyst were put into the autoclave. Put hydrogen in an oil bath and slowly heat up to 140°C, adjust the hydrogen valve to make the system pressure reach 2.0MPa, react for 30min, and analyze by gas chromatography after cooling, the conversion rate of raw materials is 100%, and the product cis-H 6 The selectivity of BMMF was 96.1%.

Embodiment 3

[0025] In an autoclave with a volume of 75 milliliters, 2.03 grams of BMMF, 20 milliliters of n-hexane, and 0.25 grams of activated modified skeleton nickel catalyst were put into the autoclave, and the reactor was closed, replaced with nitrogen for 3 times, replaced with hydrogen for 3 times, and then filled with 0.5MPa Put the hydrogen in an oil bath and slowly heat up to 130°C, adjust the hydrogen valve to make the system pressure reach 2.0MPa, react for 60min, and analyze it by gas chromatography after cooling. The conversion rate of raw materials is 100%, and the product cis-H 6 The selectivity of BMMF was 96.2%.

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Abstract

The invention relates to a method for selective catalytic hydrogenation for 9,9-bi(methoxymethylated) fluorine (BMMF), which comprises the following steps: adding BMMF, solvent and a modified skeleton nickel catalyst in an autoclave, wherein the mass ratio of the solvent to the BMMF is 1:1-10:1, the dosage of the modified skeleton nickel catalyst is 1-20wt% of that of the BMMF; replacing air after closing the autoclave; then introducing a certain amount of hydrogen; putting the autoclave into oil bath, and heating slowly to the reaction temperature, wherein the reaction temperature is 100-250DEG C; and adjusting a hydrogen valve so as to enable the system pressure to be 0.5-4.0MPa and keeping for 0.5-5h, wherein the selectivity of cis-H6BMMF can be up to 98%. The method has the characteristics of simple operation, good repeatability, high product stereoselectivity and the like.

Description

technical field [0001] The invention belongs to the application field of catalytic hydrogenation, and relates to a method for selective catalytic hydrogenation of 9,9-bis(methoxymethyl)fluorene (BMMF). This method can prepare high stereoselective cis-1,2,3,4,4a,9a-hexahydro-9,9-bis(methoxymethyl)fluorene (cis-H 6 BMMF). Background technique [0002] Since Natta discovered TiCl in 1954 4 、TiCl 3 / AlR 3 or AlR 2 Since Cl can prepare high-isotactic polypropylene, Ziegler-Natta catalyst has been greatly developed, the efficiency of the catalyst is getting higher and higher, and the preparation process is becoming more and more exquisite. A new generation of Ziegler-Natta catalysts synthesized with diether compounds as electron donors can obtain highly active catalysts and high isotactic polypropylene without the need for additional electron donors. Since no external electron donor is needed in the polymerization process, the complexity of the reaction system is reduced, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/164C07C41/18
Inventor 吕连海杜文强胡少伟刘益材李化毅候召民
Owner DALIAN UNIV OF TECH
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