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A kind of inclusion separation preparation method of (2-octyl)-ferrocene

A technology of ferrocene and moisture, applied in the field of inclusion separation and preparation of ferrocene, which can solve the problems of long cycle, difficult operation, low recovery rate, etc.

Active Publication Date: 2018-02-06
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in this process, there are the following problems: long cycle, high cost, low recovery rate, difficult operation, which is not conducive to industrial production

Method used

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  • A kind of inclusion separation preparation method of (2-octyl)-ferrocene
  • A kind of inclusion separation preparation method of (2-octyl)-ferrocene
  • A kind of inclusion separation preparation method of (2-octyl)-ferrocene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Add 150 g of Immo-CD-2 (silica gel: β-CD=4:1) 200-300 mesh filler Immo-CD-2 (silica gel: β-CD=4:1) with 5.5% water content mixed with 300 mL n-hexane to the 30 × 600 mm chromatographic column, and add (2-octyl 0.35g of the mixture of (2-octyl)-ferrocene and (3-octyl)-ferrocene was sampled with a 20mL sample bottle, and the purity of each sample was tracked and analyzed by GC. The highest value of (2-octyl)-ferrocene was The purity is 90.28%.

Embodiment 2

[0051] Add 150 g of Immo-CD-2 (silica gel: β-CD=4:1) 200-300 mesh packing with 5.5% water content mixed with 300 mL cyclohexane to the 30×600 mm chromatography column, and add (2-octyl 0.35g of the mixture of (2-octyl)-ferrocene and (3-octyl)-ferrocene was sampled with a 20mL sample bottle, and the purity of each sample was tracked and tested by GC. The highest concentration of (2-octyl)-ferrocene was The purity is 80.84%.

Embodiment 3

[0053] Add 150 g of Immo-CD-2 (silica gel: β-CD=4:1) 200-300 mesh filler Immo-CD-2 (silica gel: β-CD=4:1) containing 5.5% water and mix well with 300 mL of n-hexane into the 30×600 mm chromatographic column, and add (2-octyl )-ferrocene and (3-octyl)-ferrocene mixture 0.35g, sampled with 20mL sample bottle, tracked and tested each sample purity with GC, the highest purity of (2-octyl)-ferrocene was 90.72%.

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Abstract

The invention relates to a method for preparing (2-octyl)-ferrocene through inclusion separation. According to the method, high-purity C8-ferrocene separated with a method presented in the patent CN104876973A is taken as a raw material and subjected to column chromatography isolation once, a by-product (2-octyl)-ferrocene and (3-octyl)-ferrocene mixture of a leacheate is collected and subjected to solvent removal, on the basis that the (2-octyl)-ferrocene and (3-octyl)-ferrocene mixture is separated out, cyclodextrin (represented in the drawing 2) with an outer hydrophilic and inner hydrophobic structure is used for including silica gel, and a product is taken as filler (Immo-CD-2) to fill a chromatographic column which then separates a higher-purity (2-octyl)-ferrocene isomer from the (2-octyl)-ferrocene and (3-octyl)-ferrocene mixture, and a foundation is laid for theoretical research and industrial application of (2-octyl)-ferrocene.

Description

technical field [0001] The invention belongs to the field of separation and purification of octyl ferrocene, in particular to a preparation method for inclusion separation and separation of (2-octyl)-ferrocene. Background technique [0002] Ferrocene and its derivatives have been widely used in many fields such as medicine, electrochemistry, liquid crystal materials, photosensitive materials, fuel oil-saving smoke suppressants, and gas combustion-supporting catalysts. As one of the derivatives of ferrocene, octyl ferrocene is one of the most widely used rocket fuel catalysts. Adding it to rocket fuel can promote the full combustion of fuel and play a role in smoke suppression. It is used in aviation, aerospace and navigation It has played a huge role in industry and other fields. Due to the isomerism of the octyl substituent on the ring, the octyl ferrocenes are usually (2-octyl)-ferrocene, (3-octyl)-ferrocene and (4-octyl) base)-ferrocene mixture. However, the catalytic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 马晓燕高燕孙坤刘强朱林
Owner NORTHWESTERN POLYTECHNICAL UNIV