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Method for interlaminar oxidation of mercaptan compounds by supermolecular structure nanometer reactor

A thiol compound, nano-reactor technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problem of single selectivity of oxidation products

Inactive Publication Date: 2008-04-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for interlayer oxidation of mercaptan compounds using a supramolecular structure nanoreactor, which solves the problem of single selectivity of oxidation products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step A: 20.48g (0.08mol) of solid Mg(NO 3 ) 2 ·6H 2 O and 15.00g (0.04mol) of solid Al(NO 3 ) 3 9H 2 O dissolved in 50mL to remove CO 2 in deionized water (solution 1); another 10.64g (0.08mol) L-cysteine ​​and 14.08g (0.352mol) NaOH were dissolved in 50mL to remove CO 2 deionized water (solution 2).

[0025] Step B: Place solution 2 in a three-necked flask, under N 2 Under the condition of air protection, while vigorously stirring, solution 1 was slowly added dropwise to solution 2, and the drop was completed in about 2 hours.

[0026] Step C: After the dropwise addition, adjust the pH value to 10 with 5 mol / L NaOH solution, and heat to reflux for 6 hours.

[0027] Step D: CO removal with freshly prepared 2 The deionized hot water was centrifuged and washed to a pH of about 7, and dried at 70°C for 24 hours to obtain a magnesium-aluminum cysteine-intercalated hydrotalcite material.

[0028] According to the XRD spectrum, FT-IR spectrum, thermogravimetric spec...

Embodiment 2

[0032] The preparation method of L-cysteine ​​intercalated hydrotalcite is the same as in Example 1.

[0033] Take 1g of L-cysteine ​​intercalated hydrotalcite, add it to a three-necked bottle, add 50ml 2 Deionized water, N 2 Under protection, stir vigorously for 3h to make it highly dispersed. Then slowly drop a little Br 2 ([Br 2 ] / [CySH]=0.5), after 1 hour of reaction, suction filtration and washing, vacuum drying at room temperature for 48 hours to obtain the oxidized product.

[0034] By XRD, FT-IR, Raman, 13 C NMR and elemental analysis characterization shows that, unlike the open system, due to the influence of the confined space between the hydrotalcite layers, the Br 2 Diffusion becomes more difficult. Br 2 The oxidation product of interlayer cysteine ​​in oxidized hydrotalcite does not change with the amount of oxidant, and the oxidation product is only cysteine ​​sulfonic acid.

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Abstract

The present invention provides preparation process of supermolecular structure nanometer reactor and belongs to the field of organic-inorganic composite material preparing and applying technology. Mercaptan compound is first inserted into hydrotalcite layers by means of co-precipitation or ion exchange process; and mercaptan compound is then oxidized with hydrotalcite as molecular reactor and through intercalating hydrotalcite with small amount of L-cysteine, adding CO2-eliminated deionized water, stirring under N2 protection for 1-3 hr for high dispersing, dropping small amount of oxidant to react for 0.5-1 hr, sucking filtering, washing, and vacuum drying at normal temperature for 24-48 hr to obtain oxidized product. The present invention is superior in that the laminated nanometer space of hydrotalcite is used as the reactor for oxidizing mercaptan compound so as to obtain single oxidized product.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of organic-inorganic composite materials, and in particular provides a method for interlayer oxidation of mercaptan compounds by using a supramolecular structure nano-reactor. It involves the preparation of a hydrotalcite composite material with an intercalation structure and the study of its reactor characteristics by an interlayer oxidation method. Background technique [0002] Organisms and life processes are the product of hundreds of millions of years of evolution. Various biomolecules are assembled at different levels from microscopic to macroscopic. Complex but precise assembly systems are formed spontaneously to achieve various specific biological functions and other functions. The research of modern supramolecular science shows that synthetic molecules can also have this kind of spontaneous assembly behavior. According to the principles of bionics, the assembly behavi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/16C07C309/01C01B31/24C01B32/60
CPCC07K5/0215C07C303/16C07C309/18
Inventor 段雪卫敏史志宇
Owner BEIJING UNIV OF CHEM TECH
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