Decomposing process for salicylic acid and its isomer using hydrotalcite

A technology for hydrotalcite and isomers, which is applied in the field of separation of structural isomers, can solve problems such as difficult separation, and achieve the effects of easy reaction, convenient and fast detection, and simple process

Inactive Publication Date: 2007-07-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is more difficult to resolve structural isomers with small differences in physical and chemical properties.

Method used

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  • Decomposing process for salicylic acid and its isomer using hydrotalcite
  • Decomposing process for salicylic acid and its isomer using hydrotalcite
  • Decomposing process for salicylic acid and its isomer using hydrotalcite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step A: AlCl 3 Soluble in a certain proportion with LiCl to remove CO 2 Deionized water was used to make a salt solution, and a certain concentration of NaOH alkali solution was prepared at the same time, and the two solutions were placed in the normal pressure funnel respectively, and the N 2 Drop it into the reactor under protection, stir to make it evenly mixed, and adjust the rate of addition to make the pH value 10.5. Crystallized at 65°C for 6h. The product was centrifuged and washed to neutrality; a small amount of sample was taken out and dried at 70°C for 20 hours for characterization, and [Li-Al-Cl] hydrotalcite was obtained.

[0026] Step B: Add equimolar mixed isomers of p-hydroxybenzoic acid and m-hydroxybenzoic acid to the hydrotalcite suspension, adjust the pH value of the solution to neutral, and react at 100°C for 10 hours. After the reaction is completed, suction filter, wash and dry , to obtain intercalation products.

[0027] It can be seen from ...

Embodiment 2

[0029] Step A: According to the method similar to Step A in Example 1, [Li-Al-Cl] hydrotalcite was obtained.

[0030] Step B: Add equimolar mixed isomers of o-hydroxybenzoic acid and m-hydroxybenzoic acid to the hydrotalcite suspension, adjust the pH value of the solution to neutrality, and react at 100°C for 10 hours. After the reaction, suction filter, wash and dry , to obtain intercalation products.

[0031] It can be seen from the X-ray diffraction pattern that the XRD pattern (b) of the intercalation reaction of the equimolar mixture of o-hydroxybenzoic acid and m-hydroxybenzoic acid with [Li-Al-Cl]LDHs is the same as that of the two isomers alone. It can be seen from the comparison of the XRD spectrum that the spectrum is very similar to the spectrum (a) of the intercalation of o-hydroxybenzoic acid alone, and the characteristic peaks of the 003 crystal plane appear at 2θ=5° and 16°. However, the spectrum (c) of intercalation with m-hydroxybenzoic acid alone is very dif...

Embodiment 3

[0033] Step A: According to the method similar to Step A in Example 1, [Li-Al-Cl] hydrotalcite was obtained.

[0034] Step B: Add equimolar mixed isomers of o-hydroxybenzoic acid and p-hydroxybenzoic acid to the hydrotalcite suspension, adjust the pH value of the solution to neutrality, and react at 100°C for 10 hours. After the reaction, suction filter, wash and dry , to obtain intercalation products.

[0035] It can be seen from the X-ray diffraction diagram, as shown in Figure 3.8, that the three spectra a, b, and c all have characteristic peaks at 2θ=5°, so it is difficult to judge p-hydroxybenzoic acid and o-hydroxybenzoic acid from the XRD spectrum alone. The amount of hydroxybenzoic acid entering the interlayer of [Li-Al-Cl] LDHs needs to be further detected and analyzed by high performance liquid chromatography (see Example 5 for details).

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Abstract

This invention relates to a method of using hydrotalcite lamellar material to split structural isomer, belongs to structural isomer separation areas. The process steps: Prepare hydrotalcite precursors which has layer anion Cl-, and molar ratio of plywood bivalence and trevalence basic ion M2 + / + M3 = 2 ~ 3; ortho-oxybenzoic acid and its isomer's sodium salt dissolved in deionized water of removed carbon dioxide; add referred hydrotalcite precursors, ortho-oxybenzoic acid and its isomer into the solution, under N2 protection and mixing, control the temperature at 70 ~ 100deg C for 8 to 12 hours; then the product fully washed by CO2 water, centrifugation, dry under 40 ~ 70 deg C. The advantage lies in: compare with the current widespread use of gamma-Al (OH) 3-situ synthesis method, coprecipitaion [Li-Al-Cl] LDHs precursors is low-cost, mild, fast response, small impurity peaks.

Description

[0001] Field [0002] The invention belongs to the field of separation of structural isomers, and provides a method for separating salicylic acid and its isomers by using lithium aluminum hydrotalcite, an inorganic functional material. Background technique [0003] Those with the same molecular formula but different order of linkage of atoms or groups in the molecule are called structural isomers. Isomers are a ubiquitous phenomenon in the biological world and one of the foundations for the survival of life. Most of the isomer compounds that exist in nature or are synthesized by ordinary methods are mixtures of several isomers, but for a special purpose, only one of the isomers often works, and because other isomers The mixing of isomers may weaken or even completely cancel the special effect of this isomer. Therefore, the resolution technology of structural isomers is the focus of many chemical companies' research and development. For the resolution of structural isomers w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/47C07C65/10C07C65/03C07B57/00B01J20/12
CPCB01D15/00C07C51/00C07B63/04B01J20/08
Inventor 卫敏陆刚段雪
Owner BEIJING UNIV OF CHEM TECH
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