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Supercritical technology-based method for separating and purifying high-purity alpha-methylnaphthalene

A technology of supercritical technology and purification method, which is applied in the field of separation and purification of high-purity α-methylnaphthalene, can solve problems affecting the purity of α-methylnaphthalene, achieve mild oxidation method, improve the effect, and use less acid Effect

Active Publication Date: 2018-09-28
PENG CHEN NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen from the above prior art that α-methylnaphthalene can be separated and purified by adding solvent and batch rectification, and the main impurities of α-methylnaphthalene are methylbenzothiophene, biphenyl, quinoline and indole, However, to remove quinoline and indole in the separation method, there will inevitably be acid or alkali residues, which will affect the purity of α-methylnaphthalene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Methylnaphthalene containing sulfides such as methylnaphthalene, quinoline, indole, biphenyl, methylbenzothiophene, thianaphne and methylthiane, and the total methylnaphthalene content is not less than 60% Distillate, according to the volume ratio of ethanolamine and total methylnaphthalene is 3:5, add ethanolamine, after mixing uniformly by pre-mixer, transfer to supercritical reactor, heat up to 180°C at a rate of 20°C / min, Turn on condensed water, cool and stir at a rate of 150r / min, then lower the temperature to 166°C at a rate of 5°C / min, stop heating after 1 hour of constant temperature reaction, and separate and collect gas-liquid products to obtain a nitrogen-removing methylnaphthalene composition.

[0025] (2) According to the molar ratio of acetic anhydride catalyst, hydroxide peroxide and sulfide is 5.1:6.5:1, preheat the nitrogen-removing methylnaphthalene composition to 70°C, and slowly add ethyl alcohol dropwise at 1mL / 5min. An acid anhydride catalyst ...

Embodiment 2

[0028] (1) Methylnaphthalene containing sulfides such as methylnaphthalene, quinoline, indole, biphenyl, methylbenzothiophene, thianaphne and methylthiane, and the total methylnaphthalene content is not less than 60% Fraction, according to the volume ratio of ethanolamine and total methylnaphthalene is 3: 10, add ethanolamine, after premixer mixes, transfer to and place in supercritical reactor, be warming up to 180 ℃ with the speed of 25 ℃ / min, Turn on condensed water, cool and stir at a rate of 200r / min, then lower the temperature to 168°C at a rate of 10°C / min, stop heating after 6 hours of constant temperature reaction, and separate and collect gas-liquid products to obtain a nitrogen-removing methylnaphthalene composition.

[0029] (2) According to the molar ratio of acetic anhydride catalyst, hydroxide peroxide and sulfide is 5.3:7.5:1, after preheating the methylnaphthalene composition for nitrogen removal to 80°C, slowly add ethyl alcohol dropwise at 5mL / 5min An acid a...

Embodiment 3

[0032](1) Methylnaphthalene containing sulfides such as methylnaphthalene, quinoline, indole, biphenyl, methylbenzothiophene, thianaphne and methylthiane, and the total methylnaphthalene content is not less than 60% Distillate, according to the volume ratio of ethanolamine and total methylnaphthalene is 3:6, add ethanolamine, after mixing uniformly by pre-mixer, transfer to place in supercritical reactor, heat up to 180°C at a rate of 23°C / min, Turn on condensed water, cool and stir at a rate of 180r / min, then lower the temperature to 167°C at a rate of 6°C / min, stop heating after 4 hours of constant temperature reaction, and separate and collect gas-liquid products to obtain a nitrogen-removing methylnaphthalene composition.

[0033] (2) According to the molar ratio of acetic anhydride catalyst, hydroxide peroxide and sulfide as 5.2:6.8:1, preheat the nitrogen-removing methylnaphthalene composition to 75°C, and slowly add ethyl alcohol dropwise at 3mL / 5min. An acid anhydride ...

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Abstract

The invention provides a supercritical technology-based method for separating and purifying high-purity alpha-methylnaphthalene. The method comprises the steps of: adding ethanolamine into a methylnaphthalene fraction, conducting even mixing by using a pre-mixer, transferring the mixture to a supercritical reactor, raising the temperature to 180 DEG C, performing cool stirring by introducing condensed water, then decreasing the temperature to 166-168 DEG C, performing a constant temperature reaction, stopping heating, and performing separation and collection on gas-liquid products to obtain anitrogen-removed methylnaphthalene composition; preheating the nitrogen-removed methylnaphthalene composition, adding an acetic anhydride catalyst and hydrogen peroxide slowly and dropwise, performinghigh-speed stirring under the action of heating and ultrasonic waves, performing extraction and rectification to obtain a sulfur-removed methylnaphthalene composition, adding ethylene glycol into thesulfur-removed methylnaphthalene combination, performing azeotropy, collecting gas, condensing the collected gas to obtain a high-purity alpha+beta methylnaphthalene composition, then adding 2-amino-3-methylpyridine to the high-purity alpha+beta methylnaphthalene composition, and performing azeotropy and separation to obtain the high-purity alpha-methylnaphthalene with a purity up to 99.8%.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of α-methylnaphthalene, in particular to a method for separating and purifying high-purity α-methylnaphthalene based on supercritical technology. Background technique [0002] α-Methylnaphthalene, also known as 1-methylnaphthalene, is a colorless or light yellow liquid with blue fluorescence at room temperature, with the smell of naphthalene, insoluble in water and alkali, soluble in ether and acetone And aromatic hydrocarbons, melting point is -22 ℃, boiling point is 244.6 ℃, density is 1.02, refined α-methylnaphthalene can be used to synthesize 1, 4 naphthalene dicarboxylic acid, used as raw material for the production of fluorescent whitening agent dyes, and also used in production engineering Resin for plastics, synthetic 1-naphthoic acid as a plant growth hormone, synthetic 1-naphthoic acid as a raw material for color photographic dyes, and can also be used as a pharmaceut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/00C07C7/06C07C7/10C07C7/148C07C15/24
CPCC07C7/005C07C7/06C07C7/10C07C7/14858C07C7/14875C07C15/24Y02P20/54
Inventor 谈勇谈俊江晓龙
Owner PENG CHEN NEW MATERIALS TECH CO LTD
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