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Supercritical technology-ultrasonic wave-based method for separating and refining beta-methylnaphthalene

A refining method and technology of methylnaphthalene fractions, applied in the field of separation and purification of β-methylnaphthalene, can solve the problems of harsh process conditions of β-methylnaphthalene and low product yield, and achieve mild oxidation method and high desulfurization efficiency , the effect of less acid consumption

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

Known from above-mentioned prior art, the process condition of refining and purifying β-methylnaphthalene in heavy aromatics is harsh, and product yield is low, therefore it is necessary to improve the yield of high-purity refining β-methylnaphthalene

Method used

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  • Supercritical technology-ultrasonic wave-based method for separating and refining beta-methylnaphthalene

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 composition is not less than 60% After the fraction was first treated with 10% ammonium bisulfate aqueous solution, according to the volume ratio of ethanolamine and total methylnaphthalene as 3:5, after adding ethanolamine and mixing uniformly through a premixer, it was transferred to and placed in a supercritical reactor. Raise the temperature to 120°C at a rate of ℃ / min, turn on the condensed water and cool and stir at a rate of 150r / min for 0.5h, raise the temperature to 180°C at a rate of 20°C / min, turn on the condensed water and cool and stir at a rate of 150r / min for 2h, and then Cool down 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.

...

Embodiment 2

[0028] (1) Methylnaphthalene containing sulfides such as methylnaphthalene, quinoline, indole, biphenyl, methylbenzothiophene, thianaphne, and methylthiane, and the total methylnaphthalene composition is not less than 60% After the cut was first treated with 20% ammonium bisulfate aqueous solution, according to the volume ratio of ethanolamine and total methylnaphthalene as 3:10, add ethanolamine after the premixer mixes uniformly, transfer to be placed in the supercritical reactor, with 16 The temperature is raised to 130°C at a rate of ℃ / min, the condensed water is cooled and stirred at a rate of 150r / min for 1h, the temperature is raised to 180°C at a rate of 25°C / min, the condensed water is cooled and stirred at a rate of 150r / min for 4h, and then The temperature was lowered to 168°C at a rate of 10°C / min, the heating was stopped after 6 hours of constant temperature reaction, and the gas-liquid products were separated and collected to obtain a nitrogen-removing methylnapht...

Embodiment 3

[0032] (1) Methylnaphthalene containing sulfides such as methylnaphthalene, quinoline, indole, biphenyl, methylbenzothiophene, thianaphne, and methylthiane, and the total methylnaphthalene composition is not less than 60% After the cut was first treated with 15% ammonium bisulfate aqueous solution, according to the volume ratio of ethanolamine and total methylnaphthalene as 3:7, add ethanolamine after the premixer mixes uniformly, transfer to be placed in the supercritical reactor, with 15 Raise the temperature to 125°C at the rate of ℃ / min, cool and stir at the rate of 150r / min for 0.8h when the condensed water is turned on, raise the temperature to 180°C at the rate of 23°C / min, cool and stir at the rate of 150r / min for 3h when the condensed water is turned on, and then The temperature was lowered to 167°C at a rate of 7°C / min, the heating was stopped after 3 hours of constant temperature reaction, and the gas-liquid products were separated and collected to obtain a nitrogen-...

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Abstract

The invention provides a supercritical technology-ultrasonic wave-based method for separating and refining beta-methylnaphthalene. The method comprises the following steps of: treating a methylnaphthalene fraction firstly by using an aqueous solution of ammonium bisulfate, adding ethanolamine, conducting even mixing by using a pre-mixer, transferring the mixture to a supercritical reactor, raisingthe temperature to 180 DEG C at a rate of 20-25 DEG C / min, performing cool stirring by introducing condensed water, then decreasing the temperature to 166-168 DEG C at a rate of 5-10 DEG C / min, performing a constant temperature reaction for 1-6 h, stopping heating, and performing separation and collection on gas-liquid products to obtain a nitrogen-removed methylnaphthalene composition; preheating the composition to 65-75 DEG C, adding an acetic anhydride catalyst and hydrogen peroxide slowly and dropwise, performing high-speed stirring for 60-90 min under the action of ultrasonic waves at 70-80 DEG C, performing extraction and rectification to obtain a sulfur-removed methylnaphthalene composition, adding ethylene glycol into the sulfur-removed methylnaphthalene combination, heating the mixture to 190-195 DEG C under the action of ultrasonic waves, collecting gas, condensing the collected gas to obtain a high-purity alpha+beta methylnaphthalene composition, then placing the high-purity alpha+beta methylnaphthalene composition in a freezing microtome, performing freezing crystallizing at -25-(-15) DEG C, performing separation, and performing redissolving to prepare the beta-methylnaphthalene at 36-38 DEG C.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of β-methylnaphthalene, and in particular relates to a method for separating and refining β-methylnaphthalene based on supercritical and ultrasonic waves. Background technique [0002] High-purity refined β-methylnaphthalene is β-methylnaphthalene with a purity higher than 95%, and it is a raw material for the synthesis of vitamin K drugs such as 2-methyl-1,4-naphthoquinone, hemostatic drugs and feed additives. It can also be used to synthesize 2-naphthaleneacetic acid and 2,3-naphthalene diacid organic dyes, etc. It is an important organic chemical raw material. Methylnaphthalene contained in heavy aromatics prepared by petroleum catalytic cracking, catalytic reforming and thermal cracking, etc., can be obtained by cutting the distillate with a distillation range of 230-245 ° C. The crude product of β-methylnaphthalene also contains α-formazan Base naphthalene, naphthalene, q...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/00C07C7/04C07C7/05C07C7/10C07C7/14C07C7/148C07C15/24
CPCC07C7/005C07C7/04C07C7/05C07C7/10C07C7/14C07C7/14858C07C7/14875C07C15/24Y02P20/54
Inventor 谈勇谈俊江晓龙
Owner PENG CHEN NEW MATERIALS TECH CO LTD
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