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Novel technique for preparing refined naphthalene from industrial naphthalin

A technology for industrial naphthalene and refined naphthalene, which is applied in chemical modification purification/separation, organic chemistry, distillation purification/separation, etc., can solve the problems of large consumption of organic acids and hydrogen peroxide, high cost, low yield of refined naphthalene, etc. , to achieve the effect of high selectivity, low consumption and high process yield

Inactive Publication Date: 2013-04-17
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the deficiencies in the prior art, such as large consumption of organic acid and hydrogen peroxide, low yield of refined naphthalene, high cost and other problems, and provide a kind of organic acid / hydrogen peroxide system A new process that significantly increases the reaction conversion rate of thiazene by adding inorganic acid and reduces the consumption of reaction reagents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Industrial naphthalene is 500g of raw material, which contains 96.4363% of naphthalene (mass fraction, the same below), 2.2026% of thiane, and 1.3611% of other impurities. The added reaction reagents are 30% hydrogen peroxide aqueous solution, 99% formic acid, and 95% concentrated sulfuric acid , wherein the moles of hydrogen peroxide, formic acid, and sulfuric acid are 8.9, 1.1, and 1.3 times that of thioindenne respectively, the reaction temperature is 85°C, and the reaction time is 60 minutes. 2, the pressure is 1 atm, the product purity is greater than 99.8%, the content of thiazene is 0.1461%, the product yield is greater than 95.0%, and the removal rate of thiane is greater than 93.0%.

Embodiment 2

[0016] Industrial naphthalene is raw material 500g, wherein contains thianne 1.3444%, does not meet other impurity, and the reaction reagent specification that adds is with embodiment 1, and wherein the molar number of hydrogen peroxide, formic acid, sulfuric acid is respectively 9.71, 1.06, 1.00 times of thianne, The reaction temperature is 80°C, and the reaction time is 60min. After the reaction, it is rectified by a rectification tower with 10 theoretical plates. The rate is greater than 96.5%, and the removal rate of thiane is greater than 95.0%.

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Abstract

The invention relates to a new process for preparing refined naphthalene from industrial naphthalene. The new process adopts combination of reaction and rectification, uses the industrial naphthalene as a raw material, hydrogen peroxide as an oxidant, organic acid and inorganic acid as catalysts; the mixture is subjected to chemical reaction at a temperature of between 80 and 110 DEG C for 10 to 80 minutes so that thianaphthene as a main impurity in the industrial naphthalene is oxidized to form sulfoxide or sulfones as a water-soluble oxidation product with high boiling point; water phase isseparated off; and organic phase is rectified to remove the residual oxidation product and other impurities to obtain the refined naphthalene with high impurity. The new process has the advantages that as the hydrogen peroxide, the organic acid and the inorganic acid have small consumption and thorough reaction and a reaction reagent is not needed to reclaim, the process course is simple; and theprocess of oxidation reaction has high selectivity, small loss of naphthalene and high course yield.

Description

technical field [0001] The invention belongs to the field of coal tar and fine chemicals, and relates to a process for preparing refined naphthalene from industrial naphthalene (also called crude naphthalene). Background technique [0002] The main impurity in existing industrial naphthalene is thioindenne, whose boiling point is very close to that of naphthalene and cannot be removed by rectification. Traditional methods include sulfuric acid formaldehyde method, hydrofining method, fractional crystallization method, solvent crystallization method, emulsification crystallization method, extractive distillation method, etc. The sulfuric acid method consumes a large amount of sulfuric acid, which causes the loss of naphthalene sulfonation and produces a large amount of waste liquid; the fractional crystallization method has huge equipment, high energy consumption, and low yield; the solvent crystallization method or emulsification crystallization method has low yield and cumb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C15/24C07C7/148C07C7/04
Inventor 熊杰明张丽萍
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY