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A kind of method that takes coal tar pitch as raw material to prepare benzene carboxylic acid

A technology for coal tar and benzene carboxylic acid, applied in the field of preparing benzene carboxylic acid, can solve the problems of high production cost, large investment, high purity of raw materials, and extremely high requirements on equipment materials, and achieves the effect of improving polarity and promoting contact

Active Publication Date: 2021-04-02
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this preparation process has harsh conditions, high requirements on raw material purity and equipment materials, large investment, high production cost, low reaction selectivity, and easy deactivation of catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This example illustrates that coal tar pitch taken from Datuhe Coking Plant in Shanxi Province is used as raw material (particle size <0.15mm). Take 10 g of coal tar pitch and perform Soxhlet extraction with 100 mL of methanol until the extract in the capillary is colorless. stop. The obtained raffinate was placed in a tube furnace, ventilated with air, and heated at 200 °C for 1 h to obtain a solid pyrolysis pretreated product. The solid pyrolysis pretreatment product is crushed through a 100-mesh sieve (particle size <0.15mm), and subjected to alkali-oxygen oxidation reaction. Take 2 g of sample, 10 g of sodium hydroxide, and 100 mL of deionized water in 300 mL of high-temperature and high-pressure reaction In the reactor, fill in oxygen to replace the air in the reactor, and finally fill in oxygen with an initial pressure of 5.0 MPa. Put the reaction kettle into the heating furnace, turn on the stirring, control the stirring speed to 400 r / min, wait for the temperat...

Embodiment 2

[0023] This example illustrates that coal tar pitch taken from Datuhe coking plant in Shanxi Province is used as raw material (particle size <0.15mm), and 10 g of coal tar pitch is used for 150 mL methanol and ethanol mixed solution (methanol: ethanol = 1:1). Soxhlet extraction was stopped when the extract in the capillary was colorless. The obtained raffinate was placed in a tube furnace, ventilated with air, and heated at 250 °C for 1 h to obtain a solid pyrolysis pretreated product. The solid pyrolysis pretreatment product is crushed through a 100-mesh sieve (particle size <0.15mm), and subjected to alkali-oxygen oxidation reaction. Take 2 g of sample, 8 g of sodium hydroxide, and 100 mL of deionized water in 300 mL of high-temperature and high-pressure reaction In the reactor, fill in oxygen to replace the air in the reactor, and finally fill in oxygen with an initial pressure of 6.0 MPa. Put the reaction kettle into the heating furnace, turn on the stirring, control the ...

Embodiment 3

[0025] This example illustrates that coal tar pitch obtained from Shanxi Jinyao Coking Co., Ltd. is used as raw material (particle size <0.15mm), 10 g of coal tar pitch is taken, and Soxhlet extraction is performed with 80 mL of ethanol. When the extract in the capillary is colorless stop. The obtained raffinate was placed in a tube furnace, ventilated with air, and heated at 300 °C for 0.5 h to obtain a solid pyrolysis pretreated product. The solid pyrolysis pretreatment product is crushed through a 100-mesh sieve (particle size <0.15mm), and subjected to alkali-oxygen oxidation reaction. Take 2 g of sample, 2 g of sodium hydroxide, and 100 mL of deionized water in 300 mL of high temperature and high pressure In the reactor, fill in oxygen to replace the air in the reactor, and finally fill in oxygen with an initial pressure of 4.0 MPa. Put the reaction kettle into the heating furnace, turn on the stirring, control the stirring speed to 400 r / min, wait for the temperature to...

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PUM

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Abstract

The invention relates to a method for preparing phenyl monocarboxylic acid from a raw material of coal tar pitch. The method is characterized by comprising the following steps: firstly, utilizing an organic solvent of alcohol of C2 or below to extract the coal tar pitch to obtain an extractive; then performing pyrolysis pretreatment on the extractive under the circulating air atmosphere; then breaking an obtained solid pyrolysis pretreatment product, putting into a high-temperature high-pressure reaction kettle, adding sodium hydroxide and deionized water, inflating oxygen with certain initialpressure, performing oxidative degradation reaction under the stirring condition, filtering after the reaction finishes, acidifying filtrate by diluted hydrochloric acid, removing insoluble precipitate and then performing reduced pressure evaporation to remove moisture to obtain a product of phenyl monocarboxylic acid with a concentration larger than 60%. By means of the method disclosed by the invention, the concentration of the phenyl monocarboxylic acid in the insoluble product can reach 60% or more; a yield of the phenyl monocarboxylic acid can reach 20% or more with the mass of a sampleused by the oxidizing degradation as the baseline.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemicals, and in particular relates to a method for preparing benzenecarboxylic acid from coal tar pitch. Background technique [0002] Benzene carboxylic acid is an important fine chemical, currently it is mainly obtained from the oxidation of alkylbenzenes produced in the petrochemical industry. However, my country's petroleum resources are scarce, and the supply of petroleum resources in the world has become increasingly tense in recent years. Therefore, it is of great practical significance to develop a route for preparing benzenecarboxylic acid from coal-based raw materials. The output of coal tar pitch in my country is huge, but the utilization status is not optimistic. Coal tar pitch is rich in aromatic ring structures, which can be considered as an important raw material for the production of benzenecarboxylic acid. [0003] At present, the preparation of benzenecarboxylic a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/21C07C63/00
CPCC07C51/21C07C63/00
Inventor 王玉高申峻牛泽世刘刚牛艳霞盛清涛
Owner TAIYUAN UNIV OF TECH