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Method for extracting 2-methylquinoline from isoquinoline stillage residual liquor

A technology for methylquinoline and isoquinoline is applied in the field of extracting 2-methylquinoline from isoquinoline residue liquid, and can solve the problems of long extraction period, high requirements on raw materials, and difficulty in oil-water separation. , to achieve the effect of easy oil-water separation, high selectivity and fast reaction

Active Publication Date: 2015-07-22
HUANGHUA XINNUOLIXING FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In the traditional urea addition method, the 8-methylquinoline content in the raw materials used is less than 10%, and toluene is used as the solvent. The addition reaction takes 2-3 hours, and the adduct dissociation takes another 4-5 hours. The extraction cycle is too long. long, the extraction rate is only about 70%, and when the content of 8-methylquinoline in the raw material is above 10%, it is difficult to obtain 2-methylquinoline products with a content of ≥95% by this method
[0011] Chinese patent CN102372671 improves the traditional urea method by partially replacing toluene with ethanol as the reaction medium, which greatly improves the rate of addition reaction, but the selectivity of the addition agent is hardly improved, and there are still high requirements for raw materials
Moreover, due to the introduction of ethanol, while increasing the cost of solvent recovery, it also causes difficulties in the subsequent oil-water separation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The isoquinoline residue is crudely distilled to remove asphaltenes and other insoluble matter. The obtained fraction contained 12.3% of isoquinoline, 43.7% of 2-methylquinoline and 22.4% of 8-methylquinoline.

[0035] Get 3000g of fractions obtained by crude distillation as the raw material for extracting 2-methylquinoline, and dissolve them in 3500g of coal tar light oil fractions with a distillation range between 100-155°C. Add 1125 g of industrial urea aqueous solution with a mass fraction of 40% to the above system, and stir rapidly at room temperature for 30 minutes. After the white adduct formed by the reaction stopped increasing, the adduct was centrifuged, and the solid phase was rinsed twice with the above-mentioned light oil fraction, and then dried to obtain 1512 g of the adduct. The obtained adduct was added to a solvent system consisting of 1500 g of light oil fraction / 600 g of water, and 3.8 g of sodium lauryl sulfate was added to the system. After stir...

Embodiment 2

[0037] The isoquinoline residue is crudely distilled to remove asphaltenes and other insoluble matter. The obtained fraction contained 16.7% of isoquinoline, 38.1% of 2-methylquinoline and 15.6% of 8-methylquinoline.

[0038] Get 3000g of fractions obtained by crude distillation as the raw material for extracting 2-methylquinoline, and dissolve them in 3000g of phenol oil fractions with a distillation range between 170-190°C. Add 1200 g of industrial urea aqueous solution with a mass fraction of 30% to the above system, and stir rapidly at room temperature for 30 minutes. After the white adduct formed by the reaction stopped increasing, the adduct was centrifuged, and the solid phase was rinsed twice with the above phenol oil fraction, and then dried to obtain 1301 g of the adduct. The obtained adduct was added to a solvent system consisting of 1500 g of phenol oil fraction / 600 g of water, and 5.8 g of sodium lauryl sulfate was added to the system. After stirring evenly, hea...

Embodiment 3

[0040] The isoquinoline residue is crudely distilled to remove asphaltenes and other insoluble matter. The obtained fraction contained 14.2% of isoquinoline, 41.9% of 2-methylquinoline and 18.8% of 8-methylquinoline.

[0041] Get the cut 3000g that crude distillation obtains as the raw material of extracting 2-methylquinoline, be dissolved in the 3000g industrial n-butanol. Add 800 g of industrial urea aqueous solution with a mass fraction of 35% to the above system, and stir rapidly at room temperature for 30 minutes. After the white adduct formed by the reaction stopped increasing, the adduct was centrifuged, and the solid phase was rinsed twice with n-butanol, then dried to obtain 1442 g of the adduct. The obtained adduct was added to a solvent system consisting of 1500 g of n-butanol / 600 g of water, and 7.2 g of sodium lauryl sulfate was added to the system. After stirring evenly, heat the system to 90-95°C, keep warm and dissociate. After 40 minutes, the dissociation w...

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Abstract

The invention provides a method for extracting 2-methylquinoline from isoquinoline stillage residual liquor. The specific implementation method comprises the following steps: 1, coarsely distilling the isoquinoline stillage residual liquor and removing asphaltene and other insoluble substances; 2, dissolving fraction obtained by coarse distillation in a selected solvent, adding a fixed amount of a urea aqueous solution into the solvent, and quickly stirring for 30 minutes; 3, performing centrifugal separation on an obtained white adduct, leaching, and drying; 4, quickly decomposing the obtained adduct in the presence of a trace amount of a surfactant; 5, performing oil-water separation, and recovering an oil phase through the solvent to obtain 2-methylquinoline with the purity greater than 98%. The method greatly enhances the adduction capability of 2-methylquinoline and urea, improves the adduction reaction efficiency and the reaction selectivity, effectively eliminates an emulsification phenomenon during oil-water separation, and is free of three-waste emission and suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for separating and refining coal tar chemicals, in particular to a method for extracting 2-methylquinoline from isoquinoline residue. Background technique [0002] Existing 2--methylquinoline extraction process mainly contains four classes: [0003] 1. Salt forming method [0004] This method selects inorganic acid to react with quinoline substances in raw materials to form salts, and then utilizes the difference in solubility of each component in water or other mixed solvents after salt formation to achieve the purpose of purifying 2-methylquinoline. The phosphoric acid method disclosed in "Extraction of 2-Methylquinoline from Isoquinoline Residue" (Fuel and Chemical Industry, 2001, 33 (2), 99) by Li Jian et al. is such a method. This method is easy to operate and low in cost, but the extraction rate of 2-methylquinoline is low, and a large amount of oily phosphate wastewater will be produced. At present, coal chemi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/04
CPCC07D215/04
Inventor 孟励治李永廷周小野
Owner HUANGHUA XINNUOLIXING FINE CHEM
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