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Method for extracting and separating neutral nitride in coal tar by utilizing non-toxic biodegradable ionic liquid

An ionic liquid, biodegradation technology, applied in the direction of organic chemistry, can solve the problems of by-product generation, high toxicity, poor degradability, etc., to achieve the effect of recycling, high selective separation, and increased energy consumption

Pending Publication Date: 2022-03-01
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The shortcomings and deficiencies in the extraction and separation of neutral nitrides in the prior art are: the ionic liquid used in the separation is synthesized by a multi-step method, the steps are cumbersome, and the energy consumption is high; there are by-products, and the utilization rate of atoms is low; The solvent is used for washing, which does not meet the green chemistry initiative, and the synthesis cost of ionic liquid is high
In the prior art, the cations of the ionic liquids (ILs) used are mostly imidazole rings. According to current research, the toxicity of the ionic liquids of the imidazole rings is high, and increases with the increase of the alkyl chain length. Due to the current use of ILs The degradability of ILs is poor, and ILs may accumulate in the environment and cause pollution to the environment
Moreover, the removal rate and extraction and separation effect of the existing methods are not good for neutral nitrides

Method used

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  • Method for extracting and separating neutral nitride in coal tar by utilizing non-toxic biodegradable ionic liquid
  • Method for extracting and separating neutral nitride in coal tar by utilizing non-toxic biodegradable ionic liquid
  • Method for extracting and separating neutral nitride in coal tar by utilizing non-toxic biodegradable ionic liquid

Examples

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Effect test

Embodiment 1

[0045] A method for extracting and separating neutral nitrogen compounds in coal tar by using nontoxic and biodegradable ionic liquids, comprising the steps of:

[0046] (1) Weigh the tetramethylguanidine and acetic acid used in the synthesis of the ionic liquid at a molar ratio of 1:1.2. First put tetramethylguanidine and tetramethylguanidine 3 times the volume of solvent n-hexane (tetramethylguanidine and solvent are completely miscible) into a round bottom flask, place in a magnetic stirring constant temperature water bath, set the initial temperature to 25 °C, stirring continuously to mix well. Under the condition of stirring, add the acid drop by drop into the round bottom flask through the constant pressure dropping funnel, at the beginning the dropping rate is 0.1-0.2ml / min. Adjust the rate to 0.5-1ml / min, and after adding 1 / 3 of the total mass of the acid, adjust the rate of addition to 2-6ml / min until the addition is completed. After completion, the tetramethylguani...

Embodiment 2

[0056]A method utilizing non-toxic biodegradable ionic liquid to extract and separate neutral nitrogen compounds in coal tar, as described in Example 1, the difference is: simulated oil I is replaced by simulated oil II; other steps and conditions and implementation Example 1 is consistent.

[0057] The preparation steps of simulated oil II (replacing anthracene oil) include: configure base oil according to the mass ratio of toluene:n-heptane=1:1, dissolve 1.5g carbazole and 1-3g N-methylpyrrolidone in 100g base oil Take the supernatant to obtain simulated oil II.

[0058] In this embodiment, the extraction efficiency of the neutral nitrogen compound carbazole is 99.12%, the recovery rate of the neutral nitrogen compound is 99.10%, and the recovery rate of the extraction agent tetramethylguanidine-based ionic liquid is 100.00%.

Embodiment 3

[0060] A method for extracting and separating neutral nitrogen compounds in coal tar by using nontoxic and biodegradable ionic liquids, comprising the steps of:

[0061] (1) Weigh tetramethylguanidine and formic acid used in the synthesis of ionic liquids in a molar ratio of 1:1.2. First put tetramethylguanidine and tetramethylguanidine 3 times the volume of solvent n-hexane (tetramethylguanidine and solvent are completely miscible) into a round bottom flask, place in a magnetic stirring constant temperature water bath, set the initial temperature to 25 °C, stirring continuously to mix well. Under the condition of stirring, add the acid drop by drop into the round bottom flask through the constant pressure dropping funnel, at the beginning the dropping rate is 0.1-0.2ml / min. Adjust the rate to 0.5-1ml / min, and after adding 1 / 3 of the total mass of the acid, adjust the rate of addition to 2-6ml / min until the addition is completed. After completion, the tetramethylguanidine-ba...

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Abstract

The invention provides a method for extracting and separating neutral nitrides in coal tar by utilizing non-toxic biodegradable ionic liquid. One or a combination of more than two of n-hexane, n-heptane, n-octane or n-dodecane is used as a solvent, and the non-toxic biodegradable tetramethylguanidyl ionic liquid is synthesized by a one-step method; and extracting and separating to obtain the neutral nitride through three-stage counter-current extraction, back extraction and reduced-pressure flash evaporation processes by taking the neutral nitride as an extracting agent. The tetramethylguanidyl ionic liquid is non-toxic, biodegradable, simple to synthesize, high in yield and purity, low in energy consumption, low in cost, small in waste liquid generation amount, green and environment-friendly. According to the method, the removal rate of high-boiling-point neutral nitrides in the wash oil and the anthracene oil is greatly increased, the excellent extraction and separation effect is achieved, and the extraction efficiency is high. The extraction and separation process is simple, and the device is reasonable; the nontoxic biodegradable tetramethylguanidyl ionic liquid is high in recovery rate and purity, can be recycled, and is safe and environment-friendly.

Description

technical field [0001] The invention relates to a method for extracting and separating neutral nitrogen compounds in coal tar by using a non-toxic and biodegradable ionic liquid, and belongs to the technical field of coal chemical separation. Background technique [0002] Coal tar is a by-product of coal coking, also known as coal pyrolysis oil, and is the main raw material of coal chemical industry. Coal tar includes a variety of heteroatom compounds, including phenolic compounds, nitrogen-containing compounds, sulfur-containing compounds, neutral aliphatic and aromatic compounds. Among them, nitrogen-containing compounds are mainly weakly basic pyridine, quinoline and their derivatives, as well as neutral compounds such as indole and carbazole. Among them, indole, which accounts for about 75% of the total content, is concentrated in the washing oil fraction, and indole and its derivatives are the main substances of resinization reaction due to their active nature. Due to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/06C07D209/84
CPCC07D209/06C07D209/84
Inventor 徐冬梅张涛马艺心高军张连正赵萍萍张治山
Owner SHANDONG UNIV OF SCI & TECH
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