Device and process for preparing phenolic resin from coal tar

A technology of phenolic resin and coal tar, which is applied in the processing of tar, refining tar by chemical method, petroleum industry and other directions, can solve the problems of increasing the difficulty of separation of phenolic resin, uneven phenolic resin, low utilization rate of coal tar, etc. More uniform and complete reaction, lower viscosity and lower hydrogen consumption

Active Publication Date: 2017-03-29
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the method of patent CN1693331A, although coal tar is utilized in the preparation of phenolic resin, only a small amount of coal tar is used as a raw material for the production of modified phenolic resin in the preparation process, and coal tar is not mostly utilized. low utilization
[0006] The method of patent CN103289718A, though utilizes coal tar and aldehydes to produce phenolic resin, because in its reaction process, the coal tar under the heated state still has certain viscosity, adds that viscosity increases more after being polymerized with aldehydes Fast, the reaction will be stopped ...

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  • Device and process for preparing phenolic resin from coal tar
  • Device and process for preparing phenolic resin from coal tar
  • Device and process for preparing phenolic resin from coal tar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The method of heterogeneous polymerization is used for phenolic polymerization, using benzene or toluene as solvent, medium and low temperature coal tar as the raw material for phenol and aldehydes to react with aldehydes under the action of a catalyst to obtain dephenolized oil and phenolic resin, so as to achieve medium and low temperature Coal tar is used as raw material for the purpose of preparing phenolic resin. In order to illustrate the actual effect of the present invention, the components of medium and low temperature coal tar and dephenolized oil were determined by gas chromatography-mass spectrometry.

[0051] Select medium and low temperature coal tar heavy oil and formaldehyde solution (37wt%) as reactants, toluene as solvent, and concentrated sulfuric acid with a mass fraction of 98% as catalyst, wherein the mass ratio of medium and low temperature coal tar heavy oil to formaldehyde is 1:0.97, and medium and low temperature The mass ratio of coal tar heav...

Embodiment 2

[0057] Choose medium and low temperature coal tar heavy oil > 300 ℃ distillate and formaldehyde solution (37wt%) as reactant, toluene is solvent, NaOH solution (40wt%) is catalyst, wherein, low temperature coal tar heavy oil > 300 ℃ distillate and formaldehyde The mass ratio of low-temperature coal tar heavy oil >300°C to solvent is 1:5, and the mass ratio of low-temperature coal tar heavy oil >300°C to catalyst is 1:0.18. The reaction temperature in the tar reactor 5 is 40-90° C., and the reaction time is 1.5-2 hours. After the above process was completed, the product (mainly dephenolized oil) was analyzed by gas chromatography-mass spectrometry, and the phenolic resin was analyzed by infrared spectroscopy, see Figure 4 , Figure 5 and Table 3.

[0058] In Table 3, the low-temperature coal tar heavy oil > 300 ° C fraction and its dephenolized oil (alkali-catalyzed) part of the composition list

[0059]

[0060] combine Figure 4 , Figure 5 From the results in Table ...

Embodiment 3

[0062] Select medium and low temperature coal tar heavy oil >300°C fraction and benzaldehyde as reactants, toluene as solvent, and p-toluenesulfonic acid as catalyst, wherein the mass ratio of medium and low temperature coal tar heavy oil >300°C fraction to benzaldehyde is 1:1.2, The mass ratio of medium and low temperature coal tar heavy oil >300°C fraction to solvent is 1:10, the mass ratio of medium and low temperature coal tar heavy oil >300°C fraction to catalyst is 1:0.1, the reaction temperature is controlled at 140-180°C, and the reaction time is 4~6h. After the above process was completed, the product (mainly dephenolized oil) was analyzed by gas chromatography-mass spectrometry, see Figure 4 , Figure 7 , Table 2 and Table 4.

[0063] Partial composition of dephenolized oil (benzaldehyde, acid catalyzed) fraction of low temperature coal tar heavy oil >300°C in Table 4

[0064]

[0065] combine Figure 4 with Figure 7 , Table 3 and Table 4, it was found that...

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Abstract

The invention discloses a device and a process for preparing phenolic resin from coal tar. The process includes: taking methyl benzene or benzene as a solvent, taking acid or alkaline as a catalyst, subjecting the coal tar or distillation fractions thereof to phenolic polymerization reaction with formaldehyde, benzaldehyde, paraformaldehyde and furfural under certain conditions, filtering reaction products through a closed rotary drum vacuum filter to obtain the phenolic resin as well as solvent-containing dephenolized coal tar, rectifying the solvent-containing dephenolized coal tar to realize separation of water and the solvent, and recover the solvent to realize solvent recycling. Cheap medium-and low-temperature coal tar high in phenol content is adopted for phenolic polymerization reaction with aldehydes to prepare the phenolic resin, and phenolic substances in the medium-and low-temperature coal tar can be completely removed by further reaction. Therefore, phenol removal steps are simple, solvent recycling is realized, economy and environment friendliness are achieved, and a novel coal tar processing method simple in process, low in production operation cost, remarkable in economic benefit and easy for industrialization is provided.

Description

technical field [0001] The invention relates to the technical field of coal tar processing, in particular to a process and a device for preparing phenolic resin from coal tar. Background technique [0002] With the gradual reduction of world petroleum resources, coal tar, as a valuable chemical raw material, is becoming increasingly prominent. For medium and low temperature coal tar with more phenol content, it is mainly produced by the low temperature pyrolysis process of coal, which is mainly composed of neutral compounds (aliphatic hydrocarbons and aromatic hydrocarbons), acidic compounds (mainly 30% to 40% phenolic content) , oxygen-containing and sulfur-containing compounds (very small amount). Phenolic compounds (especially phenol and cresol) are widely used in industry, agriculture, national defense, medicine and health, etc. For coal tar with a very complex composition, the current traditional methods for the separation and transformation of phenolic compounds in c...

Claims

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Application Information

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IPC IPC(8): C08G8/08C08G8/04C08G8/06C10C1/00C10C1/20
CPCC08G8/04C08G8/06C08G8/08C10C1/00C10C1/20C10C1/205
Inventor 孙鸣何超唐星冯新娟张丹马晓迅徐龙郝青青
Owner NORTHWEST UNIV(CN)
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