A process and device for preparing phenolic resin from coal tar

A technology for phenolic resin and coal tar, 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: 2018-08-17
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 prematurely due to the high viscosity and the inability to stir, resulting in insufficient contact of the reaction substance with a low conversion rate of the reaction and uneven phenolic resin produced by the reaction, which increases the difficulty of separating the phenolic resin in the later stage, and it does not No specific method for separating phenolic resins is proposed
[0007] To sum up, there are few reports on the preparation of phenolic resins by the reaction of cheap phenolic substances in coal tar and aldehydes, and they are all in the laboratory research stage, and there are more or less problems

Method used

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  • A process and device for preparing phenolic resin from coal tar
  • A process and device for preparing phenolic resin from coal tar
  • A process and device 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 table

[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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PUM

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Abstract

A process and device for preparing phenolic resin based on coal tar, using toluene or benzene as a solvent, acid or alkali as a catalyst, coal tar or its distillation fractions and formaldehyde, benzaldehyde, paraformaldehyde and furfural under certain conditions to undergo phenolic polymerization Reaction, the reaction product is filtered through a closed drum vacuum filter to obtain phenolic resin, and at the same time, dephenolized coal tar containing solvent is obtained, and the dephenolized oil containing solvent is subjected to rectification to realize the separation of water and solvent, and the solvent is recovered. The solvent can be reused. This process uses cheap medium-low temperature coal tar with high phenol content to undergo phenolic polymerization reaction with aldehydes to prepare phenolic resin. The phenolic substances in medium-low temperature coal tar can be basically completely removed through one-step reaction, and the phenol removal step is simple. At the same time, the solvent is recycled, which is economical and environmentally friendly. It is a new coal tar processing method with simple process, low production and operation costs, significant economic benefits and easy industrialization.

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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Patent Type & Authority Patents(China)
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
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