CN101220284A - A kind of preparation method of electrode impregnation pitch - Google Patents

Abstract

A method for preparing electrode-impregnated asphalt, which uses medium-temperature asphalt as a raw material and dephenolized phenol oil as a solvent, and undergoes three treatments of heating and dissolving, vacuum filtration, and solvent distillation recovery to remove quinoline insolubles in the medium-temperature asphalt, Thereby, an electrode impregnation pitch product with less than 0.1% weight of quinoline insoluble matter can be obtained. The electrode impregnated asphalt yield of the present invention can reach more than 80%; the used dephenolized phenolic oil solvent can be used again, and the filter cake can be treated as heavy asphalt; the whole production process requires less equipment, the process is simple and easy to control, the process is less, and the effect is high. Good; based on the annual processing of 5,000 tons of medium-temperature asphalt, 4,000 tons of electrode-impregnated asphalt can be produced, which is an effective method for coal tar asphalt processing.

Description

A kind of preparation method of electrode impregnation pitch

technical field

The invention belongs to the field of coal chemical industry, and in particular relates to a method for preparing electrode-impregnated asphalt by using medium-temperature asphalt.

Background technique

The preparation method of electrode impregnated asphalt is divided into coal tar, soft asphalt, medium temperature asphalt and so on according to the production raw materials. According to the production method, there are coal tar filtration method, coal tar solvent extraction method, coal tar (soft pitch) thermal polymerization method, coal tar pitch solvent precipitation method, and medium temperature pitch solvent filtration method. The key to the production of electrode impregnated asphalt by using medium-temperature pitch is to remove the content of quinoline insolubles. There are several methods for removing quinoline insolubles.

Static sedimentation separation: mainly rely on gravity sedimentation to separate the contained impurities. This method is characterized by small investment and simple process, but poor purification effect.

Centrifugal separation: Use a high-speed centrifuge to centrifugally remove the insoluble matter of primary quinoline. The equipment is huge, the metal consumption is large, and the energy consumption is high.

Hot-melt filtration: First, melt the material in the kettle for coarse filtration. The coarse filter kettle is equipped with a heating furnace, a pressure valve, and a vent valve; then use high-efficiency filter materials to filter the coarsely filtered raw materials into the fine filter kettle. The process is simple, but the filter screen is demanding.

Solvent extraction: Solvent extraction is carried out after adding solvent. This method has small investment and good purification effect, but the amount of solvent is large and the yield is low.

At present, the production of electrode impregnated pitch in our country is still in the stage of development and trial production, and the method of producing electrode impregnated pitch with medium temperature asphalt has not yet been industrialized. Therefore search, as yet identical with the present invention or similar patent document and relevant data report.

Contents of the invention

The purpose of the present invention is to provide a method with low investment, quick effect, simple process, which can effectively remove the quinoline content in medium-temperature asphalt, so as to obtain high-quality electrode-impregnated asphalt.

For this reason, the technical solution that the present invention takes is:

The method for preparing electrode-impregnated asphalt of the present invention adopts medium-temperature asphalt as a raw material, and uses dephenolized phenolic oil as a solvent, and undergoes three processes of heating and dissolving, vacuum filtration, and solvent distillation recovery to remove quinoline insolubles in the medium-temperature asphalt, Thus, an electrode-impregnated pitch product is obtained. The specific operation steps are:

1. Heating and dissolving: Mix the medium-temperature asphalt and dephenolized phenolic oil solvent at a ratio of 1:2 to 5, then heat, keep the dissolving temperature between 70°C and 110°C, and continuously stir until the medium-temperature asphalt is completely dissolved in the dephenolized phenolic oily solvent Medium; then heat on low heat, dissolve for 10 to 30 minutes, then stop heating;

2. Vacuum suction filtration: After cooling the hot mixed solution to 15-45°C at room temperature, slowly pour it into the funnel of the pre-installed vacuum suction filtration device, and carry out vacuum suction filtration while pouring, and the filtrate after suction filtration poured into a copper pot;

3. Solvent distillation recovery: distill the filtrate in the copper pot under reduced pressure, keep the final temperature of distillation at 160°C-230°C, and the distillate is a solvent, which can be reused; The sample is the electrode impregnated pitch. And the weight of the quinoline insoluble matter in the electrode impregnated asphalt is less than 0.1%.

The beneficial effect of the preparation method of electrode impregnated pitch of the present invention is:

First, the yield is high. After medium-temperature asphalt treatment, the yield of the electrode-impregnated asphalt can reach more than 80%. Second, the utilization rate is high. The used dephenolized phenolic oil solvent can be fully recovered and reused, and the filter cake produced after filtration It can be treated as heavy asphalt; third, the processing efficiency is high, the equipment required for the whole production process is not much, the process method is easy to master and control, there are few procedures, and the effect is good; fourth, the comprehensive benefits are considerable, coal tar pitch is separated from coal tar in the process of processing The bulk products produced account for about 50-60% of the total amount of coal tar. Based on the annual processing of 5,000 tons of medium-temperature pitch and a yield of 80%, 4,000 tons of electrode-impregnated pitch can be produced each year. an effective way.

Detailed ways

The present invention will be further described below in conjunction with embodiment.

The method for preparing electrode-impregnated asphalt of the present invention uses medium-temperature asphalt as a raw material, uses dephenolized phenolic oil as a solvent, and undergoes three processes of heating and dissolving, vacuum filtration, and solvent distillation recovery, thereby producing quinoline insolubles with a weight less than 0.1% Electrode impregnated pitch products.

Example 1:

Mix the medium-temperature asphalt and the dephenolized phenolic oil solvent in a ratio of 1:2, heat the mixture after mixing, and stir continuously to keep the dissolution temperature at 110°C, so that all the medium-temperature asphalt is dissolved in the dephenolized phenolic oil solvent; then Take low heat to heat, after dissolving for 10 minutes, stop heating.

After cooling the hot mixed solution to 15°C at room temperature, slowly pour it into the funnel of the pre-installed vacuum filtration device, perform vacuum filtration while pouring, and pour the filtered filtrate into a copper pot.

The filtrate in the copper pot was distilled under reduced pressure, and the final distillation temperature was 230°C. The distillate is dephenolized phenol oil solvent, which is recovered for reuse. After distillation, the sample poured out from the bottom of the kettle can obtain quinoline insoluble matter with a weight less than 0.1% electrode impregnation pitch.

Example 2:

Mix the medium-temperature asphalt and the dephenolized phenolic oil solvent in a ratio of 1:5, heat the mixture after mixing, and stir continuously, keeping the dissolution temperature at 70°C, so that all the medium-temperature asphalt is dissolved in the dephenolized phenolic oil solvent; then Take low heat to heat, after dissolving for 30 minutes, stop heating.

After cooling the hot mixed solution to 45°C at room temperature, slowly pour it into the funnel of the pre-installed vacuum filtration device, perform vacuum filtration while pouring, and pour the filtered filtrate into a copper pot.

The filtrate in the copper pot was distilled under reduced pressure, and the final distillation temperature was 160°C. The distillate is dephenolized phenol oil solvent, which is recovered for reuse. After distillation, the sample poured out from the bottom of the kettle can obtain quinoline insoluble matter with a weight less than 0.1% electrode impregnation pitch.

Claims (2)

1. the preparation method of an electrode impregnating pitch, the employing mid-temperature pitch is a raw material, it is characterized in that, and with the removal phenol carbolic oil solvent, reclaim three processing removing the quinoline insolubles in the mid-temperature pitch through heating for dissolving, vacuum filtration, solvent distillation, thereby make electrode impregnating pitch product; Its concrete operations step is:

(1), heating for dissolving: mid-temperature pitch is mixed post-heating with the removal phenol carbolic oil solvent by 1: 2～5, keep solvent temperature between 70 ℃～110 ℃, and be continuously stirring to mid-temperature pitch and all be dissolved in the removal phenol carbolic oil solvent; Take little fire heating then, dissolve after 10～30 minutes, stop heating;

(2), vacuum filtration: after hot mixing solutions at room temperature is cooled to 15～45 ℃, slowly pour in the funnel of mounted in advance vacuum filtration device, carry out vacuum filtration while pour into, the filtrate behind the suction filtration is poured in the Copper Pot;

(3), the solvent distillation is reclaimed: the filtrate in the Copper Pot is distilled under the mode of decompression, distill whole temperature and remain on 160 ℃～230 ℃, distillate is solvent, and is reusable; The sample of pouring out at the bottom of the kettle of distillation back is the electrode impregnating pitch.

2. the preparation method of electrode impregnating pitch according to claim 1 is characterized in that, quinoline insolubles weight is less than 0.1% in the described electrode impregnating pitch.