Petroleum-based impregnant asphalt as well as preparation method and application thereof

Abstract

The invention relates to petroleum-based impregnant asphalt as well as a preparation method and application thereof, and belongs to the technical field of asphalt. The technical problem that an existing impregnant asphalt preparation method seriously pollutes the environment is solved. The preparation method comprises the following steps: firstly, carrying out reduced pressure distillation on the ethylene tar, and removing light components in the ethylene tar to obtain heavy components of the ethylene tar; then in an inert atmosphere, carrying out polymerization reaction on the ethylene tar heavy component, a catalyst and a cross-linking agent, and cooling to obtain petroleum-based impregnant asphalt; wherein the cross-linking agent is one or more of 1-naphthaldehyde and 2-naphthaldehyde, and the mass percent of the cross-linking agent, the mass percent of the catalyst and the mass percent of the ethylene tar heavy component are 3%-8%, 2% and 90%-95% respectively. The preparation method is simple in technological process, high in controllability, capable of achieving continuous production and suitable for industrialization; the prepared impregnant is appropriate in asphalt softening point, high in toluene insoluble and coking value, low in quinoline insoluble content and ash content and capable of being used for preparing carbon material electrodes.

Description

Technical Field

[0001] The present invention belongs to the technical field of asphalt, and particularly relates to a petroleum-based impregnating pitch, a preparation method and an application thereof, and more particularly to the application of the petroleum-based impregnating pitch in the preparation of carbon material electrodes. Background Art

[0002] Ethylene tar is a by-product of the industrial ethylene cracking production process. Its yield varies with different process conditions, and the output accounts for about 10% - 15% of the ethylene output. At present, the domestic ethylene production industry has a large scale and a relatively large output of ethylene tar, but the utilization rate of ethylene tar is relatively low. It is mainly used as fuel such as ship fuel oil, and part of it is used to prepare materials such as needle coke and resin.

[0003] Carbon material electrodes are a kind of high-temperature-resistant graphite conductive materials, which have relatively high density and flexural strength, relatively low effective resistance, relatively few pore numbers, and low ash content. Among them, the performance indicators of high-power and ultra-high-power graphite electrodes are very strict, and they are mainly used for producing steel materials for electric arc furnaces, ladle furnaces and smelting furnaces. At present, the production method of carbon material electrodes is to subject the carbon material blank to high-temperature roasting, so that it undergoes a thermal decomposition reaction, and the generated gas volatilizes and escapes, forming a large number of pores to obtain the carbon material electrode. However, the structure of this carbon material electrode is porous, so its physical properties are poor. In the prior art, this problem is solved by impregnating and densifying the carbon material electrode with impregnating pitch, that is, under certain conditions such as temperature and pressure, the impregnating pitch is liquefied and penetrates into the interior of the carbon material blank and diffuses, filling the open pores of the carbon material electrode, reducing the porosity of the carbon material electrode, lowering the permeability of the carbon material electrode, and improving its bulk density, flexural strength, corrosion resistance and oxidation resistance.

[0004] In the prior art, impregnating pitch is mainly produced from coal tar pitch as raw material. However, coal tar pitch contains a large amount of toxic polycyclic aromatic hydrocarbons, and the pollution emissions are relatively serious, which also causes damage to human health. Therefore, it is urgent to develop an impregnating pitch with less environmental pollution. Summary of the Invention

[0005] In view of this, the purpose of the present invention is to solve the technical problem that the preparation method of impregnating pitch in the prior art causes serious environmental pollution, and to provide a petroleum-based impregnating pitch, a preparation method and an application thereof. The preparation method of the present invention has a simple process flow, high controllability, and can be continuously produced, which is suitable for industrialization; the prepared impregnating pitch has an appropriate softening point, high toluene insoluble matter and coking value, low quinoline insoluble matter content and low ash content, and can be used to prepare carbon material electrodes.

[0006] The present invention realizes the above purpose through the following technical solutions.

[0007] The present invention provides a preparation method of a petroleum-based impregnating pitch, comprising the following steps:

[0008] 1) Subject the ethylene tar to vacuum distillation to remove the light components in the ethylene tar, obtaining a heavy fraction of ethylene tar;

[0009] 2) Under an inert atmosphere, carry out a polymerization reaction on the heavy fraction of ethylene tar, a catalyst and a crosslinking agent, and cool to obtain the petroleum-based impregnating pitch;

[0010] The crosslinking agent is one or more of 1-naphthaldehyde and 2-naphthaldehyde, the catalyst is p-toluenesulfonic acid, and the mass percentages of the crosslinking agent, the catalyst and the heavy fraction of ethylene tar are 3% - 8%, 2% and 90% - 95% respectively.

[0011] Preferably, the quinoline insoluble content of the ethylene tar is 0 - 0.03 wt%, the toluene insoluble content is 0.01 wt% - 0.05 wt%, and the ash content is 0 - 0.01 wt%.

[0012] Preferably, the temperature of the vacuum distillation is 150 - 200 °C, the heating rate is 5 - 10 °C / min, the vacuum degree is 40 - 90 mmHg, and the time is 3 - 5 h; and the vacuum distillation is carried out under stirring, and the stirring speed is 200 - 300 rpm;

[0013] More preferably, the temperature of the vacuum distillation is 170 °C, the heating rate is 5 °C / min, the vacuum degree is 40 mmHg, the time is 5 h, and the stirring speed is 200 rpm.

[0014] Preferably, the softening point of the heavy fraction of ethylene tar is 70 - 90 °C, the quinoline insoluble content is 0 - 0.05 wt%, the coking value is 28 wt% - 35 wt%, and the carbon-hydrogen element ratio is 1.15 - 1.25.

[0015] Preferably, the inert atmosphere is nitrogen.

[0016] Preferably, the mass percentages of the crosslinking agent, the catalyst and the heavy fraction of ethylene tar are 5%, 2% and 93% respectively.

[0017] Preferably, the temperature of the polymerization reaction is 150 - 180 °C, the heating rate is 5 - 10 °C / min, and the time is 1 - 3 h; and the polymerization reaction is carried out under stirring, and the stirring rate is 200 - 300 rpm;

[0018] More preferably, the temperature of the polymerization reaction is 160 °C, the heating rate is 5 °C / min, the time is 2 h, and the stirring rate is 300 rpm.

[0019] The present invention also provides a petroleum-based impregnating pitch prepared by the preparation method of the above-mentioned petroleum-based impregnating pitch.

[0020] Preferably, the softening point of the petroleum-based impregnating agent is 85-95 °C, the quinoline insoluble content is 0.01 wt% - 0.1 wt%, the toluene insoluble content is 20 wt% - 30 wt%, the coking value is 50 wt% - 54 wt%, and the ash content is 0.01 wt% - 0.04 wt%.

[0021] The present invention also provides the application of the above-mentioned petroleum-based impregnating pitch in the preparation of carbon material electrodes.

[0022] The principle of the present invention is as follows: Through the molecular structure characterization of ethylene tar and impregnating pitch, it is determined that the average structure of the petroleum-based impregnating pitch is a short-side-chain aromatic hydrocarbon compound with 3-4 rings, and the heavy fraction of ethylene tar after removing the light components is a short-side-chain aromatic hydrocarbon compound with 2 or more rings. Therefore, the petroleum-based impregnating pitch can be prepared by a moderate polycondensation reaction using the heavy fraction of ethylene tar as the raw material. Furthermore, the present invention uses p-toluenesulfonic acid as a catalyst and naphthaldehyde as a cross-linking agent to carry out a catalytic cross-linking reaction on the heavy fraction of ethylene tar. The reaction is stable and the degree of polymerization is controllable. During the reaction, naphthaldehyde generates a naphthylmethyl cation under the catalysis of a protonic acid, attacks the aromatic hydrocarbon molecule with a higher electron cloud density, and undergoes an electrophilic substitution reaction to generate a polycyclic aromatic hydrocarbon molecule, thus obtaining the petroleum-based impregnating pitch.

[0023] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0024] (1) For the petroleum-based impregnating pitch prepared by the present invention, the quinoline insoluble content is less than 0.04%, which is much lower than that of the commercially available mainstream impregnating pitch.

[0025] (2) For the petroleum-based impregnating pitch prepared by the present invention, the softening point is appropriate, the toluene insoluble content is high, it has strong fluidity at high temperatures, and the residual pitch coke content is high after high-temperature roasting. It has an excellent impregnation and compaction effect on the carbon material green body and can be used for the preparation of carbon material electrodes.

[0026] (3) For the preparation method of the petroleum-based impregnating pitch of the present invention, the raw material used is ethylene tar, which is a by-product of the ethylene cracking industry. At present, the reserves of ethylene tar in China are abundant. Using it to prepare impregnating pitch effectively improves the additional utilization value of ethylene tar and broadens the domestic process route for the production of impregnating pitch, solving the current production dilemma of only coal-based impregnating pitch in China. Description of the Drawings

[0027] To more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0028] Figure 1 It is the viscosity change curves of the coal-based impregnating pitch of the prior art and the petroleum-based impregnating pitch of Embodiment 1 of the present invention at different temperatures.

[0029] Figure 2 It is the permeability change curves of the coal-based impregnating pitch of the prior art and the petroleum-based impregnating pitch of Embodiment 1 of the present invention at different temperatures. Detailed implementation manners

[0030] To further understand the present invention, the following describes the preferred implementation schemes of the present invention. However, it should be understood that these descriptions are only for further explaining the features and advantages of the present invention, rather than limiting the claims of the present invention.

[0031] The preparation method of the petroleum-based impregnating pitch of the present invention includes the following steps:

[0032] 1) Place the ethylene tar in a vacuum distillation device, carry out vacuum distillation, and remove the light components in the ethylene tar to obtain the ethylene tar heavy fraction;

[0033] 2) Under an inert atmosphere, place the ethylene tar heavy fraction, catalyst and cross-linking agent in a reaction kettle (atmospheric pressure), carry out a polymerization reaction, and cool to obtain the petroleum-based impregnating pitch.

[0034] In the above technical solution, the ethylene tar is mainly a multi-aromatic hydrocarbon compound composition system. It is a viscous fluid at room temperature, has a relatively high carbon-hydrogen ratio, a short side chain structure in the molecular structure composition, and low ash content, quinoline insoluble matter and heavy metal content. In this embodiment, it is preferred that the quinoline insoluble matter content of the ethylene tar is 0 to 0.03 wt%, the toluene insoluble matter content is 0.01 wt% to 0.05 wt%, and the ash content is 0 to 0.01 wt%.

[0035] In the above technical solution, the process conditions of the vacuum distillation are preferably: the temperature is 150 to 200 °C, the heating rate is 5 to 10 °C / min, the vacuum degree is 40 to 90 mmHg, and the time is 3 to 5 h; and the vacuum distillation is preferably carried out under stirring, and the stirring speed is 200 to 300 rpm.

[0036] In the above technical solution, the softening point of the ethylene tar heavy fraction prepared in step (1) is 70-90 °C, the quinoline insoluble content is 0-0.05 wt%, the coking value is 28 wt% - 35 wt%, and the carbon-hydrogen element ratio is 1.15 - 1.25.

[0037] In the above technical solution, the inert atmosphere is preferably nitrogen. However, it should be noted that there is no special limitation, and other inert atmospheres well-known to those skilled in the art can also be used.

[0038] In the above technical solution, the crosslinking agent is one or more of 1-naphthaldehyde and 2-naphthaldehyde, and the catalyst is p-toluenesulfonic acid. During the reaction, naphthaldehyde generates naphthylmethyl cations under the catalysis of protonic acid, attacks the aromatic hydrocarbon molecules with higher electron cloud density, and undergoes electrophilic substitution reaction to generate polycyclic aromatic hydrocarbon molecules, thus obtaining petroleum-based impregnating pitch. Moreover, the mass percentages of the crosslinking agent, catalyst, and ethylene tar heavy fraction are 3% - 8%, 2%, and 90% - 95% respectively, and petroleum-based impregnating pitch is prepared through a moderate polycondensation reaction.

[0039] In the above technical solution, the process conditions of the polymerization reaction are preferably: the temperature is 150 - 180 °C, the heating rate is 5 - 10 °C / min, and the time is 1 - 3 h; and the polymerization reaction is preferably carried out under stirring, and the stirring rate is 200 - 300 rpm.

[0040] In the above technical solution, when the following conditions are met, the properties of the obtained petroleum-based impregnating pitch are the best: the temperature of vacuum distillation is 170 °C, the heating rate is 5 °C / min, the vacuum degree is 40 mmHg, the time is 5 h, and the stirring speed is 200 rpm; the polymerization reaction temperature is 160 °C, the heating rate is 5 °C / min, the time is 2 h, the stirring rate is 300 rpm, and the mass percentages of the crosslinking agent, catalyst, and ethylene tar heavy fraction are 5%, 2%, and 93% respectively.

[0041] The petroleum-based impregnating pitch prepared by the preparation method of the petroleum-based impregnating pitch of the present invention has an appropriate softening point, high toluene insoluble content and coking value, and low quinoline insoluble content and ash content. Through experimental detection, the softening point of the petroleum-based impregnating pitch of the present invention is 85 - 95 °C, the quinoline insoluble content is 0.01 wt% - 0.1 wt%, the toluene insoluble content is 20 wt% - 30 wt%, the coking value is 50 wt% - 54 wt%, and the ash is 0.01 wt% - 0.04 wt%.

[0042] The petroleum-based impregnating pitch of the present invention can be used in the preparation of carbon material electrodes, and has an excellent impregnation and compaction effect on the carbon material green body.

[0043] The terms used in the present invention generally have the meanings commonly understood by those of ordinary skill in the art, unless otherwise specified.

[0044] To enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below in conjunction with embodiments.

[0045] In the following embodiments, various processes and methods not described in detail are conventional methods well known in the art. The materials, reagents, devices, instruments, equipment, etc. used in the following embodiments can be obtained from commercial channels without special instructions.

[0046] Example 1

[0047] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 5 h. After removing the light components in the ethylene tar, weigh the heavy components of the ethylene tar, and add 2 wt% p-toluenesulfonic acid and 5 wt% 1-naphthaldehyde. After mixing, add them into the reaction kettle and introduce nitrogen for protection. Control the temperature of the reaction kettle at 160 °C and the continuous heat preservation time to be 2 h. The reaction heating rate is 5 °C / min and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0048] Example 2

[0049] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 5 h. After removing the light components in the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% p-toluenesulfonic acid and 8 wt% 1-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 160 °C and the continuous heat preservation time to be 1 h. The reaction heating rate is 5 °C / min and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0050] Example 3

[0051] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 5 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% of p-toluenesulfonic acid and 3 wt% of 1-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 160 °C and the continuous heat preservation time to be 3 h. The reaction heating rate is 5 °C / min and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0052] Example 4

[0053] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 5 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% of p-toluenesulfonic acid and 5 wt% of 1-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 150 °C and the continuous heat preservation time to be 3 h. The reaction heating rate is 5 °C / min and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0054] Example 5

[0055] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 5 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% of p-toluenesulfonic acid and 5 wt% of 1-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 180 °C and the continuous heat preservation time to be 1 h. The reaction heating rate is 5 °C / min and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0056] Example 6

[0057] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 5 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% p-toluenesulfonic acid and 5 wt% 2-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 160 °C, and the continuous heat preservation time is 2 h. The reaction heating rate is 5 °C / min, and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0058] Example 7

[0059] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 40 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 200 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 3 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% p-toluenesulfonic acid and 5 wt% 2-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 180 °C, and the continuous heat preservation time is 1 h. The reaction heating rate is 5 °C / min, and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0060] Example 8

[0061] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 90 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 200 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 3 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% p-toluenesulfonic acid and 5 wt% 1-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 180 °C, and the continuous heat preservation time is 1 h. The reaction heating rate is 5 °C / min, and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0062] Example 9

[0063] Take 500 g of ethylene tar (quinoline insoluble content is 0.01 wt%, toluene insoluble content is 0.03 wt%, ash content is 0.01 wt%) and add it to a vacuum distillation device. Control the vacuum degree of the distillation system to be 90 mmHg, the heating rate to be 5 °C / min, the temperature to be controlled at 170 °C, the stirring speed to be 200 rpm, and the continuous distillation time to be 3 h. After removing the light components from the ethylene tar, weigh the heavy components of the ethylene tar, add 2 wt% p-toluenesulfonic acid and 5 wt% 1-naphthaldehyde, mix and add them into the reaction kettle, and introduce nitrogen for protection. Control the temperature of the reaction kettle at 180 °C, and the continuous heat preservation time is 1 h. The reaction heating rate is 5 °C / min, and the stirring rate is 300 rpm. After the reaction is completed, wait for cooling and take out the product to obtain petroleum-based impregnating pitch, and its properties are shown in Table 1.

[0064] Table 1 Properties of Petroleum-Based Impregnating Pitch in Examples 1-9

[0065]

[0066] As can be seen from Table 1, under the process conditions of Example 1, the prepared petroleum-based impregnating pitch has the best effect, with a moderate softening point, low quinoline insoluble and ash content, and high toluene insoluble and coking value.

[0067] The rheological properties of commercially available coal-based impregnating pitch and the petroleum-based impregnating pitch prepared in Example 1 were studied, and the results are as Figure 1 and Table 2 show.

[0068] Table 2 Viscosities of Coal-Based Impregnating Pitch of the Prior Art and Petroleum-Based Impregnating Pitch of Example 1 at Different Temperatures

[0069]

[0070]

[0071] From Figure 1 and Table 2, it can be seen that the kinematic viscosity of the petroleum-based impregnating pitch of the present invention is lower than that of the commercially available coal-based impregnating pitch under different temperature conditions.

[0072] The penetration properties of commercially available coal-based impregnating pitch and the petroleum-based impregnating pitch prepared in Example 1 were studied, and the results are as Figure 2 and Table 3 show.

[0073] Table 3 Penetration Rates of Coal-Based Impregnating Pitch of the Prior Art and Petroleum-Based Impregnating Pitch of Example 1 at Different Temperatures

[0074]

[0075] From Figure 2As can be seen from Table 3, the permeability of the petroleum-based impregnating pitch of the present invention is higher than that of the commercially available coal-based impregnating pitch under different temperature conditions.

[0076] The impregnation process of the carbon material electrode theoretically includes two processes in total: the first step is that the impregnating pitch changes from a solid state to a fluid flow state and contacts the surface of the carbon material green body; the second step is that the impregnating pitch enters the micropores inside the carbon material green body through the open pores of the carbon material green body and penetrates within the carbon material green body to fill the microporous structure of the carbon material green body. This process is related to the rheological properties and permeation properties of the impregnating pitch respectively. Therefore, good high-temperature fluidity and permeation properties are the most important indicators for judging the quality of the impregnating pitch. Based on the above experimental description, the petroleum-based pitch impregnating agent of the present invention has good high-temperature fluidity and permeation properties and can be used in the preparation of carbon material electrodes.

[0077] Obviously, the above embodiments are merely examples given for clear illustration and are not limitations on the embodiments. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to enumerate all embodiments here. And the obvious changes or modifications derived therefrom still fall within the protection scope of the present invention.

Claims

1. A method for preparing a petroleum-based impregnating pitch, characterized in that, It includes the following steps: 1) Subject the vinyl tar to vacuum distillation to remove the light components in the vinyl tar, and obtain the heavy components of vinyl tar; 2) Under an inert atmosphere, carry out a polymerization reaction on the heavy components of vinyl tar, a catalyst and a crosslinking agent, and cool to obtain a petroleum-based impregnating pitch; The crosslinking agent is one or more of 1-naphthaldehyde and 2-naphthaldehyde, the catalyst is p-toluenesulfonic acid, and the mass percentages of the crosslinking agent, the catalyst and the heavy components of vinyl tar are 3% - 8%, 2% and 90% - 95% respectively.

2. The preparation method of the petroleum-based impregnating agent pitch according to claim 1, characterized in that, The quinoline-insoluble content of the vinyl tar is 0 - 0.03 wt%, the toluene-insoluble content is 0.01 wt% - 0.05 wt%, and the ash content is 0 - 0.01 wt%.

3. The preparation method of the petroleum-based impregnating agent pitch according to claim 1, characterized in that, The temperature of the vacuum distillation is 150 - 200 °C, the heating rate is 5 - 10 °C / min, the vacuum degree is 40 - 90 mmHg, and the time is 3 - 5 h; and the vacuum distillation is carried out under stirring, and the stirring speed is 200 - 300 rpm.

4. The preparation method of the petroleum-based impregnating agent pitch according to claim 1, characterized in that, The softening point of the heavy components of vinyl tar is 70 - 90 °C, the quinoline-insoluble content is 0 - 0.05 wt%, the coking value is 28 wt% - 35 wt%, and the carbon-hydrogen element ratio is 1.15 - 1.

25.

5. The preparation method of the petroleum-based impregnating agent pitch according to claim 1, characterized in that, The inert atmosphere is nitrogen.

6. The preparation method of the petroleum-based impregnating agent pitch according to claim 1, characterized in that, The temperature of the polymerization reaction is 150 - 180 °C, the heating rate is 5 - 10 °C / min, and the time is 1 - 3 h; and the polymerization reaction is carried out under stirring, and the stirring rate is 200 - 300 rpm.

7. The preparation method of the petroleum-based impregnating agent pitch according to claim 1, characterized in that, The temperature of the vacuum distillation is 170 °C, the heating rate is 5 °C / min, the vacuum degree is 40 mmHg, the time is 5 h, and the stirring speed is 200 rpm; the temperature of the polymerization reaction is 160 °C, the heating rate is 5 °C / min, the time is 2 h, the stirring rate is 300 rpm, and the mass percentages of the crosslinking agent, the catalyst and the heavy components of vinyl tar are 5%, 2% and 93% respectively.

8. The petroleum-based impregnating pitch prepared by the preparation method of the petroleum-based impregnating pitch according to any one of claims 1 - 7.

9. The petroleum-based impregnating agent pitch according to claim 8, characterized in that, The softening point of the petroleum-based impregnating pitch is 85 - 95 °C, the quinoline-insoluble content is 0.01 wt% - 0.1 wt%, the toluene-insoluble content is 20 wt% - 30 wt%, the coking value is 50 wt% - 54 wt%, and the ash is 0.01 wt% - 0.04 wt%.

10. The application of the petroleum-based impregnating pitch according to claim 8 in the preparation of a carbon material electrode.

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