Impregnated asphalt as well as preparation method and application thereof

A method using pretreated aromatics and ethylene tar with hydrogenation processes addresses the lack of high-quality impregnated asphalt in China, producing a petroleum-based product that meets stringent quality standards and improves graphite electrode performance.

CN119081722APending Publication Date: 2024-12-06CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202310652418.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-06-05
Publication Date
2024-12-06

AI Technical Summary

Technical Problem

China lacks high-quality impregnated asphalt suitable for high-power and ultra-high-power graphite electrodes, with existing methods being complex, energy-intensive, and using environmentally harmful coal-based raw materials, failing to meet the stringent quality requirements for quinoline insoluble matter and softening point.

Method used

A preparation method using pretreated aromatics extracted oil and ethylene tar, combined with a hydrogenation process, to produce impregnated asphalt with low quinoline insoluble matter and controlled softening point, utilizing petroleum-based raw materials and optimized composition through blending, oxidation, and distillation.

Benefits of technology

The method produces impregnated asphalt that meets Chinese standards for high-end carbon materials, reducing environmental impact and production costs while enhancing mechanical strength and thermal conductivity of graphite electrodes.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention discloses impregnated asphalt as well as a preparation method and application thereof. The impregnated asphalt comprises the following components in parts by weight: 100 parts of pretreated aromatic hydrocarbon extract oil; 50 to 90 parts of pretreated ethylene tar; and 20 to 60 parts of a composite component. The impregnated asphalt disclosed by the invention can meet the index requirements of the national coking impregnated asphalt standard GB / T 35074-2018 coking impregnant asphalt on the No.2 product.
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Description

Technical Field

[0001] The invention relates to the field of special asphalt processing and production, and in particular to an impregnated asphalt and a preparation method and application thereof. Background Art

[0002] Impregnation asphalt is a common densification and reinforcement agent in the production of carbon materials. It is mainly used in the impregnation process of high-power and ultra-high-power graphite electrodes and high-tech carbon products, such as special graphite for aerospace and military use. Carbon materials are porous materials, and their carbon products have more or less pores. Generally, the pores account for about 1 / 4 of the volume of the carbon product itself. The presence of pores reduces the mechanical strength of carbon products, increases resistivity, and hinders thermal conductivity. When used under high temperature conditions, the oxidation rate is accelerated, the corrosion resistance drops sharply, and it is easier to penetrate. In order to reduce the porosity and improve the performance of carbon products, the roasted products need to be impregnated and densified during the production process.

[0003] The production methods of impregnating asphalt mainly include: (1) Coal tar filtration method (Western Europe): impregnating asphalt is directly produced in the coal tar processing device. This method has a simple process and low energy consumption, but it has strict requirements on the filter screen and harsh process conditions. (2) Coal tar solvent extraction method: The Polish National Coal Chemical Research Institute uses coal tar solvent extraction method to prepare impregnating asphalt. This method has a good purification effect, but the solvent consumption is large and the process energy consumption is high. (3) Thermal polymerization method: According to different raw material routes, it can also be divided into: thermal polymerization method with anthracene oil as the raw material, Cherry-T method, and soft asphalt flash polymerization method. Among them, Cherry-T method is a more representative thermal polymerization method. In the tar distillation process, asphalt and heavy oil fractions are directly polymerized and modified to produce impregnating asphalt. The yield of impregnating asphalt products produced by thermal polymerization method is low, the polymerization temperature is difficult to control, the polymerization effect is poor when the temperature is too low, and secondary quinoline insolubles are easily produced when the temperature is too high.

[0004] China has not yet widely adopted special impregnating asphalt for carbon materials, especially the impregnating asphalt for high-power and ultra-high-power electrodes is still in the research and development stage. Chinese graphite electrode manufacturers all use medium-temperature asphalt as impregnating asphalt (quinoline insoluble matter QI content is about 5%), and reduce its viscosity and softening point by adding anthracene oil and light oil. For example, Jilin Carbon Plant used medium-temperature asphalt produced by Anshan Iron and Steel and Benxi Steel to mix and dilute it as impregnating asphalt, and Hefei Carbon Plant used medium-temperature coal tar to add a little coal tar and lower the softening point as impregnating asphalt. However, as China's graphite electrodes develop towards large specifications and ultra-high power, graphite electrode companies have also put forward higher requirements for the quality indicators of impregnating asphalt, such as requiring the quinoline insoluble matter QI content to be below 5%.

[0005] CN101289625A discloses a production process for impregnating asphalt. Aliphatic hydrocarbon solvent and aromatic hydrocarbon solvent are selected to prepare a mixed solvent; medium-temperature coal tar pitch or coal tar soft asphalt and the mixed solvent enter at least three-stage mixers according to a certain ratio, and enter an extraction tower for separation after being fully mixed; light phase asphalt and heavy phase asphalt with less quinoline insoluble content are extracted and separated in the extraction tower; the light phase asphalt is stripped in a stripping tower to obtain the impregnating asphalt. Since a mixed solvent needs to be used and the light phase (containing the solvent) needs to be distilled twice, the process is complicated and the energy consumption is high.

[0006] CN112779042A discloses a method for producing high-quality impregnated asphalt. Tar is heated to a certain temperature by two-stage heat exchange to achieve a lower viscosity and better fluidity, reduce its density, and is separated by a disc centrifuge with a higher separation factor. The centrifuge discharges slag regularly, and the interval between slag discharges needs to be set to allow the slag phase to have better fluidity to prevent clogging of the disc and slag cavity. The tar after centrifugal purification is distilled and the parameters are appropriately controlled to meet the softening point, toluene insolubles, quinoline insolubles, coking value, ash content and other requirements of high-quality impregnated asphalt. The method for preparing impregnated asphalt has a complex process and uses coal tar as the main raw material, which is unfavorable to the environment and human health.

[0007] In summary, developing a high-quality impregnated asphalt to meet China's application needs for high-end carbon material products, replace imported products, and solve the problems of expensive raw materials used in special carbon materials and difficult supply guarantees has great social and economic significance. Summary of the invention

[0008] In view of the shortcomings of the prior art, the object of the present invention is to provide an impregnated asphalt and a preparation method and application thereof. The impregnated asphalt of the present invention can meet the index requirements of the Chinese domestic coking impregnated asphalt standard "GB / T 35074-2018 Coking Impregnating Agent Asphalt" for No. 2 products.

[0009] The first aspect of the present invention provides an impregnated asphalt, which comprises the following components in parts by weight:

[0010] Pre-treated aromatics extracted oil: 100 parts;

[0011] Pretreated ethylene tar: 50-90 parts, preferably 55-80 parts;

[0012] Composite component: 20 to 60 parts, preferably 20 to 45 parts.

[0013] The pretreated aromatic extracted oil is a fraction with a temperature greater than 300° C. cut from the aromatic extracted oil after distillation.

[0014] The pretreated ethylene tar is a fraction with a temperature greater than 320° C. cut from the ethylene tar after distillation.

[0015] The aromatic extracted oil is at least one of a three-line minus distillate oil and a four-line minus distillate oil, and is preferably at least one of a three-line minus furfural refined extracted oil and a four-line minus furfural refined extracted oil.

[0016] The main properties of the aromatic extracted oil include: saturated components account for 27wt% to 30wt%, aromatic components account for 52wt% to 60wt%, colloids account for 13wt% to 19wt%, asphaltene accounts for 0wt% to 0.2wt%, and the four-component analysis method is T0618-1993 asphalt chemical component test (four-component method); ar 15wt%~17wt%, H α 25wt%~28wt%, H β Accounting for 43wt%~46t%, H γ It accounts for 14wt% to 16wt%, the C / H molar ratio is 0.82 to 0.88, the aromatic carbon fraction is 48wt% to 51wt%, the cycloalkane carbon fraction is 15wt% to 18wt%, and the alkyl carbon fraction is 35wt% to 37wt%.

[0017] The main properties of the ethylene tar include: saturated fraction accounts for 0.1wt% to 2.6wt%, aromatic fraction accounts for 54wt% to 69wt%, colloid accounts for 25wt% to 34wt%, asphaltene accounts for 0.5wt% to 4.1wt%, the four-component analysis method is T0618-1993 asphalt chemical component test (four-component method), the residual carbon value is 11wt% to 15wt%, the C / H molar ratio is 12 to 14, and the S / N molar ratio is 14 to 20; H ar Accounting for 45wt%~48wt%, H α Accounting for 31wt%~35wt%, H β Accounting for 14wt%~16wt%, H γ The composite components include the following components by weight:

[0018] Medium component: 100 parts;

[0019] Light component: 15 to 30 parts, preferably 15 to 25 parts.

[0020] The middle mass component refers to the colloid obtained after solvent deasphalting. The middle mass component has the following properties: kinematic viscosity at 100°C is 50 mm 2 / s~65mm 2 / s, the flash point is 206℃~220℃, by mass fraction, the saturated fraction accounts for 30%~42%, the aromatic fraction accounts for 48%~57%, the gum accounts for 8%~13%, and the asphaltene content is less than 2%; the weight average molecular weight is 1990~2140, and the molecular weight distribution width is 1.6~3.7.

[0021] The light component refers to vacuum wax oil. The light component has the following properties: 50°C kinematic viscosity is 10 mm 2 / s~16mm 2 / s, density at 20℃ is 760~900kg / m 3 , by mass fraction, the saturated content accounts for 60% to 78%, the aromatic content accounts for 20% to 35%, the total content of colloid and asphaltene is less than 6%; the residual carbon is less than 0.15wt%, the sulfur content is less than 0.3wt%, the nitrogen content is less than 1wt%, and the hydrogen-carbon molar ratio is 1.5 to 1.8.

[0022] The second aspect of the present invention provides a method for preparing the above-mentioned impregnated asphalt, comprising:

[0023] (1) blending, oxidizing and condensing the pretreated aromatics extracted oil and the pretreated ethylene tar to obtain a carbon-rich component;

[0024] (2) preparing composite components;

[0025] (3) The composite component obtained in step (2) is mixed with the carbon-rich component obtained in step (1) and subjected to reduced pressure distillation to obtain the impregnated asphalt.

[0026] In step (1), the pretreatment process of the pretreated aromatic extracted oil and the pretreated ethylene tar is distillation, wherein the pretreated aromatic extracted oil is a fraction greater than 300° C. cut from the aromatic extracted oil after distillation, and the pretreated ethylene tar is a fraction greater than 320° C. cut from the ethylene tar after distillation.

[0027] In step (1), the pretreated aromatics extracted oil and the pretreated ethylene tar are blended at 180°C to 200°C, the stirring speed of the blending process is 700 to 900 r / min, and the time is 4 to 6 hours. After the blending is completed, oxidation and condensation are carried out in the reactor. The temperature of the oxidation process is 240°C to 255°C, and the gas flow rate is 0.05 to 0.15 m 3 / (kg.h), the oxidation time is 150-180min, the gas is oxygen-enriched air, and the oxygen volume content is 60%-75%; the temperature of the condensation process is 330℃-350℃, and the inert gas flow rate is 0.10-0.25m 3 / (kg.h), the condensation time is 200-230min, and the inert gas is preferably nitrogen.

[0028] In step (2), the process of preparing the composite component is as follows:

[0029] i. After the medium components and light components heated to a fluid state are mixed, hydrogen is added for hydrogenation treatment;

[0030] ii. subjecting the material obtained in step i to atmospheric and vacuum distillation to obtain the composite component.

[0031] In step i, the operating conditions of the hydrotreatment are: reaction temperature of 365°C to 390°C, reaction pressure of 12MPa to 22MPa, volume space velocity of 0.5 to 1.8h -1 , hydrogen-to-oil volume ratio is 400-1500; the preferred operating conditions are: reaction temperature is 370°C-390°C, reaction pressure is 13MPa-20MPa, volume space velocity is 0.5-1.2h -1 , the volume ratio of hydrogen to oil is 500-1100.

[0032] In step i, the reactor used for the hydrotreatment can be at least one of a fixed bed hydrogenation reactor, an ebullated bed hydrogenation reactor or a suspended bed hydrogenation reactor, preferably an ebullated bed hydrogenation reactor.

[0033] In step i, the catalyst used in the hydroprocessing can be a commercially available catalyst, for example, one or more of the FF, FH, and FZC series catalysts developed by Sinopec Dalian Petrochemical Research Institute can be used. The catalyst grading method can be determined according to conventional methods and is not particularly limited in the present invention.

[0034] In step ii, the atmospheric and vacuum distillation is carried out in an atmospheric and vacuum distillation kettle. There are no special requirements for atmospheric distillation. The final temperature of the vacuum distillation is 465-540°C, preferably 485-520°C.

[0035] In step (3), the final temperature of the reduced pressure distillation is 520-580°C, preferably 520-560°C.

[0036] The third aspect of the present invention provides a use of the above-mentioned impregnated asphalt in a graphite electrode.

[0037] Compared with the prior art, the present invention has the following characteristics:

[0038] (1) The present invention uses pretreated aromatics extracted oil and pretreated ethylene tar as raw materials, and by controlling the process conditions of distillation, blending, oxidation, and condensation, a carbon-rich component with low quinoline insoluble matter, low ash content, and high coking value can be obtained, which lays a foundation for the next step of blending and preparing impregnated asphalt with a moderate softening point and other qualified indicators. The preparation of the carbon-rich component adopts a traditional process, does not require a high-pressure or ultra-high-pressure environment, and is easy to implement.

[0039] (2) The composite component introduced in the present invention is obtained by hydrogenation treatment and secondary distillation of a medium component and a light component with special properties. The composition structure of the material is adjusted and optimized during the treatment process so that the material can simultaneously meet the mutually restrictive conditions of low softening point and high coking value. The composite component and the carbon-rich component are compounded and fractionated again to obtain an impregnated asphalt that meets the index requirements.

[0040] (3) The present invention uses petroleum-based raw materials to prepare impregnated asphalt. Compared with traditional coal-based raw materials, the average molecular weight of each component of the petroleum-based raw materials is small, the micropore impregnation effect is better, the thermochemical reaction activity is high, the content of native quinoline insolubles is small, the amount of harmful impurities is small, the harm to the environment and human body is small, and it has higher economic value and environmental protection effect. DETAILED DESCRIPTION

[0041] The technical solution of the present invention is further described below by way of examples, but these examples cannot limit the protection scope of the present invention, and the wt % involved is the mass fraction.

[0042] The present invention uses a Bruker Avance II 400 nuclear magnetic resonance spectrometer (Germany) to analyze the H and C contents at different positions. ar Denotes hydrogen directly attached to aromatic carbon, H α represents the hydrogen attached to the alpha carbon of the aromatic ring, H β It represents the hydrogen on the β-carbon of the aromatic ring and the hydrogen on the CH2 and CH groups connected to the β-carbon. γ It represents the hydrogen on the γ carbon of the aromatic ring and the hydrogen on the CH3 group connected to the γ carbon. 1 H-NMR can directly provide the distribution information of hydrogen atoms or carbon atoms at different positions through the difference in chemical shift values.

[0043] Example 1

[0044] (1) Aromatic extracted oil (main properties see Table 1) and ethylene tar (main properties see Table 2) were pre-treated by distillation, and 100 parts of pre-treated aromatic extracted oil (fraction above 300°C) and 65 parts of pre-treated ethylene tar (fraction above 320°C) were blended at 185°C and 800 r / min for 5 hours to make the two mixed evenly. The mixed material was first oxidized in a reactor at a temperature of 245°C and an oxygen-enriched air flow rate of 0.12 m 3 / / (kg.h), the oxidation time is 180min, the oxygen volume content in the oxygen-enriched air is 70%; after the oxidation is completed, a condensation reaction is carried out, the temperature of the condensation process is 340°C, and the nitrogen flow rate is 0.20m 3 / / (kg.h), the condensation time is 230min, and the desired carbon-rich component is obtained after the reaction is completed.

[0045] (2) 100 parts of the medium component (main properties are shown in Table 3) heated to a fluid state and 20 parts of the light component (main properties are shown in Table 4) were reacted at a reaction temperature of 380°C, a reaction pressure of 16 MPa, and a volumetric space velocity of 0.8 h -1 The hydrogenation treatment is carried out under the condition of a hydrogen-to-oil volume ratio of 900. The FZC-301 catalyst developed by Sinopec Dalian Petrochemical Research Institute is selected as the hydrogenation catalyst. The hydrogenation product is subjected to atmospheric and vacuum distillation. The distillation product above 510°C is the desired composite component.

[0046] (3) The carbon-rich component obtained in step (1) is uniformly mixed with 35 parts of the composite component obtained in step (2) and subjected to reduced pressure distillation to obtain a fraction with a temperature greater than 550° C., which is the impregnation asphalt A1.

[0047] Example 2

[0048] (1) Aromatic extracted oil (main properties see Table 1) and ethylene tar (main properties see Table 2) were pre-treated by distillation, and 100 parts of pre-treated aromatic extracted oil (fraction above 300°C) and 60 parts of pre-treated ethylene tar (fraction above 320°C) were blended at 185°C and 800 r / min for 5 hours to make the two mixed evenly. The mixed material was first oxidized in a reactor at a temperature of 240°C and an oxygen-enriched air flow rate of 0.10 m 3 / h, the oxidation time is 180min, the oxygen volume content in the oxygen-enriched air is 70%; after the oxidation is completed, a condensation reaction is carried out, the temperature of the condensation process is 340°C, and the nitrogen flow rate is 0.20m 3 / h, the condensation time is 220min, and the desired carbon-rich component is obtained after the reaction is completed.

[0049] (2) 100 parts of the medium component (main properties are shown in Table 3) heated to a fluid state and 20 parts of the light component (main properties are shown in Table 4) were reacted at a reaction temperature of 380°C, a reaction pressure of 16 MPa, and a volumetric space velocity of 0.8 h -1 The hydrogenation treatment is carried out under the condition of a hydrogen-to-oil volume ratio of 900. The FZC-301 catalyst developed by Sinopec Dalian Petrochemical Research Institute is selected as the hydrogenation catalyst. The hydrogenation product is subjected to atmospheric and vacuum distillation. The distillation product above 500°C is the desired composite component.

[0050] (3) The carbon-rich component obtained in step (1) is uniformly mixed with 40 parts of the composite component obtained in step (2) and subjected to reduced pressure distillation to obtain a fraction with a temperature greater than 545° C., which is the impregnation asphalt A2.

[0051] Example 3

[0052] (1) Aromatic extracted oil (main properties see Table 1) and ethylene tar (main properties see Table 2) were pre-treated by distillation, and 100 parts of pre-treated aromatic extracted oil (fraction above 300°C) and 70 parts of pre-treated ethylene tar (fraction above 320°C) were blended at 185°C and 800 r / min for 5 hours to make the two mixed evenly. The mixed material was first oxidized in a reactor at a temperature of 250°C and an oxygen-enriched air flow rate of 0.15 m 3 / h, the oxidation time is 180min, the oxygen volume content in the oxygen-enriched air is 70%; after the oxidation is completed, a condensation reaction is carried out, the temperature of the condensation process is 340°C, and the nitrogen flow rate is 0.22m 3 / h, the condensation time is 230min, and the desired carbon-rich component is obtained after the reaction is completed.

[0053] (2) 100 parts of the medium component (main properties are shown in Table 3) heated to a fluid state and 20 parts of the light component (main properties are shown in Table 4) were reacted at a reaction temperature of 375°C, a reaction pressure of 17 MPa, and a volumetric space velocity of 0.8 h -1 The hydrogenation treatment is carried out under the condition of a hydrogen-to-oil volume ratio of 900. The FZC-301 catalyst developed by Sinopec Dalian Petrochemical Research Institute is selected as the hydrogenation catalyst. The hydrogenation product is subjected to atmospheric and vacuum distillation. The distillation product above 520°C is the desired composite component.

[0054] (3) The carbon-rich component obtained in step (1) is uniformly mixed with 30 parts of the composite component obtained in step (2) and subjected to reduced pressure distillation to obtain a fraction with a temperature greater than 550° C., which is the impregnation asphalt A3.

[0055] Example 4

[0056] The same as Example 1, except that the properties of the aromatic extracted oil, ethylene tar, medium component and light component used are shown in Tables 5 to 8, respectively, to obtain impregnated asphalt A4.

[0057] Example 5

[0058] The same as Example 2, except that the properties of the aromatic extracted oil, ethylene tar, medium component and light component used are shown in Tables 5 to 8, respectively, to obtain impregnated asphalt A5.

[0059] Comparative Example 1

[0060] The same as Example 1, except that during the preparation process, 100 parts of pretreated aromatic extracted oil (fractions above 300°C) and 65 parts of pretreated ethylene tar (fractions above 320°C) are replaced with 165 parts of pretreated aromatic extracted oil (fractions above 300°C) to obtain impregnation asphalt B1.

[0061] Comparative Example 2

[0062] The same as Example 1, except that during the preparation process, 100 parts of pretreated aromatic extracted oil (fraction above 300°C) and 65 parts of pretreated ethylene tar (fraction above 320°C) are replaced with 165 parts of pretreated ethylene tar (fraction above 320°C) to obtain impregnation asphalt B2.

[0063] Comparative Example 3

[0064] The same as Example 1, except that no composite component is added during the preparation process, to obtain impregnated asphalt B3.

[0065] Comparative Example 4

[0066] The same as Example 1, except that during the preparation of the composite component, 100 parts of the medium component heated to a fluid state (the main properties are shown in Table 3) and 20 parts of the light component (the main properties are shown in Table 4) are replaced with 120 parts of the light component (the main properties are shown in Table 4) to obtain impregnated asphalt B4.

[0067] Comparative Example 5

[0068] The same as Example 1, except that during the preparation process, 65 parts of pretreated ethylene tar (fraction greater than 320°C) are replaced with 65 parts of pretreated ethylene tar (fraction greater than 280°C) to obtain impregnation asphalt B5.

[0069] Test Case

[0070] The main properties of the raw materials used in the embodiments and comparative examples were analyzed and tested, as shown in Tables 1 to 8. The main property indicators of the impregnated asphalt prepared in the embodiments and comparative examples were analyzed. The analysis method referred to the requirements of "GB / T35074-2018 Coking Impregnating Agent Asphalt", and the results are shown in Table 9.

[0071] Table 1 Partial properties of aromatic oils used in Examples 1 to 3 and Comparative Examples

[0072] Saturated fraction / wt% 27.31 Aromatic content / wt% 54.22 Gel / wt% 18.36 Asphaltene / wt% 0.11 <![CDATA[H ar / wt%]]> 15.24 <![CDATA[H α / wt%]]> 27.15 <![CDATA[H β / wt%]]> 43.36 <![CDATA[H γ / wt%]]> 14.25 C / H (molar ratio) 0.87 Aromatic carbon fraction / wt% 49 Cycloalkane carbon fraction / wt% 16 Alkyl carbon fraction / wt% 35

[0073] Table 2 Partial properties of ethylene tar used in Examples 1 to 3 and Comparative Examples

[0074] Carbon residue value / wt% 14.28 Saturated fraction / wt% 1.07 Aromatic content / wt% 65.14 Gel / wt% 32.58 Asphaltene / wt% 1.21 <![CDATA[H ar / wt%]]> 46.52 <![CDATA[H α / wt%]]> 33.41 <![CDATA[H β / wt%]]> 15.03 <![CDATA[H γ / wt%]]> 5.04 C / H (molar ratio) 12.37 S / N (molar ratio) 16.44

[0075] Table 3 Properties of some of the intermediate components used in Examples 1 to 3 and Comparative Examples

[0076]

[0077]

[0078] Table 4 Properties of some light components used in Examples 1 to 3 and Comparative Examples

[0079] Saturated fraction / wt% 69.21 Aromatic content / wt% 26.36 Gel / wt% 4.32 Asphaltene / wt% 0.11 Carbon residue value / wt% 0.13 Sulfur content / wt% 0.24 Nitrogen content / wt% 0.18 Hydrogen-carbon molar ratio 1.8 <![CDATA[50℃ kinematic viscosity / mm 2 / s]]> 13 <![CDATA[Density at 20°C / kg / m 3 > 817

[0080] Table 5 Partial properties of aromatic oil extracted from Examples 4 to 5

[0081]

[0082]

[0083] Table 6 Partial properties of ethylene tar used in Examples 4 to 5

[0084] Carbon residue value / wt% 14.47 Saturated fraction / wt% 0.86 Aromatic content / wt% 66.42 Gel / wt% 32.13 Asphaltene / wt% 0.59 <![CDATA[H ar / wt%]]> 47.02 <![CDATA[H α / wt%]]> 33.84 <![CDATA[H β / wt%]]> 14.97 <![CDATA[H γ / wt%]]> 4.17 C / H (molar ratio) 12.62 S / N (molar ratio) 16.12

[0085] Table 7 Properties of some of the intermediate components used in Examples 4 to 5

[0086] Saturated fraction / wt% 33.41 Aromatic content / wt% 56.65 Gel / wt% 9.92 Asphaltene / wt% 0.02 <![CDATA[Kinematic viscosity at 100℃ / mm 2 / s]]> 55 Flash point / ℃ 217 Weight average molecular weight 2138 Molecular weight distribution width 2.1

[0087] Table 8 Properties of some light components used in Examples 4 to 5

[0088] Saturated fraction / wt% 66.07 Aromatic content / wt% 28.44 Gel / wt% 5.46 Asphaltene / wt% 0.03 Carbon residue value / wt% 0.12 Sulfur content / wt% 0.21 Nitrogen content / wt% 0.06 Hydrogen-carbon molar ratio 1.7 <![CDATA[50℃ kinematic viscosity / mm 2 / s]]> 13 <![CDATA[Density at 20°C / kg / m 3 > 856

[0089] Table 9 Properties of impregnated asphalt prepared in Examples and Comparative Examples

[0090]

[0091]

[0092] The protection scope of the present invention is not limited by the above embodiments, but by the claims. Those skilled in the art may make appropriate changes to these embodiments without departing from the technical concept and purpose of the present invention, and these changed embodiments are also included in the protection scope of the present invention.

Claims

1. An impregnated asphalt, characterized in that: By weight, it includes the following components: Pre-treated aromatics extracted oil: 100 parts; Pretreated ethylene tar: 50-90 parts, preferably 55-80 parts; Composite component: 20 to 60 parts, preferably 20 to 45 parts.

2. The impregnated asphalt according to claim 1, characterized in that The pretreated aromatic extracted oil is a fraction with a temperature greater than 300° C. cut from the aromatic extracted oil after distillation.

3. The impregnated asphalt according to claim 1, characterized in that The pretreated ethylene tar is a fraction with a temperature greater than 320° C. cut from the ethylene tar after distillation.

4. The impregnated asphalt according to claim 2, characterized in that The aromatic extracted oil is at least one of a three-line minus distillate oil and a four-line minus distillate oil, and is preferably at least one of a three-line minus furfural refined extracted oil and a four-line minus furfural refined extracted oil.

5. The impregnated asphalt according to claim 2 or 4, characterized in that The properties of the aromatic extracted oil include: saturated components account for 27wt% to 30wt%, aromatic components account for 52wt% to 60wt%, colloids account for 13wt% to 19wt%, and asphaltenes account for 0wt% to 0.2wt%; ar 15wt%~17wt%, H α 25wt%~28wt%, H β Accounting for 43wt%~46t%, H γ It accounts for 14wt% to 16wt%, the C / H molar ratio is 0.82 to 0.88, the aromatic carbon fraction is 48wt% to 51wt%, the cycloalkane carbon fraction is 15wt% to 18wt%, and the alkyl carbon fraction is 35wt% to 37wt%.

6. The impregnated asphalt according to claim 3, characterized in that The properties of the ethylene tar include: saturated fraction accounts for 0.1wt% to 2.6wt%, aromatic fraction accounts for 54wt% to 69wt%, colloid accounts for 25wt% to 34wt%, asphaltene accounts for 0.5wt% to 4.1wt%; the residual carbon value is 11wt% to 15wt%, the C / H molar ratio is 12 to 14, the S / N molar ratio is 14 to 20; H ar Accounting for 45wt%~48wt%, H α 31wt%~35wt%, H β Accounting for 14wt%~16wt%, H γ It accounts for 4wt% to 7wt%.

7. The impregnating asphalt according to claim 1, characterized in that The composite components include the following components by weight: Medium component: 100 parts; Light component: 15 to 30 parts, preferably 15 to 25 parts.

8. The impregnating asphalt according to claim 7, characterized in that The middle mass component refers to the colloid obtained after solvent deasphalting; the middle mass component has the following properties: kinematic viscosity at 100°C is 50 mm 2 / s~65mm 2 / s, the flash point is 206℃~220℃, by mass fraction, the saturated fraction accounts for 30%~42%, the aromatic fraction accounts for 48%~57%, the gum accounts for 8%~13%, and the asphaltene content is less than 2%; the weight average molecular weight is 1990~2140, and the molecular weight distribution width is 1.6~3.

7.

9. The impregnated asphalt according to claim 7, characterized in that The light component refers to vacuum wax oil; the light component has the following properties: 50°C kinematic viscosity is 10mm 2 / s~16mm 2 / s, density at 20℃ is 760~900kg / m 3 , by mass fraction, the saturated content accounts for 60% to 78%, the aromatic content accounts for 20% to 35%, the total content of colloid and asphaltene is less than 6%; the residual carbon is less than 0.15wt%, the sulfur content is less than 0.3wt%, the nitrogen content is less than 1wt%, and the hydrogen-carbon molar ratio is 1.5 to 1.

8.

10. The method for preparing the impregnated asphalt according to any one of claims 1 to 9, characterized in that: include: (1) blending, oxidizing and condensing the pretreated aromatics extracted oil and the pretreated ethylene tar to obtain a carbon-rich component; (2) preparing composite components; (3) The composite component obtained in step (2) is mixed with the carbon-rich component obtained in step (1) and subjected to reduced pressure distillation to obtain the impregnated asphalt.

11. The preparation method according to claim 10, characterized in that: In step (1), the pretreated aromatics extracted oil and the pretreated ethylene tar are blended at 180°C to 200°C, the stirring speed of the blending process is 700 to 900 r / min, and the time is 4 to 6 hours; the temperature of the oxidation process is 240°C to 255°C, and the gas flow rate is 0.05 to 0.15 m 3 / (kg.h), the oxidation time is 150-180min, the gas is oxygen-enriched air, and the oxygen volume content is 60%-75%; the temperature of the condensation process is 330℃-350℃, and the inert gas flow rate is 0.10-0.25m 3 / (kg.h), the condensation time is 200-230min, and the inert gas is preferably nitrogen.

12. The preparation method according to claim 10, characterized in that: In step (2), the process of preparing the composite component is as follows: i. After the medium and light components heated to a fluid state are mixed, hydrogen is added for hydrogenation treatment; ii. The material obtained in step i is subjected to atmospheric and vacuum distillation to obtain a composite component.

13. The preparation method according to claim 12, characterized in that: In step i, the operating conditions of the hydrotreatment are: reaction temperature of 365°C to 390°C, reaction pressure of 12MPa to 22MPa, volume space velocity of 0.5 to 1.8h -1 , hydrogen-oil volume ratio is 400-1500; the preferred operating conditions are: reaction temperature is 370℃-390℃, reaction pressure is 13MPa-20MPa, volume space velocity is 0.5-1.2h -1 , the volume ratio of hydrogen to oil is 500-1100.

14. The preparation method according to claim 12, characterized in that: In step ii, the atmospheric and vacuum distillation is carried out in an atmospheric and vacuum distillation kettle, and the final temperature of the vacuum distillation is 465-540°C, preferably 485-520°C.

15. The preparation method according to claim 10, characterized in that: In step (3), the final temperature of the reduced pressure distillation is 520-580°C, preferably 520-560°C.

16. Use of the impregnated asphalt according to any one of claims 1 to 9 or the impregnated asphalt prepared by the method according to any one of claims 10 to 15 in graphite electrodes.

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