Kerosene co-refined residual-based hard pitch and preparation method thereof

Abstract

The present application relates to the technical field of high-performance asphalt material preparation, and discloses a kerosene co-refined residual-based hard asphalt and a preparation method thereof. The raw material for preparing the kerosene co-refined residual-based hard asphalt contains base asphalt, kerosene co-refined residue, a compatibilizer, a crosslinking agent and a stabilizer. The weight ratio of the base asphalt, the kerosene co-refined residue, the compatibilizer, the crosslinking agent and the stabilizer is 100:10-30:0.5-2:0.5-2:0.1-0.5. The compatibilizer is one or two or more of high-aromatic oil, rubber oil and reduced three-line extracted oil. The kerosene co-refined residual-based hard asphalt prepared by the method can improve the high-temperature performance of the base asphalt, improve the ductility of the asphalt and has good anti-rutting performance. Meanwhile, compared with traditional polymer modified asphalt, the kerosene co-refined residual-based hard asphalt has obvious performance advantages and price advantages.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field, and in particular to a coal oil co-refining residue-based hard asphalt and a preparation method thereof. BACKGROUND

[0002] Coal oil co-refining technology is a process of producing light oil products by hydrogenation of coal and heavy oil together, which is a high-efficiency clean utilization method of coal. The characteristic of the coal oil co-refining process is to use heavy oil or residual oil to replace the hydrogen-donor solvent in the coal liquefaction process, and the coal and oil slurry are fully reacted in the reactor to be cracked into gasoline, diesel and other light oil products. The coal oil co-refining residue is a byproduct of the process, accounting for about 20% of the weight of the raw coal. The coal oil co-refining residue contains a large amount of high-molecular-weight hydrocarbon compounds, has a high degree of aromaticity and a high content of carbon and hydrogen elements, and is suitable as a high-quality road asphalt modifier.

[0003] With the development of China's economy, the demand for transportation is increasing. As the main mode of road transportation, in recent years, with the increase of vehicle load and the repeated action on the asphalt pavement in a short time, the pavement is prone to cracking, rutting and other diseases. In order to solve the diseases of the asphalt pavement, engineering personnel often use polymer modified asphalt as road asphalt, but the compatibility of the polymer modifier and the base asphalt is not good, and segregation phenomenon is easy to occur. The price of the polymer modifier is relatively high, which increases the cost of the road modified asphalt.

[0004] At present, the methods for high-value utilization of coal oil co-refining residue in China mainly include: patent CN202011312778.8 discloses a method for preparing activated carbon adsorbent from coal oil co-refining residue, which mixes and conditions waste passion fruit peel particles and coal oil co-refining residue particles, and then processes them through a series of steps to improve the adsorption performance of the activated carbon and realize the resource utilization of the coal oil co-refining residue. Patent CN201911082820.9 discloses a coal oil co-refining residue resource utilization process, which processes the coal oil co-refining residue and an activator to prepare a residue-based catalyst carrier, and loads a coal oil co-refining catalyst for recycling, which has a wide application prospect in industry. It can be seen from the above that there is no related report in the prior art about using coal oil co-refining residue to modify base asphalt. SUMMARY

[0005] The purpose of the present application is to overcome the problems of poor deformation resistance, poor low-temperature crack resistance and poor fatigue resistance of base asphalt in the prior art, and to overcome the problems of high price and poor compatibility of traditional polymer modified asphalt. The present application provides a coal oil co-refining residue-based hard asphalt and a preparation method, which can improve the high-temperature performance of base asphalt, improve the ductility of asphalt and have good anti-rutting performance. Compared with traditional polymer modified asphalt, the present application has obvious performance advantages and price advantages.

[0006] The first aspect of the present application provides a raw material composition of a kerosene co-refining residue-based hard pitch, and the raw material for preparing the kerosene co-refining residue-based hard pitch comprises base pitch, kerosene co-refining residue, compatibility agent, cross-linking agent and stabilizer.

[0007] The weight ratio of the base pitch, the kerosene co-refining residue, the compatibility agent, the cross-linking agent and the stabilizer is 100:10-30:0.5-2:0.5-2:0.1-0.5.

[0008] The compatibility agent is one or more than two of high aromatic oil, rubber oil and reduced three-line extracted oil.

[0009] Preferably, the softening point of the kerosene co-refining residue is 100-150℃.

[0010] Preferably, the content of tetrahydrofuran soluble in the kerosene co-refining residue is 60-70wt%, and the ash content is 5-15wt%.

[0011] Preferably, the penetration of the base pitch at 25℃ and a depth of 0.1mm is 60-100.

[0012] Preferably, the cross-linking agent is one or more than two of benzaldehyde, formaldehyde and glyoxal.

[0013] Preferably, the stabilizer is one or more than two of organic polysulfide compound, mercaptan compound and sulfur.

[0014] The second aspect of the present application provides a method for preparing the kerosene co-refining residue-based hard pitch as described above, and the method comprises the following steps:

[0015] (1) heating the kerosene co-refining residue and the base pitch to a molten state respectively.

[0016] (2) mixing the molten kerosene co-refining residue and the molten base pitch at 120-150℃ for 10-20min, then adding the cross-linking agent and the compatibility agent and shearing and dispersing at 120-150℃ for 30-150min, then adding the stabilizer and stirring and developing at 120-150℃ for 2-3h to obtain the kerosene co-refining residue-based hard pitch.

[0017] Preferably, the heating temperature of the kerosene co-refining residue is 110-160℃.

[0018] Preferably, in step (1), the heating temperature of the base pitch is 100-240℃.

[0019] Preferably, in step (2), the stirring rate of the mixing is 3000-5000r / min.

[0020] Preferably, in step (2), the stirring rate of the stirring development is 450-600 r / min.

[0021] Compared with the prior art, the present invention has the following advantages:

[0022] The hard asphalt provided by this invention is of great significance for the efficient and high-value utilization of residues generated during the coal-oil co-refining process. Based on the coal-oil co-refining residue, after being blended with matrix asphalt, compatibilizers, crosslinking agents, and stabilizers are added for composite modification. The resulting hard asphalt has the characteristics of high softening point and high low-temperature ductility, and has good high and low temperature performance, especially improving the low-temperature crack resistance of the matrix asphalt.

[0023] The preparation method provided by this invention uses a composite modification approach to prepare hard asphalt. The raw materials selected are readily available and inexpensive, and the product is economical, suitable for areas with high temperatures and heavy traffic loads.

[0024] In conclusion, kerosene co-refining residue shows great promise as a modifier for base asphalt. It offers economic advantages over polymer modifiers and avoids segregation issues. This study proposes a new approach for the resource-based treatment of kerosene co-refining residue. Detailed Implementation

[0025] The following provides a detailed description of specific embodiments of the present invention. It should be understood that the specific embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the scope of the invention.

[0026] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0027] In the description of this application, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating relative importance or implying the number of technical features indicated. Therefore, unless otherwise stated, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature; "multiple" means two or more. The term "comprising" and any variations thereof mean non-exclusive inclusion, where one or more other features, integers, steps, operations, units, components, and / or combinations thereof may be present or added.

[0028] The first aspect of the present application provides a kerosene co-refining residue-based hard pitch, and the raw material for preparing the kerosene co-refining residue-based hard pitch contains base pitch, kerosene co-refining residue, compatibility agent, cross-linking agent and stabilizer.

[0029] In the present application, the kerosene co-refining residue is used as a modifier of the base pitch, and the compatibility agent, the cross-linking agent and the stabilizer are used for composite modification, which can greatly improve the high and low temperature performance of the base pitch, and especially can improve the low temperature crack resistance of the base pitch.

[0030] In the present application, the source of the base pitch is not limited. In the specific embodiment, the base pitch can be straight-run pitch, and the components are composed of saturates, aromatics, resins and asphaltenes according to the group composition analysis method. In the preferred embodiment, the penetration of the base pitch at 25℃ and the depth of 0.1mm is 60-100, and specifically, for example, it can be 60, 70, 80, 90 or 100.

[0031] In the present application, the kerosene co-refining residue is inferior oil residue by-produced from a kerosene co-refining device, which contains heavy oil, pitchene, pre-pitchene and THF insoluble, and the softening point thereof can be 100-150℃, and specifically, for example, it can be 100℃, 110℃, 120℃, 130℃, 140℃ or 150℃. In the preferred embodiment, the content of tetrahydrofuran soluble in the kerosene co-refining residue is 60-70wt%, and the ash content is 5-15wt%.

[0032] In the present application, the compatibility agent can be one or more than two of high aromatic oil, rubber oil and reduced three-line extraction oil. In the preferred embodiment, the compatibility agent is high aromatic oil, and the aromatic content thereof is ≥80wt%, and the main component of the high aromatic oil is condensed ring aromatic hydrocarbon. In the present application, the high aromatic oil added into the blend can supplement the content of light components therein, so that the formed blend has more stable colloidal structure.

[0033] In the present application, the cross-linking agent can promote the cross-linking between the kerosene co-refining residue, the base pitch and the compatibility agent, and the condensed ring polymerization reaction occurs. In the specific embodiment, the cross-linking agent can be an organic aldehyde cross-linking agent. In the more specific embodiment, the cross-linking agent can be one or more than two of benzaldehyde, formaldehyde and glyoxal. In order to generate macromolecular compounds, the plasticity of the pitch is stronger, and the low temperature crack resistance is stronger, and in the preferred embodiment, the cross-linking agent can be benzaldehyde.

[0034] In the present application, the addition of the stabilizer can improve the anti-aging performance of the kerosene co-refining residue-based hard asphalt, the storage stability is more excellent, and the penetration ratio of the kerosene co-refining residue-based hard asphalt is improved. In the specific embodiment, the stabilizer can be one or more of organic polysulfide compounds, mercaptan compounds and sulfur. In the preferred embodiment, the stabilizer is sulfur.

[0035] In the preferred embodiment, the weight ratio of the base asphalt, the kerosene co-refining residue, the compatibilizer, the crosslinking agent and the stabilizer is 100:10-30:0.5-2:0.5-2:0.1-0.5; specifically, it can be 100:10:0.5:0.5:0.1, 100:20:1:1:0.5, 100:20:1.2:0.7:0.3, 100:25:0.2:1.1:0.3, 100:30:1.8:2:0.5 or 100:10:0.9:1.5:0.2.

[0036] The present application uses kerosene co-refining residue as a modifier, and further adds compatibilizers, crosslinking agents and stabilizers as auxiliary additives for asphalt modification, thereby improving the anti-deformation ability of the kerosene co-refining residue-based hard asphalt; not only further optimizing the low-temperature crack resistance and fatigue resistance of the kerosene co-refining residue-based hard asphalt, but also realizing efficient utilization of the residue generated in the kerosene co-refining process.

[0037] The second aspect of the present application provides a method for preparing the kerosene co-refining residue-based hard asphalt described above, which comprises the following steps:

[0038] (1) heating the kerosene co-refining residue and the base asphalt to a molten state respectively;

[0039] (2) mixing the molten kerosene co-refining residue and the molten base asphalt at 120-150°C for 10-20 min, then adding the crosslinking agent and the compatibilizer and shearing and dispersing at 120-150°C for 30-150 min, then adding the stabilizer and stirring at 120-150°C for 2-3 h to prepare the kerosene co-refining residue-based hard asphalt.

[0040] In the method described in the present application, the kerosene co-refining residue is added to the base asphalt as a physical blending process, which can be regarded as not involving chemical reaction. The compatibilizer adjusts the composition of the asphalt to achieve a stable structure. The crosslinking agent causes the polyaromatic ring structure in the compatibilizer to polymerize. The stabilizer has a similar effect as the crosslinking agent, which can change the asphalt molecular chain from a two-dimensional structure to a three-dimensional structure, and the relative sliding between the molecular chains in the asphalt is constrained, so that the viscosity of the asphalt is improved, the low-temperature toughness of the asphalt is increased, and the high-temperature flow resistance is improved.

[0041] In the specific embodiment, the kerosene co-refining residue is crushed before being heated to the molten state. In the preferred embodiment, the particle size of the kerosene co-refining residue after crushing is less than 2 mm. In the specific embodiment, the heating method of the kerosene co-refining residue is not limited, and preferably, heating is carried out in an oven. The heating temperature can be 110-160°C, and specifically, for example, it can be 110°C, 120°C, 125°C, 130°C, 140°C, 150°C or 160°C.

[0042] In the specific embodiment, the heating method of the matrix asphalt is not limited, and preferably, heating is carried out in an oven. The heating temperature can be 100-240°C, and specifically, for example, it can be 100°C, 120°C, 140°C, 160°C, 180°C, 200°C, 220°C or 240°C.

[0043] In the specific embodiment, the stirring and mixing of step (2) is carried out in a stirrer, and after stirring, there are no fine particles in the mixture of molten kerosene co-refining residue and molten matrix asphalt.

[0044] In the preferred embodiment, the temperature of the stirring and mixing of step (2) can be 120-150°C; and specifically, for example, it can be 120°C, 125°C, 130°C, 140°C or 150°C.

[0045] In the preferred embodiment, the temperature of the stirring and mixing of step (2) can be 120-150°C; and specifically, for example, it can be 120°C, 125°C, 130°C, 140°C or 150°C.

[0046] In the method of the present application, the specific process of step (2) includes: first, stirring and mixing the molten kerosene co-refining residue and the molten matrix asphalt at 120-150°C for 10-20 min; then, first adding the crosslinking agent and carrying out first shear dispersion at 120-150°C for 30-60 min; then, adding the compatibilizer and carrying out second shear dispersion at 120-150°C for 30-60 min; finally, adding the stabilizer and stirring for 2-3 h at 120-150°C to prepare the kerosene co-refining residue-based hard asphalt.

[0047] In the specific embodiment, the first shear dispersion is carried out in a high-speed shear emulsifier. The high-speed shear machine is used to ensure the dispersion effect of the kerosene co-refining residue in the matrix asphalt. After adding the kerosene co-refining residue, the composition changes and a new colloid structure is formed.

[0048] In preferred embodiments, in step (2), the first shear dispersion can have a rate of 3000-5000 r / min; specifically, for example, it can be 3000 r / min, 3500 r / min, 4000 r / min, 4500 r / min, and 5000 r / min.

[0049] In preferred embodiments, in step (2), the first shear dispersion can have a temperature of 120-150 °C; specifically, for example, it can be 120 °C, 125 °C, 130 °C, 135 °C, 145 °C, and 150 °C.

[0050] In preferred embodiments, in step (2), the first shear dispersion can have a time of 30-60 min; specifically, for example, it can be 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, and 60 min.

[0051] In specific embodiments, the second shear dispersion is performed in a high-speed shearing emulsifier.

[0052] In preferred embodiments, in step (2), the second shear dispersion can have a rate of 3000-5000 r / min; specifically, for example, it can be 3000 r / min, 3500 r / min, 4000 r / min, 4500 r / min, and 5000 r / min.

[0053] In preferred embodiments, in step (2), the second shear dispersion can have a temperature of 120-150 °C; specifically, for example, it can be 120 °C, 125 °C, 130 °C, 135 °C, 145 °C, and 150 °C.

[0054] In preferred embodiments, in step (2), the second shear dispersion can have a time of 30-60 min; specifically, for example, it can be 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, and 60 min.

[0055] In preferred embodiments, in step (2), the stirring development can have a temperature of 120-150 °C; specifically, for example, it can be 120 °C, 125 °C, 130 °C, 135 °C, 145 °C, and 150 °C.

[0056] In preferred embodiments, in step (2), the stirring development can have a time of 2-3 h; specifically, for example, it can be 2 h, 2.5 h, or 3 h.

[0057] In a preferred embodiment, in step (2), the stirring rate of the stirring development can be 450-600 r / min, specifically, for example, can be 450 r / min, 500 r / min, 550 r / min or 600 r / min.

[0058] A kerosene co-refining residue-based hard pitch and a preparation method thereof are further illustrated by examples below. The examples are implemented on the premise of the technical solutions of the present application, and detailed implementation modes and specific operation processes are given, but the protection scope of the present application is not limited to the examples below.

[0059] In the following examples, the experimental methods are all conventional methods in the art unless otherwise specified. The experimental materials used in the examples below are all commercially available unless otherwise specified.

[0060] Example 1

[0061] The kerosene co-refining residue-based hard pitch provided in this example is made of the following components by weight: 100 grams of base pitch, 12 grams of kerosene co-refining residue, 0.5 grams of compatibilizer, 0.5 grams of crosslinking agent, and 0.1 grams of stabilizer.

[0062] The base pitch has a penetration of 72 at 25°C and 0.1 mm; the kerosene co-refining residue has a softening point of 113°C, and after being treated by a Soxhlet extractor, the content of tetrahydrofuran-soluble substance is 66.1 wt%, and the ash content is 12.3 wt%; the compatibilizer is high-aromatic oil, and the content of aromatic hydrocarbon is 84 wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0063] The preparation method of the kerosene co-refining residue-based hard pitch comprises the following steps:

[0064] The kerosene co-refining residue is crushed to a particle size of less than 2 mm and heated to a molten state at 125°C;

[0065] The base pitch is heated to a molten state at 120°C;

[0066] The molten kerosene co-refining residue and the molten base pitch are mixed and maintained at 145°C, and then dispersed by a stirrer for 20 min;

[0067] The compatibilizer is added to the blend of the kerosene co-refining residue and the base pitch, and then sheared by a high-speed shearing emulsifier at 3500 r / min for 45 min at 140°C;

[0068] The crosslinking agent is added to the blend of the kerosene co-refining residue and the base pitch to which the compatibilizer is added, and then sheared by the high-speed shearing emulsifier at 4000 r / min for 30 min at 150°C;

[0069] The stabilizer is added to the blend prepared in the above step, and stirred at 450 r / min at 130℃ for 2.5h, the stirring is stopped, and the kerosene co-refined residue-based hard pitch is prepared after cooling.

[0070] Example 2

[0071] The kerosene co-refined residue-based hard pitch provided in the example is prepared from the following components by weight: 100g of base pitch, 20g of kerosene co-refined residue, 1.2g of compatibilizer, 0.7g of crosslinking agent, and 0.3g of stabilizer.

[0072] The base pitch has a penetration of 90 at 25℃ and 0.1mm; the kerosene co-refined residue has a softening point of 113℃, and the content of tetrahydrofuran-soluble substance is 66.1wt% and the ash content is 12.3wt% after being treated by a Soxhlet extractor; the compatibilizer is high aromatic oil with an aromatic content of 84wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0073] The preparation method of the kerosene co-refined residue-based hard pitch comprises the following steps:

[0074] The kerosene co-refined residue is crushed to a particle size of less than 2mm, and heated to a molten state at 125℃;

[0075] The base pitch is heated to a molten state at 120℃;

[0076] The molten kerosene co-refined residue and the molten base pitch are mixed and kept at 145℃, and then dispersed by a stirrer for 20min;

[0077] The compatibilizer is added to the blend of the kerosene co-refined residue and the base pitch, and sheared by a high-speed shearing emulsifier at 4000r / min at 140℃ for 60min;

[0078] The crosslinking agent is added to the blend of the kerosene co-refined residue and the base pitch with the compatibilizer, and sheared by the high-speed shearing emulsifier at 4000r / min at 140℃ for 30min;

[0079] The stabilizer is added to the blend prepared in the above step, and stirred at 450 r / min at 130℃ for 2.5h, the stirring is stopped, and the kerosene co-refined residue-based hard pitch is prepared after cooling.

[0080] Example 3

[0081] The kerosene co-refined residue-based hard pitch provided in the example is prepared from the following components by weight: 100g of base pitch, 20g of kerosene co-refined residue, 1.2g of compatibilizer, 0.7g of crosslinking agent, and 0.3g of stabilizer.

[0082] The needle penetration of the base asphalt at 25°C and 0.1mm is 92;

[0083] The softening point of the kerosene co-refined residue is 113°C, and the content of the tetrahydrofuran soluble substance is 66.1wt% and the ash content is 12.3wt% after being treated by a Soxhlet extractor; the compatibilizer is high aromatic oil with an aromatic content of 84wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0084] The preparation method of the kerosene co-refined residue-based hard asphalt comprises the following steps:

[0085] The kerosene co-refined residue is crushed to a particle size of less than 2mm and heated to a molten state at 125°C;

[0086] The base asphalt is heated to a molten state at 120°C;

[0087] The molten kerosene co-refined residue and the molten base asphalt are mixed and kept at 130°C, and a stirrer is used for dispersion for 20min;

[0088] The compatibilizer is added to the blend of the kerosene co-refined residue and the base asphalt, and a high-speed shearing emulsifier is used for shearing at 4000r / min for 60min at 130°C;

[0089] The crosslinking agent is added to the blend of the kerosene co-refined residue and the base asphalt to which the compatibilizer is added, and the high-speed shearing emulsifier is continuously used for shearing at 4000r / min for 30min at 140°C, and then the shearing is stopped;

[0090] The stabilizer is added to the blend prepared in the above step, and stirring is carried out at 550r / min for 2h at 140°C, and then the stirring is stopped and the blend is cooled to prepare the kerosene co-refined residue-based hard asphalt.

[0091] Example 4

[0092] The kerosene co-refined residue-based hard asphalt provided in this example is prepared from the following components by weight: 100g of base asphalt, 30g of kerosene co-refined residue, 1.8g of compatibilizer, 2g of crosslinking agent, and 0.5g of stabilizer.

[0093] The needle penetration of the base asphalt at 25°C and 0.1mm is 68; the softening point of the kerosene co-refined residue is 113°C, and the content of the tetrahydrofuran soluble substance is 66.1wt% and the ash content is 12.3wt% after being treated by a Soxhlet extractor; the compatibilizer is high aromatic oil with an aromatic content of 84wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0094] The preparation method of the kerosene co-refined residue-based hard asphalt comprises the following steps:

[0095] The kerosene co-refined residue is crushed to a particle size of 2 mm or less and heated to a molten state at 125°C;

[0096] The base pitch is heated to a molten state at 120°C;

[0097] The molten kerosene co-refined residue and the molten base pitch are mixed and kept at 125°C, and then dispersed by a stirrer for 30 min;

[0098] The compatibilizer is added to the blend of the kerosene co-refined residue and the base pitch, and sheared by a high-speed shearing emulsifier at 4000 r / min for 60 min at 140°C;

[0099] The crosslinking agent is added to the blend of the kerosene co-refined residue and the base pitch to which the compatibilizer is added, and sheared by the high-speed shearing emulsifier at 4000 r / min for 30 min at 140°C, and then the shearing is stopped;

[0100] The stabilizer is added to the blend prepared in the above step, and stirred at 500 r / min for 3 h at 140°C, and then the stirring is stopped and the blend is cooled to prepare the kerosene co-refined residue-based hard pitch.

[0101] Example 5

[0102] The kerosene co-refined residue-based hard pitch provided in this example is prepared from the following components by weight: 100 g of base pitch, 10 g of kerosene co-refined residue, 0.9 g of compatibilizer, 1.5 g of crosslinking agent, and 0.2 g of stabilizer.

[0103] The base pitch has a penetration of 68 at 25°C and 0.1 mm; the kerosene co-refined residue has a softening point of 113°C, and after being treated by a Soxhlet extractor, the content of tetrahydrofuran-soluble substance is 66.1 wt%, and the ash content is 12.3 wt%; the compatibilizer is high-aromatic oil, and the content of aromatic hydrocarbon is 84 wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0104] The method for preparing the kerosene co-refined residue-based hard pitch comprises the following steps:

[0105] The kerosene co-refined residue is crushed to a particle size of 2 mm or less and heated to a molten state at 125°C;

[0106] The base pitch is heated to a molten state at 120°C;

[0107] The molten kerosene co-refined residue and the molten base pitch are mixed and kept at 145°C, and then dispersed by a stirrer for 20 min until no fine particles are observed in the blend;

[0108] The compatibilizer is added to the blend of the kerosene co-processing residue and the base pitch, and sheared at 4000 r / min for 60 min at 140°C using a high-speed shearing emulsifier;

[0109] The cross-linking agent is added to the blend of the kerosene co-processing residue and the base pitch to which the compatibilizer is added, and sheared at 4000 r / min for 30 min at 130°C using a high-speed shearing emulsifier, and then the shearing is stopped;

[0110] The stabilizer is added to the blend prepared in the above step, and stirred at 600 r / min for 3 h at 130°C, and then the stirring is stopped, and the kerosene co-processing residue-based hard pitch is prepared after cooling.

[0111] Comparative Example 1

[0112] The raw material proportions in the present comparative example are different from those in the examples.

[0113] The kerosene co-processing residue-based hard pitch provided in the present comparative example is prepared from the following raw material components by weight: base pitch 100 g, kerosene co-processing residue 50 g, compatibilizer 0.9 g, cross-linking agent 1.5 g, and stabilizer 0.2 g.

[0114] The base pitch has a penetration of 68 at 25°C and 0.1 mm; the kerosene co-processing residue has a softening point of 113°C, and after treatment by a Soxhlet extractor, the content of tetrahydrofuran-soluble substances is 66.1 wt%, and the ash content is 12.3 wt%; the compatibilizer is a high-aromatic oil, and the content of aromatic hydrocarbons is 84 wt%; the cross-linking agent is benzaldehyde; and the stabilizer is sulfur.

[0115] The method for preparing the kerosene co-processing residue-based hard pitch comprises the following steps:

[0116] The kerosene co-processing residue is crushed to a particle size of less than 2 mm, and heated to a molten state at 125°C;

[0117] The base pitch is heated to a molten state at 120°C;

[0118] The molten kerosene co-processing residue and the molten base pitch are mixed, and then dispersed using a stirrer for 20 min at 145°C;

[0119] The compatibilizer is added to the blend of the kerosene co-processing residue and the base pitch, and sheared at 4000 r / min for 60 min at 140°C using a high-speed shearing emulsifier;

[0120] The cross-linking agent is added to the blend of the kerosene co-processing residue and the base pitch to which the compatibilizer is added, and sheared at 4000 r / min for 30 min at 130°C using a high-speed shearing emulsifier, and then the shearing is stopped;

[0121] The stabilizer is added to the blend prepared in the above step, and stirred at 550 r / min for 2 h at 130 °C, the stirring is stopped, and the blend is cooled to prepare the kerosene co-refined residue based hard asphalt.

[0122] Comparative Example 2

[0123] The kerosene co-refined residue is not added in the present comparative example.

[0124] The asphalt provided in the present comparative example is prepared from the following components by weight: 100 g of base asphalt, 0.9 g of compatibilizer, 1.5 g of crosslinking agent, and 0.2 g of stabilizer.

[0125] The base asphalt has a penetration of 68 at 25 °C and 0.1 mm; the compatibilizer is high aromatic oil with an aromatic content of 84 wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0126] The method for preparing the asphalt comprises the following steps:

[0127] The base asphalt is heated to a molten state at 120 °C;

[0128] The compatibilizer is added to the molten base asphalt, and sheared at 3500 r / min for 60 min at 130 °C using a high-speed shearing emulsifier;

[0129] The crosslinking agent is added to the base asphalt blend with the compatibilizer, and sheared at 4000 r / min for 30 min at 140 °C using the high-speed shearing emulsifier;

[0130] The stabilizer is added to the blend prepared in the above step, and stirred at 550 r / min for 2 h at 130 °C, the stirring is stopped, and the blend is cooled to prepare the kerosene co-refined residue based hard asphalt.

[0131] Comparative Example 3

[0132] The compatibilizer is not added in the present comparative example.

[0133] The kerosene co-refined residue based hard asphalt provided in the present comparative example is prepared from the following components by weight: 100 g of base asphalt, 10 g of kerosene co-refined residue, 1.5 g of crosslinking agent, and 0.2 g of stabilizer.

[0134] The base asphalt has a penetration of 68 at 25 °C and 0.1 mm; the kerosene co-refined residue has a softening point of 113 °C, a content of tetrahydrofuran soluble of 66.1 wt% after treatment by a soxhlet extractor, and an ash content of 12.3 wt%; the crosslinking agent is benzaldehyde; and the stabilizer is sulfur.

[0135] The method for preparing the kerosene co-refined residue based hard asphalt comprises the following steps:

[0136] The kerosene co-refining residue is crushed to a particle size of 2 mm or less, and heated to a molten state at 125 DEG C;

[0137] The base pitch is heated to a molten state at 120 DEG C;

[0138] The kerosene co-refining residue in a molten state is mixed with the base pitch in a molten state, and maintained at 125 DEG C, and dispersed by a stirrer for 30 min;

[0139] The crosslinking agent is added to the kerosene co-refining residue and base pitch blend, and sheared by a high-speed shearing emulsifier at 4000 r / min for 60 min at 140 DEG C;

[0140] The stabilizer is added to the blend prepared in the above step, and stirred at 600 r / min for 3 h at 130 DEG C, and then cooled to prepare the kerosene co-refining residue-based hard pitch.

[0141] Test Example 1

[0142] The indicators of the kerosene co-refining residue-based hard pitch prepared in the examples are detected, and the results are shown in Table 1.

[0143] The indicators of the sample prepared in the comparative example are detected, and the results are shown in Table 2.

[0144] The technical requirements of GB / T 38075-2019 "Hard Road Petroleum Pitch" are shown in Table 3.

[0145] Table 1

[0146]

[0147]

[0148] Table 2

[0149]

[0150] Table 3

[0151]

[0152] By comparing Table 1 and Table 2, the kerosene co-refining residue-based prepared according to the examples of the present application has obvious advantages in penetration, softening point, ductility and anti-aging performance.

[0153] Table 3 is the technical requirements of GB / T 38075-2019 "Hard Road Petroleum Pitch" for No. 35 and No. 45 hard pitch, and by comparing Table 2 and Table 3, it can be seen that the kerosene co-refining residue-based hard pitch provided by the present application meets the relevant requirements.

[0154] The preferred embodiments of the present application are described in detail above, but the present application is not limited thereto. Within the technical concept of the present application, various simple modifications can be made to the technical solutions of the present application, including that each technical feature is combined in any other suitable manner. These simple modifications and combinations should also be considered as disclosed by the present application and fall within the protection scope of the present application.

Claims

1. A kerosene co-refining residue-based hard bitumen, characterized in that, The raw materials for preparing this kerosene co-refining residue-based hard pitch consist of matrix pitch, kerosene co-refining residue, compatibilizer, crosslinking agent, and stabilizer. The weight ratio of the base asphalt, the kerosene co-refining residue, the compatibilizer, the crosslinking agent, and the stabilizer is 100:20~30:0.5~2:0.5~2:0.1~0.

5. The compatibilizer is a high-aromatic oil with an aromatic content ≥80 wt%; The softening point of the kerosene co-refining residue is 100-150℃, the content of tetrahydrofuran solubles in the kerosene co-refining residue is 60-70wt%, and the ash content is 5-15wt%. The crosslinking agent is one or more of benzaldehyde, formaldehyde, and glyoxal.

2. The kerosene co-refining residue-based hard pitch according to claim 1, characterized in that, The penetration of the base asphalt at 25°C and a depth of 0.1 mm is 60-100.

3. The kerosene co-refining residue-based hard pitch according to claim 1 or 2, characterized in that, The stabilizer is one or more of organic polysulfide compounds, thiols, and sulfur.

4. A method for preparing kerosene co-refining residue-based hard pitch according to any one of claims 1-3, characterized in that, The method includes the following steps: (1) Heat the kerosene co-refining residue and the base bitumen to a molten state respectively; (2) Mix the molten kerosene co-refining residue and the molten base asphalt at 120-150℃ for 10-20 min, then add the crosslinking agent and compatibilizer and shear disperse at 120-150℃ for 30-150 min, then add the stabilizer and stir at 120-150℃ for 2-3 h to obtain kerosene co-refining residue-based hard asphalt.

5. The method according to claim 4, characterized in that, In step (1), the temperature at which the kerosene co-refining residue is heated is 110-160℃.

6. The method according to claim 4 or 5, characterized in that, In step (1), the base asphalt is heated to a temperature of 100-240°C.

7. The method according to claim 4 or 5, characterized in that, In step (2), the stirring rate of the mixing is 3000-5000 r / min.

8. The method according to claim 4 or 5, characterized in that, In step (2), the stirring rate of the stirring development is 450~600 r / min.

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