CN108059970B - Method for utilizing catalytic slurry oil - Google Patents
Method for utilizing catalytic slurry oil Download PDFInfo
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- CN108059970B CN108059970B CN201610983412.0A CN201610983412A CN108059970B CN 108059970 B CN108059970 B CN 108059970B CN 201610983412 A CN201610983412 A CN 201610983412A CN 108059970 B CN108059970 B CN 108059970B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G7/00—Distillation of hydrocarbon oils
- C10G7/006—Distillation of hydrocarbon oils of waste oils other than lubricating oils, e.g. PCB's containing oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G7/00—Distillation of hydrocarbon oils
- C10G7/06—Vacuum distillation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4012—Pressure
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for utilizing catalytic slurry oil. The method comprises the following steps: adding a modifier into the catalytic slurry oil, and stirring to prepare modified catalytic slurry oil; mixing the obtained modified catalytic slurry oil with atmospheric residue oil, then carrying out vacuum distillation, and obtaining vacuum residue oil after vacuum distillation; wherein, taking the total raw material mass in the step (1) as a reference, and according to the mass fraction, the catalytic slurry oil comprises the following components: 95.0-99.9%, modifier: 0.1 to 5.0 percent; the modifier is one or more of condensed aluminum phosphate and silicon phosphate curing agents. The method can fully utilize the catalytic slurry oil, can improve the problems of poor temperature sensitivity and ageing resistance of the catalytic slurry oil, improves the flash point of the vacuum residue oil, and can be used for preparing road asphalt with excellent performance or a production raw material of the road asphalt.
Description
Technical Field
The invention relates to a method for utilizing catalytic slurry oil, in particular to a method for producing road asphalt.
Background
The catalytic cracking of heavy oil is one of the important secondary processing means in petroleum processing, and in order to reduce the carbon deposition of the catalyst and prolong the service life of the catalyst, a certain proportion of oil slurry is thrown out from a catalytic cracking unit, and is mostly used for producing fuel oil or mixed with residual oil to a coking unit, but the combustion performance of the FCC oil slurry is affected due to the existence of catalyst particles in the FCC oil slurry, and in addition, the catalytic cracking of heavy oil is not the best utilization way in terms of the principle of maximizing the benefit.
In order to increase the value of the FCC slurry oil, some companies have begun to use the slurry oil for the production of bitumen. The most widely used technique is to mix the slurry oil with crude oil and to produce asphalt by vacuum distillation. However, because the oil slurry contains more double bond components, catalyst particles and the like, the catalytic oil slurry has the characteristics of poor high-temperature performance, poor temperature sensitivity and poor aging resistance, which are shown in that the softening point, the dynamic viscosity at 60 ℃, the penetration index and the properties after an aging test of the blended asphalt are poor, and the change is more obvious along with the increase of the addition amount of the asphalt. As a result, either lower grades of road asphalt can be produced or the quality and performance of the original grade asphalt is reduced, and the addition of too much asphalt can affect a series of problems in the process of sale and use.
CN1302841A discloses a method for treating catalytic slurry oil, wherein the catalytic slurry oil needs to be subjected to reduced pressure distillation, and the obtained heavy component is mixed with solvent deoiled asphalt, slag-reduced after oxidation or mixed with reduced pressure residual oil and then oxidized to produce qualified road asphalt.
CN103554926A discloses a low-grade high-grade road asphalt and a preparation method thereof, wherein catalytic slurry oil and normal slag are mixed and then subjected to vacuum distillation, and then the mixture is mixed with one or more of deoiled asphalt, solvent refined extract oil and unmodified hard vacuum residue to prepare the low-grade high-grade road asphalt by a modulation method. The method still cannot solve the problem of poor temperature sensitivity and ageing resistance inherent in the catalytic slurry oil.
CN102559250A discloses a method for producing asphalt blend oil by catalyzing atmospheric distillation of slurry oil. Adding a certain amount of steam partial pressure regulator and peroxide into oil slurry, heating the mixture to 360-420 ℃, and introducing the mixture into a fractionating tower for fractionating to obtain heavy fraction at the bottom of the tower, which is higher than 360 ℃, as asphalt blending oil. The method can obtain the asphalt blending component by adopting an atmospheric distillation method, but does not mention the improvement of the temperature sensitivity and the ageing resistance of the produced road asphalt, and the increase of the viscosity of the heavy oil slurry, namely the blending oil at 100 ℃ after oxidation is mainly caused by distilling out light fractions.
CN 105273421A discloses a catalytic slurry oil utilization method, which comprises the steps of adopting bottom reducing residue oil obtained by vacuum distillation of catalytic slurry oil as a raw material, adding a cross-linking agent into the bottom reducing residue oil to carry out cross-linking condensation reaction to prepare condensed slurry oil, and blending the condensed slurry oil and matrix asphalt to obtain road asphalt, wherein the cross-linking agent is one or more of a peroxide cross-linking agent, a sulfur and sulfide cross-linking agent and a metal oxide. The method utilizes the improved catalytic slurry oil as a modifier for the base asphalt, but specific improvement effects cannot be known from the patented method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a utilization method of catalytic slurry oil. The method can fully utilize the catalytic slurry oil, can improve the problems of poor temperature sensitivity and ageing resistance of the catalytic slurry oil, improves the flash point of the vacuum residue oil, and can be used for preparing road asphalt with excellent performance or a production raw material of the road asphalt.
The invention provides a method for utilizing catalytic slurry oil, which comprises the following steps:
(1) adding a modifier into the catalytic slurry oil, and stirring to prepare modified catalytic slurry oil;
(2) mixing the modified catalytic slurry oil obtained in the step (1) with atmospheric residue oil, then carrying out reduced pressure distillation, and obtaining reduced pressure residue oil after reduced pressure distillation;
wherein, based on the total raw material mass in the step (1), the raw materials are counted by mass fraction,
catalyzing slurry oil: 95.0 to 99.9 percent, preferably 97.0 to 99.8 percent;
modifying agent: 0.1 to 5.0 percent, preferably 0.2 to 3.0 percent;
the modifier is one or more of condensed aluminum phosphate and silicon phosphate curing agents.
The modifier is preferably condensed aluminum phosphate and silicon phosphate curing agent, wherein the mass ratio of the condensed aluminum phosphate to the silicon phosphate curing agent is (1: 9) - (9: 1), and preferably (3: 7) - (7: 3).
The condensed aluminum phosphate can be one or more of aluminum tripolyphosphate, modified aluminum tripolyphosphate and aluminum dihydrogen tripolyphosphate, and the fineness of the condensed aluminum phosphate is more than 325 meshes. The modified aluminum tripolyphosphate can be obtained by a conventional modification method, for example, modification by one or more methods such as an inorganic compound and a surfactant, and the inorganic compound can be one or more compounds containing common modification elements such as silicon, zinc, calcium, magnesium and the like. The fineness of the silicon phosphate curing agent is more than 1000 meshes, and the water content is less than or equal to 0.8 wt%.
The utilization method of the catalytic slurry oil comprises the following raw material components in percentage by mass:
atmospheric residue: 70 to 99 percent, preferably 80 to 97 percent;
modifying the catalytic slurry oil: 1 to 30%, preferably 3 to 20%.
In the utilization method of the catalytic slurry oil, in the step (1), the modifier is added into the catalytic slurry oil heated to 140-200 ℃, preferably into the catalytic slurry oil heated to 150-190 ℃, and the stirring time is 0.5-5.0 hours, preferably 1.0-4.0 hours.
In the step (2) of the utilization method of the catalytic slurry oil, the temperature for mixing the modified catalytic slurry oil obtained in the step (1) and the atmospheric residue is 100-300 ℃, and preferably 120-250 ℃.
In the utilization method of the catalytic slurry oil, the initial boiling point of the obtained vacuum residue is 400-550 ℃, and the initial boiling point is preferably 420-530 ℃, so that the vacuum residue can be directly used as straight-run asphalt or used as a raw material for blending road asphalt.
In the utilization method of the catalytic oil slurry, the oil slurry is catalytic cracking oil slurry and can be one or more of distillate oil catalytic cracking oil slurry, heavy oil catalytic cracking oil slurry, residual oil catalytic cracking oil slurry or distillate oil blending residual oil catalytic cracking oil slurry; the residual oil comprises one or more of atmospheric residual oil and vacuum residual oil, the heavy oil can be obtained by subjecting crude oil to topping treatment, and the distillate oil comprises one or more of Vacuum Gas Oil (VGO) and Atmospheric Gas Oil (AGO).
Compared with the prior art, the invention has the following advantages:
according to the invention, the catalytic oil slurry is modified, unstable double bond components in the oil slurry are subjected to cross-linking condensation and other reactions with a modifier, the obtained modified catalytic oil slurry is mixed and distilled with the atmospheric residue oil, and the heavier components in the modified catalytic oil slurry, which are beneficial to improving the performance of the asphalt, are retained in the vacuum residue oil through mass transfer, so that the temperature sensitivity of the asphalt, especially the high-temperature anti-rutting performance, is further improved, the ageing resistance of the asphalt is improved, the flash point of the asphalt is also improved, and the heating safety index of the asphalt is ensured.
The invention opens up a feasible way for effectively utilizing the catalytic slurry oil, reducing the production cost of the road asphalt and improving the economic benefit of enterprises while improving the performance of the road asphalt.
Detailed Description
The technical solution of the present invention is further described below by way of examples, but these examples are not intended to limit the present invention, and wt% referred to is mass fraction.
Example 1
Heating the catalytic slurry oil to 190 ℃, adding powdery condensed aluminum phosphate (aluminum tripolyphosphate with the fineness of 800 meshes) into the catalytic slurry oil, wherein the catalytic slurry oil accounts for 98.7wt% of the total amount, the condensed aluminum phosphate accounts for 1.3wt% of the total amount, and stirring and mixing at 190 ℃ for 240min to react to obtain the modified catalytic slurry oil.
Adding the modified catalytic slurry oil into atmospheric residuum (with the density of 0.975g/cm at 25℃)3Softening point 32.5 deg.C, flash point 221 deg.C, the same below), wherein the modified catalytic slurry oil accounts for 5wt%, then vacuum distilling to distill off<The yield of the light fraction at 515 ℃ is 36wt%, and the vacuum residue with excellent properties is obtained. The properties are shown in Table 2.
Example 2
The catalytic slurry oil accounted for 95.0wt% of the total amount, and condensed aluminum phosphate (aluminum dihydrogen tripolyphosphate, fineness 800 mesh) accounted for 5.0wt% of the total amount, and the other conditions were the same as in example 1, to obtain a modified catalytic slurry oil.
The conditions for mixing the modified catalytic slurry oil with the atmospheric residue and then distilling under reduced pressure were the same as in example 1. The properties of the vacuum residue are shown in Table 2.
Example 3
The catalytic slurry oil accounts for 99.8wt% of the total amount, the condensed aluminum phosphate accounts for 0.2wt% of the total amount, and other conditions are the same as in example 1, so that the modified catalytic slurry oil is obtained.
The conditions for mixing the modified catalytic slurry oil with the atmospheric residue and then distilling under reduced pressure were the same as in example 1. The properties of the vacuum residue are shown in Table 2.
Example 4
Heating the catalytic slurry oil to 180 ℃, adding a powdery silicon phosphate curing agent (with the fineness of 1000 meshes and the water content of less than or equal to 0.8%) into the catalytic slurry oil, wherein the catalytic slurry oil accounts for 99.1wt% of the total amount, the powdery silicon phosphate curing agent accounts for 0.9wt% of the total amount, and carrying out ordinary stirring and mixing reaction at 180 ℃ for 180min to obtain the modified catalytic slurry oil.
Adding the modified catalytic slurry oil into atmospheric residue, wherein the proportion of the modified catalytic slurry oil accounts for 10 wt%, then carrying out reduced pressure distillation to distill light fraction at the temperature of less than 500 ℃, and the yield of the light fraction is 31wt%, thus obtaining the vacuum residue with excellent properties. The properties are shown in Table 2.
Example 5
The catalytic slurry oil accounts for 95.5wt% of the total amount, the silicon phosphate curing agent accounts for 4.5wt%, and the other conditions are the same as those in example 1, so that the modified catalytic slurry oil is obtained.
The conditions for vacuum distillation after mixing the modified catalytic slurry oil with the atmospheric residue were the same as in example 4. The properties of the vacuum residue are shown in Table 3.
Example 6
The catalytic slurry oil accounts for 99.8wt% of the total amount, the silicon phosphate curing agent accounts for 0.2wt% of the total amount, and the other conditions are the same as in example 4, so that the modified catalytic slurry oil is obtained.
The conditions for vacuum distillation after mixing the modified catalytic slurry oil with the atmospheric residue were the same as in example 4. The properties of the vacuum residue are shown in Table 3.
Example 7
Heating catalytic cracking slurry oil to 180 ℃, adding powdery silicon phosphate curing agent (fineness is 1000 meshes and water content is less than or equal to 0.8 wt%) and condensed aluminum phosphate (aluminum tripolyphosphate, fineness is 800 meshes) into the catalytic slurry oil, wherein the catalytic slurry oil accounts for 98.7wt% of the total amount, the silicon phosphate curing agent accounts for 0.8wt% of the total amount, and the condensed aluminum phosphate accounts for 0.5wt% of the total amount, and carrying out ordinary stirring and mixing reaction at 170 ℃ for 150min to obtain the modified catalytic slurry oil.
The conditions for mixing the modified catalytic slurry oil with the atmospheric residue and then distilling under reduced pressure were the same as in example 1. The properties of the vacuum residue are shown in Table 3.
Example 8
Heating the catalytic slurry oil to 170 ℃, adding a silicon phosphate curing agent (with the fineness of 1000 meshes and the water content of less than or equal to 0.8%) and condensed aluminum phosphate (aluminum tripolyphosphate and the fineness of 800 meshes) into the catalytic slurry oil, wherein the catalytic slurry oil accounts for 99.2wt% of the total amount, the silicon phosphate curing agent accounts for 0.6wt% of the total amount, and the condensed aluminum phosphate accounts for 0.3wt% of the total amount, and performing ordinary stirring and mixing reaction at 170 ℃ for 180min to obtain the modified catalytic slurry oil.
The conditions for vacuum distillation after mixing the modified catalytic slurry oil with the atmospheric residue were the same as in example 4. The properties of the vacuum residue are shown in Table 3.
Comparative example 1
The conditions were the same as in example 4, and no modifier was added to the slurry, and the slurry was stirred and heated at 180 ℃ for 180min to obtain a comparative slurry.
The comparative slurry oil after heat treatment was added to the atmospheric residue of the same example 1, wherein the modified catalytic slurry oil proportion was 10 wt%, and then vacuum distillation was carried out to distill off a light fraction at <500 ℃ with a yield of light components of 33wt%, to obtain a vacuum residue. The properties are shown in Table 2.
TABLE 1 amount of modifier used in examples and comparative examples
| Examples | Condensed aluminum phosphate,% by weight | Silicon phosphate curing agent (wt%) |
| Example 1 | 1.3 | - |
| Example 2 | 5.0 | - |
| Example 3 | 0.2 | - |
| Example 4 | - | 0.9 |
| Example 5 | - | 4.5 |
| Example 6 | - | 0.2 |
| Example 7 | 0.5 | 0.8 |
| Example 8 | 0.3 | 0.6 |
| Comparative example 1 | - | - |
TABLE 2 Properties of vacuum residue obtained in examples and comparative examples
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| Atmospheric residuum, wt.% | 95 | 95 | 95 | 90 | 90 |
| Modified catalytic slurry oil,% by weight | 5 | 5 | 5 | 10 | 10 |
| Penetration (25 deg.C), 0.1mm | 75 | 67 | 80 | 86 | 96 |
| Softening point, DEG C | 47.8 | 49.2 | 46.7 | 46.4 | 45.4 |
| Ductility (10 ℃), cm | 55 | 49 | 64 | 73 | 56 |
| Kinematic viscosity (60 ℃ C.), Pa.s | 188.2 | 197.0 | 183.5 | 181.1 | 152.4 |
| Flash point, DEG C | 330 | 339 | 319 | 310 | 287 |
| Penetration Index (PI) | -0.41 | -0.22 | -0.60 | -0.49 | -1.14 |
| TFOT(163℃，5h) | |||||
| Penetration ratio of | 67.3 | 69.5 | 66.0 | 66.7 | 61.3 |
| Ductility (10 ℃), cm | 13 | 10 | 16 | 14 | 8 |
TABLE 3 Properties of vacuum residue obtained in examples and comparative examples
| Item | Example 5 | Example 6 | Example 7 | Example 8 |
| Atmospheric residuum, wt.% | 90 | 90 | 95 | 90 |
| Modified catalytic slurry oil,% by weight | 10 | 10 | 5 | 10 |
| Penetration (25 deg.C), 0.1mm | 83 | 91 | 71 | 83 |
| Softening point, DEG C | 46.1 | 45.8 | 47.9 | 46.8 |
| Ductility (10 ℃), cm | 71 | 81 | 58 | 75 |
| Kinematic viscosity (60 ℃ C.), Pa.s | 183.4 | 178.0 | 190.4 | 189.5 |
| Flash point, DEG C | 314 | 307 | 332 | 320 |
| Penetration Index (PI) | 0.20 | -0.51 | -0.27 | -0.36 |
| TFOT(163℃，5h) | ||||
| Penetration ratio of | 66.9 | 65.9 | 67.8 | 67.0 |
| Ductility (10 ℃), cm | 12 | 13 | 14 | 15 |
Claims (15)
1. A method of utilizing a catalytic slurry oil comprising:
(1) adding a modifier into the catalytic slurry oil, and stirring to prepare modified catalytic slurry oil;
(2) mixing the modified catalytic slurry oil obtained in the step (1) with atmospheric residue oil, then carrying out reduced pressure distillation, and obtaining reduced pressure residue oil after reduced pressure distillation;
wherein, based on the total raw material mass in the step (1), the raw materials are counted by mass fraction,
catalyzing slurry oil: 95.0 percent to 99.9 percent;
modifying agent: 0.1 to 5.0 percent;
the modifier is one or more of condensed aluminum phosphate and silicon phosphate curing agents.
2. The method of claim 1, wherein: taking the total raw material mass in the step (1) as a reference, and according to mass fraction, catalyzing oil slurry: 97.0 percent to 99.8 percent; modifying agent: 0.2 to 3.0 percent.
3. The method of claim 1, wherein: in the step (1), the modifier is added into the catalytic slurry oil heated to 140-200 ℃, and the stirring time is 0.5-5.0 hours.
4. A method according to claim 3, characterized by: in the step (1), the modifier is added into the catalytic slurry oil heated to 150-190 ℃, and the stirring time is 1.0-4.0 hours.
5. The method of claim 1, wherein: the modifier is condensed aluminum phosphate and a silicon phosphate curing agent, wherein the mass ratio of the condensed aluminum phosphate to the silicon phosphate curing agent is (1: 9) - (9: 1).
6. The method of claim 5, wherein: the modifier is condensed aluminum phosphate and a silicon phosphate curing agent, wherein the mass ratio of the condensed aluminum phosphate to the silicon phosphate curing agent is (3: 7) - (7: 3).
7. The method of claim 1 or 5 or 6, wherein: the condensed aluminum phosphate is one or more of aluminum tripolyphosphate, modified aluminum tripolyphosphate and aluminum dihydrogen tripolyphosphate, and the fineness of the condensed aluminum phosphate is more than 325 meshes; the fineness of the silicon phosphate curing agent is more than 1000 meshes, and the water content is less than or equal to 0.8 wt%.
8. The method of claim 1, wherein: in the step (2), the raw materials comprise the following components in percentage by mass:
atmospheric residue: 70% -99%;
modifying the catalytic slurry oil: 1 to 30 percent.
9. The method of claim 8, wherein: in the step (2), the raw materials comprise the following components in percentage by mass:
atmospheric residue: 80% -97%;
modifying the catalytic slurry oil: 3 to 20 percent.
10. The method of claim 1, wherein: the mixing temperature of the modified catalytic slurry oil obtained in the step (1) and the atmospheric residue oil is 100-300 ℃.
11. The method of claim 10, wherein: the mixing temperature of the modified catalytic slurry oil obtained in the step (1) and the atmospheric residue oil is 120-250 ℃.
12. The method of claim 1, wherein: the initial boiling point of the obtained vacuum residue is 400-550 ℃.
13. The method of claim 1, wherein: the initial boiling point of the obtained vacuum residue is 420-530 ℃.
14. The method of claim 1, wherein: the obtained vacuum residue can be directly used as straight-run asphalt or used as raw material for preparing road asphalt.
15. The method of claim 1, wherein: the catalytic oil slurry is one or more of distillate oil catalytic cracking oil slurry, heavy oil catalytic cracking oil slurry, residual oil catalytic cracking oil slurry or distillate oil blending residual oil catalytic cracking oil slurry; the residual oil comprises one or more of atmospheric residual oil and vacuum residual oil, the heavy oil is obtained by performing topping treatment on crude oil, and the distillate oil comprises one or more of vacuum gas oil and atmospheric gas oil.
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| CN1635051A (en) * | 2003-12-25 | 2005-07-06 | 中国石油化工股份有限公司 | Asphalt aqueous emulsion and method for preparation |
| CN103554926A (en) * | 2013-10-16 | 2014-02-05 | 中国石油化工股份有限公司 | Low-strength and high-grade road asphalt and preparation method thereof |
| CN103773011A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Asphalt regenerant and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5076910A (en) * | 1990-09-28 | 1991-12-31 | Phillips Petroleum Company | Removal of particulate solids from a hot hydrocarbon slurry oil |
| CN1635051A (en) * | 2003-12-25 | 2005-07-06 | 中国石油化工股份有限公司 | Asphalt aqueous emulsion and method for preparation |
| CN103773011A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Asphalt regenerant and preparation method thereof |
| CN103554926A (en) * | 2013-10-16 | 2014-02-05 | 中国石油化工股份有限公司 | Low-strength and high-grade road asphalt and preparation method thereof |
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