CN113621395A - 90A road petroleum asphalt and preparation method thereof - Google Patents
90A road petroleum asphalt and preparation method thereof Download PDFInfo
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- 239000010426 asphalt Substances 0.000 title claims abstract description 70
- 239000003208 petroleum Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920000137 polyphosphoric acid Polymers 0.000 claims abstract description 61
- 239000002893 slag Substances 0.000 claims abstract description 41
- 239000003607 modifier Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 29
- 125000003118 aryl group Chemical group 0.000 claims abstract description 25
- 239000000084 colloidal system Substances 0.000 claims abstract description 11
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 6
- 239000011593 sulfur Substances 0.000 claims abstract description 6
- 238000003723 Smelting Methods 0.000 claims abstract description 3
- 238000010008 shearing Methods 0.000 claims description 62
- 239000003921 oil Substances 0.000 claims description 59
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 58
- 238000003756 stirring Methods 0.000 claims description 52
- 238000006243 chemical reaction Methods 0.000 claims description 49
- 238000004821 distillation Methods 0.000 claims description 37
- 239000000203 mixture Substances 0.000 claims description 37
- 238000004321 preservation Methods 0.000 claims description 30
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000009835 boiling Methods 0.000 claims description 16
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 16
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 11
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 2
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims 1
- 239000010724 circulating oil Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000018109 developmental process Effects 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- 230000001965 increasing effect Effects 0.000 description 7
- 230000032683 aging Effects 0.000 description 4
- 239000010779 crude oil Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000004523 catalytic cracking Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000005062 Polybutadiene Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/026—Working-up pitch, asphalt, bitumen by chemical means reaction with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses No. 90A-grade road petroleum asphalt and a preparation method thereof. The 90A road petroleum asphalt comprises the following raw material components in parts by weight: slag-smelting: 100 parts of (A); polyphosphoric acid: 0.1-2 parts; initiator: 0.02-0.1 part; component regulator: 5-30 parts of a solvent; low-temperature modifier: 1-15 parts; the properties of the normal slag comprise: the flash point is 246-258 ℃, the sulfur content is 2.77-3.63%, and the weight percentage of the saturated component accounts for 26.1-37.7%, the aromatic component accounts for 20.2-34.5%, the colloid accounts for 18.3-24.8%, and the asphaltene accounts for 21.3-30.1%. The invention takes the difficult-to-process inferior normal slag as the raw material to obtain the No. 90A-grade road asphalt which has excellent low-temperature performance and the flash point and other indexes which can meet the standard requirements.
Description
Technical Field
The invention relates to road asphalt and a preparation method thereof, in particular to 90A road petroleum asphalt and a preparation method thereof.
Background
Along with the increasing heaviness of crude oil, the yield of the vacuum residue oil is gradually improved, the heavy metal content, the sulfur content and the like in the residue oil are increased, the processing difficulty of the residue oil for lightening is increased, and the production of asphalt by using inferior residue oil is a simpler processing scheme and has higher economic benefit. The production of Chinese asphalt mainly adopts a distillation blending process, but with the deterioration of residual oil, the relative content of saturated components and asphaltenes in the residual oil is increased, the relative content of aromatic components and colloids is reduced, the association degree of the asphaltenes is increased, and the existing form is more complicated. At the moment, qualified road asphalt is difficult to produce by adopting a simple distillation blending process, and the production of No. 90A road asphalt with higher requirements on crude oil properties is more difficult.
For example, the thick oil of the tower river is an important petroleum resource, but the structural composition and the physical and chemical properties of the thick oil of the tower river are greatly different from those of other oil sources, and the yield of the vacuum residue of the tower river exceeds 70 percent, and the thick oil of the tower river belongs to residue with high sulfur, high carbon residue, high asphaltene and high heavy metal content. The Tahe refining Limited liability company produces Tahe No. 90 grade A asphalt in 2005, and when the asphalt is in the process, the vacuum residue oil penetration is 60-70 ℃, and the flash point is 260-270 ℃. With the lapse of mining time, the tower and river crude oil gradually becomes heavier, the slag-reducing asphaltene content reaches 15% and 23% in 2007 and 2009, respectively, and the asphaltene content exceeds 40% in 2019, under the present situation, the product with the flash point and the low-temperature performance meeting the requirement of No. 90A road asphalt cannot be prepared by adopting the original production process, so that only the residual oil of a tower and river refinery can be coked or No. 60 asphalt can be produced, but the industrial benefit is greatly reduced. Therefore, it is important to develop a production scheme for acceptable 90A bitumen for the currently increasingly inferior crude oils.
CN109593541A discloses No. 90A-grade road petroleum asphalt and a preparation method thereof. The No. 90A-grade road asphalt is prepared from No. 70A-grade road petroleum asphalt, catalytic cracking slurry oil fraction and polyphosphoric acid, the penetration degree of the asphalt is improved through the catalytic cracking slurry oil fraction, and indexes such as viscosity, softening point and the like are improved through the polyphosphoric acid. The method only simply blends a plurality of materials, although the No. 70A road petroleum asphalt can be finally blended into 90A, the ageing resistance and the low-temperature elongation performance of the asphalt are correspondingly reduced due to the addition of the catalytic cracking slurry oil, the flash point of the asphalt is also reduced due to the addition of the light components, and the 90A asphalt cannot be produced by the method.
CN110484009A discloses No. 110 road petroleum asphalt and a preparation method thereof. The method blends and stirs the No. 70 road petroleum asphalt, the three-line wax oil and the polyphosphoric acid to obtain a product which accords with the No. 110A-grade road petroleum asphalt standard, and the preparation process is simple and convenient. But the direct addition of the three-line wax reducing oil reduces the flash point of the asphalt, the direct doping of the polyphosphoric acid does not play the real role, and the delay increasing effect of the three-line wax reducing oil is also inhibited to a certain extent.
CN103102498A discloses a production method of styrene butadiene rubber modified asphalt. The method greatly increases the low-temperature extensibility of the asphalt and solves the problem that the asphalt with high asphaltene and low aromatic substance is difficult to modify. However, the method only increases the low-temperature ductility of the asphalt and does not substantially contribute to the flash point, the ageing resistance and the like of the asphalt.
In conclusion, the above methods are not suitable for producing high-grade road asphalt from degraded raw materials, and the traditional blending method can not enable the obtained product to simultaneously meet the requirements of low-temperature performance and flash point. Therefore, for the raw materials with high asphaltene and low aromatic component, a new asphalt production process needs to be developed in a targeted manner to improve the added value of low-quality resources.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides No. 90A-grade road petroleum asphalt and a preparation method thereof. The invention takes the difficult-to-process inferior normal slag as the raw material to obtain the No. 90A-grade road asphalt which has excellent low-temperature performance and the flash point and other indexes which can meet the standard requirements.
The invention provides 90A road petroleum asphalt which comprises the following raw material components in parts by weight:
slag-smelting: 100 parts of (A);
polyphosphoric acid: 0.1-2 parts, preferably 0.2-1.8 parts;
initiator: 0.02-0.1 part, preferably 0.04-0.1 part;
component regulator: 5-30 parts, preferably 10-25 parts;
low-temperature modifier: 1-15 parts, preferably 3-10 parts;
the properties of the normal slag comprise: the flash point is 246-258 ℃, the sulfur content is 2.77-3.63 wt%, the saturated component accounts for 26.1-37.7 wt%, the aromatic component accounts for 20.2-34.5 wt%, the colloid accounts for 18.3-24.8 wt%, the asphaltene accounts for 21.3-30.1 wt%, and the asphaltene is preferably 21.3-25.0 wt%.
The normal slag also has the following basic properties: the carbon residue value is 19-28 wt%, the nitrogen content is 0.11-0.52 wt%, the total content of nickel and vanadium is 310-365 mu g/g, and the condensation index CI is 0.22-0.30.
The normal slag can be tower and river normal slag or other normal slag meeting the properties. The normal slag is a fraction with an initial boiling point of more than 350 ℃.
The polyphosphoric acid comprises polyphosphoric acid with low phosphoric acid content and polyphosphoric acid with high phosphoric acid content, wherein the polyphosphoric acid with low phosphoric acid content accounts for 20-50% of the total mass of the polyphosphoric acid, and the polyphosphoric acid with high phosphoric acid content accounts for 50-80% of the total mass of the polyphosphoric acid.
The low-phosphoric-acid-content polyphosphoric acid refers to phosphoric acid (as H) contained in polyphosphoric acid3PO4Calculated) is 105-125 percent, preferably 110-120 percent.
The high-phosphoric-acid-content polyphosphoric acid refers to phosphoric acid (as H) contained in polyphosphoric acid3PO4Measured), the mass content is 130-145%, preferably 130-140%.
The initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium metabisulfite, azobisisobutyronitrile, azobisisoheptonitrile and cumene hydroperoxide.
The component regulator is one or more of coker gas oil, extract oil, catalytic slurry oil and coking cycle oil. The component regulator comprises, by mass, 25-50% of a saturated component, 30-60% of an aromatic component, 10-30% of a colloid, and 0-3% of an asphaltene, wherein the boiling range of the component regulator is from 295-310 ℃ at an initial boiling point and from 430-455 ℃ at a final boiling point.
The low-temperature modifier comprises the following components in parts by weight:
aromatic-rich distillate oil: 100 parts of (A);
styrene-butadiene rubber: 5 to 30 parts, preferably 10 to 20 parts.
The mass content of aromatic hydrocarbon of the aromatic hydrocarbon-rich distillate oil is 30-90%, the initial boiling point of the boiling range of the aromatic hydrocarbon-rich distillate oil is 300-315 ℃, the final boiling point of the aromatic hydrocarbon-rich distillate oil is 440-478 ℃, and the aromatic hydrocarbon-rich distillate oil can be one or a mixture of a first-line-reduced extract oil, a second-line-reduced extract oil, a third-line-reduced extract oil and a fourth-line-reduced extract oil, and is preferably one or a mixture of the third-line-reduced extract oil and the fourth-line-reduced extract oil.
The styrene butadiene rubber is one or the mixture of low-temperature poly-Emulsion Styrene Butadiene Rubber (ESBR) and solution polymerized styrene butadiene rubber (SSBR).
The invention also provides a preparation method of the 90A road petroleum asphalt, which comprises the following steps:
(1) preparing a low-temperature modifier;
(2) adding the normal slag and part of polyphosphoric acid which are heated to flow state into a reaction kettle, continuously stirring and heating to reaction temperature, reacting under protective gas, and carrying out heat preservation treatment after the reaction is finished;
(3) adding the rest polyphosphoric acid, the initiator and the component regulator into the material obtained in the step (2), uniformly stirring, and then shearing;
(4) carrying out reduced pressure distillation on the material sheared in the step (3) to obtain slag reduction;
(5) and (3) adding the low-temperature modifier prepared in the step (1) into the slag removed in the step (4), shearing again, then developing under stirring, and obtaining the 90A road petroleum asphalt after the development is finished.
Wherein, the low-temperature modifier in the step (1) adopts the following preparation method:
after being crushed, styrene butadiene rubber is added into preheated aromatic hydrocarbon-rich distillate oil and is sheared under the heating condition to obtain a pre-modifier; the obtained pre-modifier is stirred and developed under inert atmosphere, heat preservation is carried out after the development is finished, and the low-temperature modifier is obtained after the heat preservation is finished.
Further, preparation of low temperature modifierIn the method, the particle size of the pulverized styrene-butadiene rubber is 0.1-3.0 cm, preferably 0.1-1.5 cm. Preheating the aromatic hydrocarbon-rich distillate oil at 100-110 ℃, heating at 120-140 ℃ during shearing, shearing at a speed of 2000-5000 r/min, preferably 3000-4500 r/min, and shearing for 40-120 min, preferably 40-80 min. The weight ratio of the styrene butadiene rubber to the aromatic-rich oil is (5-30): 100, preferably (10-20): 100. The inert atmosphere is inert gas and/or N during development2The stirring speed is 200-500 r/min, the development temperature is 110-120 ℃, and the development time is 120-180 min; the temperature for heat preservation is 80-100 ℃, and the heat preservation time is 3-6 h.
In the step (2), the reaction kettle is a high-pressure reaction kettle, and the initial temperature of the reaction kettle is adjusted to be 100-120 ℃.
In the step (2), the polyphosphoric acid added is polyphosphoric acid having a high phosphoric acid content (which means phosphoric acid contained in polyphosphoric acid as H3PO4Measured), the mass content is 130-145%, preferably 130-140%), and the addition amount is 50-80% of the total mass of the polyphosphoric acid.
In the step (2), the stirring speed is 600-900 r/min. The heating to the reaction temperature is realized by adopting temperature programming heating to the reaction temperature, the heating rate is 1-3 ℃/min, the heating temperature is 130-150 ℃, and the preferable temperature is 135-150 ℃.
In the step (2), the protective gas is inert gas and/or N2The amount of the shielding gas is such that the pressure in the reaction kettle is maintained at 0.2-0.9 MPa, preferably 0.3-0.8 MPa. The reaction time is 3-6 h. The heat preservation treatment condition is that the heat preservation is carried out for 8-12 hours at the temperature of 80-110 ℃.
In the step (3), the polyphosphoric acid added is polyphosphoric acid having a low phosphoric acid content (which means phosphoric acid contained in polyphosphoric acid as H3PO4Calculated) is 105-125 percent, preferably 110-120 percent, and the adding amount is 20-50 percent of the total mass of the polyphosphoric acid.
In the step (3), the shearing speed is 2000-4000 r/min, the shearing time is 40-100 min, and the temperature required by shearing is 130-150 ℃.
In the step (4), the reduced pressure distillation is carried out in a reduced pressure distillation kettle. The reduced pressure distillation conditions are as follows: the temperature of the bottom of the reduced pressure distillation tower is controlled to be above 400 ℃ (converted atmospheric temperature), the final temperature of reduced pressure distillation is 425-440 ℃, and the rotation speed of the rotor in the reduced pressure distillation kettle is 100-300 r/min in the process of reduced pressure distillation.
In the step (5), the shearing rate is 2000-4500 r/min, preferably 3000-4000 r/min, the shearing time is 40-80 min, and the required temperature during shearing is 120-160 ℃, preferably 120-140 ℃. The stirring speed is 300-600 r/min, preferably 400-600 r/min, and the stirring time is 2-4 h. The temperature for development is 130-160 ℃, and preferably 140-160 ℃.
Compared with the prior art, the 90A road petroleum asphalt and the preparation method thereof have the following advantages:
(1) the invention adopts the normal slag with special properties as the raw material, which can influence the normal production of asphalt, for example, the qualified No. 90A grade road asphalt can not be obtained by adopting the existing mode for the tower and river normal slag with high asphaltene content, very special existing form and extremely poor comprehensive performance as the raw material. However, the specific common slag, polyphosphoric acid, an initiator, a component regulator and a low-temperature modifier are cooperatively matched, so that the obtained No. 90A-grade road asphalt has excellent low-temperature performance, and the flash point and other indexes can meet the standard requirements of No. 90A-grade road asphalt.
(2) The polyphosphoric acid is added twice, and the types and reaction conditions of the polyphosphoric acid are different in different adding periods, so that the asphaltene cluster and the chain-shaped light component in the residual oil are subjected to targeted adjustment, the process of replacing the light component by middle fraction is more thorough, the distillation effect is better, and the flash point is improved more obviously.
(3) In addition to polyphosphoric acid added in a specific mode, other suitable component regulators are introduced, the components have synergistic effect, light components in the residual oil are evaporated out and middle fractions are supplemented in a reinforced mixed distillation mode, the composition structure of the residual oil is regulated in a microscopic level, in addition, the introduced low-temperature modifier improves the low-temperature extensibility of the asphalt, and the preparation process of the low-temperature modifier avoids thermal oxidation aging, so that the modifier has better performance and stronger subsequent aging resistance.
(4) According to the invention, the composition structure is adjusted by only introducing a small amount of additives, rather than introducing a large amount of other oil source asphalt for traditional blending, so that the process is simpler, the production cost is lower, and the used additives have high boiling points and no volatilization and are harmless to human bodies and the environment.
Detailed Description
The technical solution of the present invention is further described by the following examples, but these examples do not limit the scope of the present invention, and the wt% referred to is mass fraction.
Example 1
(1) Firstly, crushing 15 parts of solution polymerized styrene butadiene rubber (SSBR) to the particle size of 0.5cm, then adding the crushed SSBR into 100 parts of aromatic-rich distillate oil (the aromatic content is 45wt%, the boiling range is 310-450 ℃) preheated to 110 ℃, and shearing at 130 ℃ for 60min at the shearing speed of 4000 r/min; after shearing, pouring the mixture into a reaction kettle, and stirring and developing the mixture for 120min under the nitrogen atmosphere, wherein the stirring speed is 400r/min, and the development temperature is 115 ℃; after the development is finished, the mixture is placed in a 100 ℃ oven for heat preservation for 5 hours to obtain a low-temperature modifier for later use.
(2) Adding 100 parts of tower river slag (properties shown in Table 1) heated to flow state into a high-pressure reaction kettle at 110 deg.C, stirring, and adding 0.2 part of phosphoric acid (as H)3PO4Calculated) 135 percent of polyphosphoric acid is slowly added into the reaction kettle (after the polyphosphoric acid is added within 3 min), the temperature is programmed to be 140 ℃ according to the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is increased2Carrying out reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 4 h; after the reaction is finished, the mixture is placed in an oven for heat preservation, the heat preservation temperature is 100 ℃, and the heat preservation time is 8 hours.
(3) 0.1 part of phosphoric acid (in terms of H)3PO4Calculated by mass) 110% of polyphosphoric acid is added into the tower and river normal slag reacted in the step (2), after uniform stirring, 0.05 part of dicumyl peroxide and 0.01 part of azobisisobutyronitrile are added, after uniform mixing, 15 parts of component regulator (calculated by mass) are addedAccording to the percentage, the saturated component accounts for 25 percent, the aromatic component accounts for 50 percent, the colloid accounts for 24 percent, and the asphaltene accounts for 1 percent), and the mixed system is subjected to high-speed shearing, wherein the shearing speed is 4000r/min, the shearing time is 50min, and the heating temperature during shearing is 140 ℃.
(4) And (4) putting the mixture obtained in the step (3) into a reduced pressure distillation kettle for reduced pressure distillation, adjusting the rotation speed of the rotor in the kettle to be 300 r/min, and ending the reduced pressure distillation until the temperature reaches 430 ℃ (the normal pressure temperature after conversion) to obtain reduced residue A1.
(5) Adding 5 parts of low-temperature modifier into the slag-reduced A1 obtained in the step (4), and shearing at 130 ℃ for 50min at the shearing rate of 4000 r/min; after shearing, stirring and developing at 140 ℃, wherein the stirring speed is 400r/min, the stirring time is 3h, and 90A asphalt A11 is obtained after the development is finished, and the specific properties are shown in Table 2.
Example 2
(1) Firstly, crushing 15 parts of solution polymerized styrene butadiene rubber (SSBR) to the particle size of 0.5cm, then adding the crushed SSBR into 100 parts of aromatic-rich distillate oil (the aromatic content is 45wt%, the boiling range is 310-450 ℃) preheated to 110 ℃, and shearing at 130 ℃ for 60min at the shearing speed of 4000 r/min; after shearing, pouring the mixture into a reaction kettle, and stirring and developing the mixture for 120min under the nitrogen atmosphere, wherein the stirring speed is 400r/min, and the development temperature is 115 ℃; after the development is finished, the mixture is placed in a 100 ℃ oven for heat preservation for 5 hours to obtain a low-temperature modifier for later use.
(2) Adding 100 parts of the tower river slag (properties shown in Table 1) into a high-pressure reaction kettle at 110 deg.C, stirring, and adding 0.1 part of phosphoric acid (as H)3PO4Calculated) 135 percent of polyphosphoric acid is slowly added into the reaction kettle (after the polyphosphoric acid is added within 3 min), the temperature is programmed to be 140 ℃ according to the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is increased2Carrying out reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 4 h; after the reaction is finished, the mixture is placed in an oven for heat preservation, the heat preservation temperature is 100 ℃, and the heat preservation time is 8 hours.
(3) 0.1 part of phosphoric acid (in terms of H)3PO4Calculated) 115 percent polyphosphoric acid is added into the tower and river normal slag reacted in the step (2), 0.05 part of peroxide is added after the mixture is evenly stirredAfter uniformly mixing benzoyl and 0.01 part of azobisisobutyronitrile, adding 18 parts of component regulator (the saturated component accounts for 25%, the aromatic component accounts for 50%, the colloid accounts for 24%, and the asphaltene accounts for 1%), and shearing the mixed system at a high speed of 4000r/min for 50min at a heating temperature of 140 ℃.
(4) And (4) putting the mixture obtained in the step (3) into a reduced pressure distillation kettle for reduced pressure distillation, adjusting the rotation speed of the rotor in the kettle to be 300 r/min, and ending the reduced pressure distillation to 433 ℃ (the converted normal pressure temperature) to obtain reduced residue A2.
(5) Adding 5 parts of low-temperature modifier into the slag-reduced A2 in the step (4), and shearing at 130 ℃ for 50min at the shearing rate of 4000 r/min; and after shearing, stirring and developing at 140 ℃, wherein the stirring speed is 400r/min, the stirring time is 3h, and 90A asphalt A22 is obtained after the development is finished.
Example 3
(1) Firstly, 13 parts of low-temperature poly-latex butadiene rubber (ESBR) is crushed to the particle size of 0.5cm, then the crushed ESBR is added into 100 parts of aromatic-rich distillate oil (the aromatic content is 50 wt%, the process is 310-460 ℃) preheated to 110 ℃, and the mixture is sheared for 60min at the temperature of 130 ℃, and the shearing speed is 3600 r/min; after shearing, pouring the mixture into a reaction kettle, and stirring and developing the mixture for 120min under the nitrogen atmosphere, wherein the stirring speed is 400r/min, and the development temperature is 115 ℃; after the development is finished, the mixture is placed in an oven with the temperature of 100 ℃ for heat preservation for 4 hours to obtain the low-temperature modifier for later use.
(2) Adding 100 parts of the tower river slag (properties shown in Table 1) into a high-pressure reaction kettle at the temperature of 110 ℃, stirring, and adding 0.2 part of phosphoric acid (expressed as H)3PO4Calculated) 135 percent of polyphosphoric acid is slowly added into the reaction kettle (after the polyphosphoric acid is added within 3 min), the temperature is programmed to be 140 ℃ according to the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is increased2Carrying out reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5 MPa, and the reaction time is 4 h; after the reaction is finished, the mixture is placed in an oven for heat preservation, the heat preservation temperature is 100 ℃, and the heat preservation time is 8 hours.
(3) 0.2 part of phosphoric acid (in terms of H)3PO4Calculated) 110 percent of polyphosphoric acid is added into the tower and river normal slag after the reaction in the step (2),after stirring uniformly, adding 0.06 part of dicumyl peroxide, after mixing uniformly, adding 18 parts of component regulator (the saturated component accounts for 20%, the aromatic component accounts for 55%, the colloid accounts for 24.5%, and the asphaltene accounts for 0.5%), and carrying out high-speed shearing on the mixed system, wherein the shearing speed is 4000r/min, the shearing time is 50min, and the heating temperature during shearing is 140 ℃.
(4) And (4) putting the mixture obtained in the step (3) into a reduced pressure distillation kettle for reduced pressure distillation, adjusting the rotation speed of the rotor in the kettle to be 300 r/min, and ending the reduced pressure distillation until the temperature reaches 430 ℃ (the normal pressure temperature after conversion) to obtain reduced residue A3.
(5) Adding 6 parts of low-temperature modifier into the slag-reduced A3 in the step (4), and shearing at 130 ℃ for 50min at the shearing rate of 4000 r/min; and after shearing, stirring and developing at 140 ℃, wherein the stirring speed is 400r/min, the stirring time is 3h, and 90A asphalt A33 is obtained after the development is finished.
Example 4
(1) Firstly, crushing 15 parts of low-temperature poly-latex butadiene rubber (ESBR) to the particle size of 1cm, then adding the crushed ESBR into 100 parts of aromatic-rich distillate oil preheated to 110 ℃ (the aromatic content is 45wt%, the range is 305-450 ℃), and shearing at 130 ℃ for 60min at the shearing speed of 4000 r/min; after shearing, pouring the mixture into a reaction kettle, and stirring and developing the mixture for 120min under the nitrogen atmosphere, wherein the stirring speed is 400r/min, and the development temperature is 115 ℃; after the development is finished, the mixture is placed in a 100 ℃ oven for heat preservation for 5 hours to obtain a low-temperature modifier for later use.
(2) Adding 100 parts of the tower river slag (properties shown in Table 1) into a high-pressure reaction kettle at 110 deg.C, stirring, and adding 0.3 part of phosphoric acid (expressed as H)3PO4Calculated) 135 percent of polyphosphoric acid is slowly added into the reaction kettle (after the polyphosphoric acid is added within 3 min), the temperature is increased to 135 ℃ according to the speed program of 1.5 ℃/min under the stirring speed of 600r/min, and N is added after the temperature increase is finished2Carrying out reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.4 MPa, and the reaction time is 4 h; after the reaction is finished, the mixture is placed in an oven for heat preservation, the heat preservation temperature is 100 ℃, and the heat preservation time is 8 hours.
(3) 0.15 part of phosphoric acid (in terms of H)3PO4Calculated) 115% of polyphosphoric acid is added into the mixture obtained in the step (2) for reactionAfter uniformly stirring, adding 0.05 part of benzoyl peroxide and 0.01 part of azodiisobutyronitrile, uniformly mixing, adding 15 parts of component regulators (30% of saturated component, 56% of aromatic component, 14% of colloid and 0% of asphaltene), and shearing the mixed system at a high speed of 4000r/min for 50min at a heating temperature of 140 ℃.
(4) And (4) putting the mixture obtained in the step (3) into a reduced pressure distillation kettle for reduced pressure distillation, adjusting the rotation speed of the rotor in the kettle to be 200 r/min, and ending the reduced pressure distillation to 425 ℃ (the normal pressure temperature after conversion) to obtain the reduced residue A4.
(5) Adding 8 parts of low-temperature modifier into the slag-reducing A4 in the step (4), and shearing at 135 ℃ for 45min at a shearing rate of 4500 r/min; and after shearing, stirring and developing at 140 ℃, wherein the stirring speed is 400r/min, the stirring time is 3h, and 90A asphalt A44 is obtained after the development is finished.
Comparative example 1
(1) A low temperature modifier was prepared as in example 1.
(2) Directly putting the tower and river normal slag into a reduced pressure distillation kettle for reduced pressure distillation, adjusting the rotation speed of an inner rotor in the kettle to be 300 r/min, and ending the reduced pressure distillation to 430 ℃ (the normal pressure temperature after conversion) to obtain reduced slag B1.
(3) Adding 5 parts of low-temperature modifier into the slag reduction B1 in the step (2), and shearing at 130 ℃ for 50min at the shearing rate of 4000 r/min; and (3) after shearing, stirring and developing at 140 ℃, wherein the stirring speed is 400r/min, the stirring time is 3h, and 90A asphalt B11 is obtained after the development is finished.
Comparative example 2
(1) A low temperature modifier was prepared as in example 1.
(2) Adding 15 parts of component regulator (the saturated component accounts for 25%, the aromatic component accounts for 50%, the colloid accounts for 24%, and the asphaltene accounts for 1%) into 100 parts of the Tahe normal slag, and shearing the mixed system at a high speed of 4000r/min for 50min at a heating temperature of 140 ℃.
(3) And (3) putting the mixture obtained in the step (2) into a reduced pressure distillation kettle for reduced pressure distillation, adjusting the rotation speed of the rotor in the kettle to be 300 r/min, and ending the reduced pressure distillation until the temperature reaches 430 ℃ (the normal pressure temperature after conversion) to obtain the slag-reduced B2.
(4) Adding 5 parts of low-temperature modifier into the slag reduction B2 in the step (3), and shearing at 130 ℃ for 50min at the shearing rate of 4000 r/min; and (3) after shearing, stirring and developing at 140 ℃, wherein the stirring speed is 400r/min, the stirring time is 3h, and 90A asphalt B22 is obtained after the development is finished.
Comparative example 3
Same as example 1, except that the phosphoric acid content (in terms of H) was not added in an amount of 0.1 part during the preparation3PO4Calculated) 110% polyphosphoric acid, 0.05 parts dicumyl peroxide, and 0.01 parts azobisisobutyronitrile. This comparative example yielded a vacuum residue of B3 and a 90A pitch of B33.
Comparative example 4
Same as example 1, except that 0.2 part of phosphoric acid (as H) was not added during the preparation3PO4Calculated) 135% of the polyphosphoric acid was reacted. This comparative example yielded a vacuum residue of B4 and a 90A pitch of B44.
Test example
Key indexes of the tower river slag reduction and 90A asphalt obtained in the examples and the comparative examples are tested (according to road engineering asphalt and asphalt mixture test regulation JTG E20-2011), and all indexes of the qualified 90A asphalt product meet the relevant requirements of technical requirements of road petroleum asphalt JTG F40-2004.
TABLE 1 Properties of Tahe Normal slag used in examples and comparative examples
| Density (20 ℃ C.)/(g/cm)3） | 1.0211 |
| Carbon residue value/wt% | 24.1 |
| Flash point (open)/°c | 248 |
| Carbon content/wt% | 87.02 |
| Hydrogen content/wt% | 8.67 |
| Sulfur content/wt.% | 2.86 |
| Fraction of saturation/%) | 29.8 |
| Fraction of aroma/%) | 28.7 |
| Percent of pectin | 19.4 |
| Asphaltene/% | 22.1 |
| Nickel content/(μ g/g) | 43.8 |
| Vanadium content/(μ g/g) | 271.1 |
| Kinematic viscosity (80 ℃ C.)/(mm)2/s） | ＞20000 |
| Kinematic viscosity (100 ℃ C.)/(mm)2/s） | 6596 |
| Condensation index CI | 0.23 |
TABLE 2 Properties of the reduced slag and 90A asphalts obtained in the examples and comparative examples
| Penetration/0.1 mm at 25 ℃ | Softening point/. degree.C | Ductility/cm at 15 DEG C | Flash point/. degree.C | PI value | Viscosity at 60 ℃ in Pa.s | |
| Standard requirements | 80～100 | ≥45 | ≥100 | ≥245 | -1.5～+1.0 | ≥160 |
| A1 | 62 | 53 | 21 | 267 | 0.826 | 1473 |
| A11 | 91 | 48 | 107 | 255 | 0.571 | 401 |
| A2 | 61 | 54 | 23 | 267 | 0.979 | 1544 |
| A22 | 92 | 49 | 114 | 256 | 0.741 | 421 |
| A3 | 58 | 57 | 35 | 264 | 1.106 | 1347 |
| A33 | 90 | 50 | 124 | 252 | 0.512 | 336 |
| A4 | 57 | 62 | 39 | 263 | 1.145 | 1488 |
| A44 | 89 | 57 | 133 | 249 | 0.667 | 394 |
| B1 | 34 | 73 | 0 | 267 | 2.865 | 2861 |
| B11 | 70 | 65 | 32 | 261 | 1.413 | 873 |
| B2 | 43 | 64 | 6 | 245 | 1.892 | 2174 |
| B22 | 82 | 57 | 37 | 239 | 0.936 | 823 |
| B3 | 50 | 55 | 19 | 263 | 1.662 | 1364 |
| B33 | 87 | 50 | 78 | 252 | 0.701 | 576 |
| B4 | 45 | 61 | 14 | 259 | 1.541 | 1543 |
| B44 | 81 | 58 | 77 | 243 | 0.927 | 601 |
Claims (21)
1. The 90A road petroleum asphalt comprises the following raw material components in parts by weight:
slag-smelting: 100 parts of (A);
polyphosphoric acid: 0.1-2 parts, preferably 0.2-1.8 parts;
initiator: 0.02-0.1 part, preferably 0.04-0.1 part;
component regulator: 5-30 parts, preferably 10-25 parts;
low-temperature modifier: 1-15 parts, preferably 3-10 parts;
the properties of the normal slag comprise: the flash point is 246-258 ℃, the sulfur content is 2.77-3.63 wt%, and the weight percentage of the saturated component is 26.1-37.7%, the weight percentage of the aromatic component is 20.2-34.5%, the weight percentage of the colloid is 18.3-24.8%, and the weight percentage of the asphaltene is 21.3-30.1%.
2. The 90A road petroleum asphalt of claim 1, wherein: the normal slag also has the following properties: the carbon residue value is 19-28 wt%, the nitrogen content is 0.11-0.52 wt%, the total content of nickel and vanadium is 310-365 mu g/g, and the condensation index CI is 0.22-0.30.
3. The 90A road petroleum asphalt according to claim 1 or 2, characterized in that: the normal slag is tower and river normal slag.
4. The 90A road petroleum asphalt of claim 1, wherein: the polyphosphoric acid comprises polyphosphoric acid with low phosphoric acid content and polyphosphoric acid with high phosphoric acid content, wherein the polyphosphoric acid with low phosphoric acid content accounts for 20-50% of the total mass of the polyphosphoric acid, and the polyphosphoric acid with high phosphoric acid content accounts for 50-80% of the total mass of the polyphosphoric acid.
5. The 90A road petroleum asphalt of claim 4, wherein: the polyphosphoric acid with low phosphoric acid content refers to phosphoric acid contained in polyphosphoric acid, and H is used as H3PO4The mass content is 105-125%, preferably 110-120%; the high-phosphoric-acid-content polyphosphoric acid refers to phosphoric acid contained in polyphosphoric acid, and H is used as H3PO4The mass content is 130-145%, preferably 130-140%.
6. The 90A road petroleum asphalt of claim 1, wherein: the initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium metabisulfite, azobisisobutyronitrile, azobisisoheptonitrile and cumene hydroperoxide.
7. The 90A road petroleum asphalt of claim 1, wherein: the component regulator is one or more of coker gas oil, extract oil, catalytic slurry oil and coker circulating oil; the composition condition of the component regulator comprises, by mass, 25-50% of a saturated component, 30-60% of an aromatic component, 10-30% of a colloid and 0-3% of an asphaltene, wherein the initial boiling point of the boiling range is 295-310 ℃, and the final boiling point is 430-455 ℃.
8. The 90A road petroleum asphalt of claim 1, wherein: the low-temperature modifier comprises the following components in parts by weight:
aromatic-rich distillate oil: 100 parts of (A);
styrene-butadiene rubber: 5 to 30 parts, preferably 10 to 20 parts.
9. The 90A road petroleum asphalt of claim 8, wherein: in the aromatic hydrocarbon-rich distillate oil, the mass content of aromatic hydrocarbon is 30-90%, the initial boiling point of the boiling range is 300-315 ℃, and the final boiling point is 440-478 ℃; preferably, the oil is one or a mixture of a first-line-reduced extract oil, a second-line-reduced extract oil, a third-line-reduced extract oil and a fourth-line-reduced extract oil, and further preferably, one or a mixture of the third-line-reduced extract oil and the fourth-line-reduced extract oil.
10. The 90A road petroleum asphalt of claim 8, wherein: the styrene butadiene rubber is one or the mixture of low-temperature poly-emulsion butadiene styrene rubber and solution-polymerized styrene butadiene rubber.
11. A method for preparing 90A road petroleum asphalt according to any one of claims 1 to 10, comprising the steps of:
(1) preparing a low-temperature modifier;
(2) adding the normal slag and part of polyphosphoric acid which are heated to flow state into a reaction kettle, continuously stirring and heating to reaction temperature, reacting under protective gas, and carrying out heat preservation treatment after the reaction is finished;
(3) adding the rest polyphosphoric acid, the initiator and the component regulator into the material obtained in the step (2), uniformly stirring, and then shearing;
(4) carrying out reduced pressure distillation on the material sheared in the step (3) to obtain slag reduction;
(5) and (3) adding the low-temperature modifier prepared in the step (1) into the slag removed in the step (4), shearing again, then developing under stirring, and obtaining the 90A road petroleum asphalt after the development is finished.
12. The method of claim 11, wherein: the low-temperature modifier in the step (1) is prepared by the following method: after being crushed, styrene butadiene rubber is added into preheated aromatic hydrocarbon-rich distillate oil and is sheared under the heating condition to obtain a pre-modifier; the obtained pre-modifier is stirred and developed under inert atmosphere, heat preservation is carried out after the development is finished, and the low-temperature modifier is obtained after the heat preservation is finished.
13. The method of claim 12, wherein: in the preparation method of the low-temperature modifier, the particle size of the pulverized styrene-butadiene rubber is 0.1-3.0 cm, preferably 0.1-1.5 cm; preheating aromatic hydrocarbon-rich distillate oil at the temperature of 100-110 ℃, heating at the temperature of 120-140 ℃ during shearing, shearing at the speed of 2000-5000 r/min, preferably 3000-4500 r/min, and shearing for 40-120 min, preferably 40-80 min; the weight ratio of the styrene butadiene rubber to the aromatic-rich oil is (5-30): 100, preferably (10-20): 100; the inert atmosphere is inert gas and/or N during development2The stirring speed is 200-500 r/min, the development temperature is 110-120 ℃, and the development time is 120-180 min; the heat preservation temperature is 80-100 ℃, and the heat preservation time is 3-6 h.
14. The method of claim 11, wherein: in the step (2), the reaction kettle is a high-pressure reaction kettle, and the initial temperature of the reaction kettle is adjusted to be 100-120 ℃.
15. The method of claim 11, wherein: in the step (2), the added polyphosphoric acid is polyphosphoric acid with high phosphoric acid content.
16. A method according to claim 11 or 14, characterized by: in the step (2), the stirring speed is 600-900 r/min; the heating to the reaction temperature is realized by adopting temperature programming heating to the reaction temperature, the heating rate is 1-3 ℃/min, the heating temperature is 130-150 ℃, and the preferable temperature is 135-150 ℃.
17. A method according to claim 11 or 14, characterized by: in the step (2), the protective gas is inert gas and/or N2The amount of the protective gas is used for maintaining the pressure in the reaction kettle to be 0.2-0.9 MPa, preferably 0.3-0.8 MPa; the reaction time is 3-6 h; the heat preservation treatment condition is that the heat preservation is carried out for 8-12 hours at the temperature of 80-110 ℃.
18. A method according to claim 11 or 15, characterized by: in the step (3), the added polyphosphoric acid is polyphosphoric acid with low phosphoric acid content.
19. The method of claim 11, wherein: in the step (3), the shearing speed is 2000-4000 r/min, the shearing time is 40-100 min, and the temperature required by shearing is 130-150 ℃.
20. The method of claim 11, wherein: in the step (4), the reduced pressure distillation is carried out in a reduced pressure distillation kettle; the reduced pressure distillation conditions are as follows: the temperature of the bottom of the reduced pressure distillation tower is controlled to be above 400 ℃, the final temperature of reduced pressure distillation is 425-440 ℃, and the rotation speed of an inner rotor of the reduced pressure distillation kettle is 100-300 r/min in the reduced pressure distillation process.
21. The method of claim 11, wherein: in the step (5), the shearing rate is 2000-4500 r/min, preferably 3000-4000 r/min, the shearing time is 40-80 min, and the required temperature during shearing is 120-160 ℃, preferably 120-140 ℃; the stirring speed is 300-600 r/min, preferably 400-600 r/min, and the stirring time is 2-4 h; the temperature for development is 130-160 ℃, and preferably 140-160 ℃.
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Effective date of registration: 20231031 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |