CN117660035A - 90A-grade asphalt and preparation method thereof - Google Patents
90A-grade asphalt and preparation method thereof Download PDFInfo
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- CN117660035A CN117660035A CN202211041101.4A CN202211041101A CN117660035A CN 117660035 A CN117660035 A CN 117660035A CN 202211041101 A CN202211041101 A CN 202211041101A CN 117660035 A CN117660035 A CN 117660035A
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- 239000010426 asphalt Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000002893 slag Substances 0.000 claims abstract description 77
- 229920000137 polyphosphoric acid Polymers 0.000 claims abstract description 42
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 239000003607 modifier Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 90
- 239000000306 component Substances 0.000 claims description 65
- 238000003756 stirring Methods 0.000 claims description 62
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 50
- 238000004321 preservation Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 27
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 25
- 239000003921 oil Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 230000035484 reaction time Effects 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 230000003068 static effect Effects 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000012533 medium component Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- 239000000084 colloidal system Substances 0.000 claims description 9
- 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 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 125000003118 aryl group Chemical group 0.000 claims description 8
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 238000005292 vacuum distillation Methods 0.000 claims description 6
- 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 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 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
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000002383 tung oil Substances 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
- WVRNUXJQQFPNMN-VAWYXSNFSA-N 3-[(e)-dodec-1-enyl]oxolane-2,5-dione Chemical compound CCCCCCCCCC\C=C\C1CC(=O)OC1=O WVRNUXJQQFPNMN-VAWYXSNFSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 2
- 229920005652 polyisobutylene succinic anhydride Polymers 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
- 239000002904 solvent Substances 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005496 tempering Methods 0.000 claims 2
- 238000005984 hydrogenation reaction Methods 0.000 description 22
- 239000003054 catalyst Substances 0.000 description 16
- 239000012298 atmosphere Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 239000003208 petroleum Substances 0.000 description 9
- 238000004821 distillation Methods 0.000 description 8
- 230000036961 partial effect Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000010802 sludge Substances 0.000 description 5
- 239000010779 crude oil Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004523 catalytic cracking Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- 239000011273 tar residue Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses No. 90A grade asphalt and a preparation method thereof. The invention relates to No. 90 grade A asphalt, which comprises the following raw material components in parts by weight: anhydride slag reduction: 100 parts; pretreatment components: 20-80 parts; the anhydride slag reduction comprises the following raw material components in parts by weight: inferior slag reduction: 100 parts; anhydride modifier: 2-10 parts of polyphosphoric acid: 0.1-2 parts of initiator: 0.08 to 0.7 portion. The invention takes the difficult-to-treat inferior slag reduction as the raw material to obtain the No. 90A grade asphalt product which has high flash point and low temperature performance and other indexes and can meet the standard requirements.
Description
Technical Field
The invention relates to road petroleum asphalt and a preparation method thereof, in particular to 90A-grade asphalt and a preparation method thereof.
Background
With the increasing heaviness of crude oil, the yield of vacuum residuum is gradually increased, the heavy metal content, sulfur content and the like in residuum are increased, the light processing difficulty of residuum is increased, and the production of asphalt by using inferior residuum is a simpler processing scheme and has higher economic benefit. The Chinese asphalt is produced mainly by adopting a distillation blending process, but with the inferior residual oil, the relative content of saturated components and asphaltenes in the residual oil is increased, the relative content of aromatic components and colloid is reduced, the association degree of asphaltenes is increased, and the existence form is more complex. At the moment, the qualified road asphalt is difficult to produce by adopting a simple distillation blending process, and the production of the No. 90A grade road asphalt with higher requirements on the crude oil properties is more difficult.
For example, the thick oil of the tower river is an important petroleum resource, but the structure 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 belongs to residues with high sulfur, high carbon residue, high asphaltene and high heavy metal content. The Tahe refining Limited liability company starts to produce Tahe No. 90 grade A asphalt in 2005, and the penetration of vacuum residue is 60-70 when the flash point is 260-270 ℃. With the development time, the crude oil of the tower and river gradually becomes heavier, the content of the slag-reducing asphaltene reaches 15% and 23% in 2007 and 2009 respectively, and the content of the asphaltene exceeds 40% in 2019, under the current situation, the original production process is adopted, so that the product with flash point and low temperature performance meeting the requirements of the grade-A road asphalt of No. 90 can not be prepared, and therefore, only the residual oil of the tower and river refinery can be coked or 60-grade asphalt can be produced, but the industrial benefit is greatly reduced. Therefore, it is important to develop a qualified 90A asphalt production scheme for the crude oil which is increasingly inferior at present.
CN109593541a discloses a grade-90 a road petroleum asphalt and a preparation method thereof. The grade-A road asphalt of grade-A90 is prepared from grade-A70 road petroleum asphalt, catalytic cracking slurry oil fraction and polyphosphoric acid, the penetration of the asphalt is improved by the catalytic cracking slurry oil fraction, and indexes such as viscosity, softening point and the like are improved by the polyphosphoric acid. The method simply blends several materials, and although the 70A grade road petroleum asphalt can be blended into 90A finally, the aging resistance and 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 reduced due to the addition of the light components, and the 90A asphalt cannot be produced by the method.
CN110484009a discloses a 110 # road petroleum asphalt and a preparation method thereof. The method mixes and stirs the No. 70 road petroleum asphalt, the three-wire wax oil and the polyphosphoric acid to obtain a product which meets the No. 110A road petroleum asphalt standard, and the preparation process is simple and convenient. However, the direct addition of the three-wire wax oil reduces the flash point of asphalt, the polyphosphoric acid does not exert the real effect, and the extension effect of the three-wire wax oil is inhibited to a certain extent.
CN103102498A discloses a method for producing styrene-butadiene rubber modified asphalt. The method greatly increases the low-temperature extensibility of asphalt and solves the problem of difficult modification of high-asphaltene low-aromatic matrix asphalt. However, this method merely increases the low-temperature elongation of asphalt, and does not substantially contribute to the asphalt flash point, aging resistance, and the like.
In summary, none of the above methods is suitable for producing high grade road asphalt from inferior raw materials, nor is the traditional blending method capable of simultaneously satisfying low temperature performance and flash point requirements of the obtained product. Therefore, for high asphaltene and low aromatic materials, a new asphalt production process needs to be developed specifically 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 asphalt and a preparation method thereof. The invention takes the difficult-to-treat inferior slag reduction as the raw material to obtain the No. 90A grade asphalt product which has high flash point and low temperature performance and other indexes and can meet the standard requirements.
The invention provides 90 # A grade asphalt, which comprises the following raw material components in parts by weight: anhydride slag reduction: 100 parts; pretreatment components: 20 to 80 parts, preferably 40 to 60 parts; the anhydride slag reduction comprises the following raw material components in parts by weight:
inferior slag reduction: 100 parts;
anhydride modifier: 2 to 10 parts, preferably 2 to 8 parts;
polyphosphoric acid: 0.1 to 2 parts, preferably 0.2 to 1.8 parts;
and (3) an initiator: 0.08 to 0.7 part, preferably 0.15 to 0.7 part.
The pretreatment component comprises the following raw material components in parts by weight:
inferior slag reduction: 100 parts;
medium component: 20 to 50 parts, preferably 25 to 40 parts;
light components: 5 to 20 parts, preferably 6 to 15 parts.
The inferior slag reduction in the pretreatment component and the inferior slag reduction in the anhydridized slag reduction can be completely the same or different as long as the following properties are satisfied.
The inferior slag reduction has the following properties: the flash point is 241-256 ℃, the sulfur content is 2.61-3.65 wt%, the saturated fraction is 26.1-37.7 wt%, the aromatic fraction is 20.2-34.5 wt%, the colloid is 18.3-24.8 wt%, the asphaltene is 21.3-30.1 wt%, and the asphaltene is preferably 21.3-26.0 wt%.
The inferior slag reduction also has the following properties: the carbon residue value is 21wt percent to 29wt percent, the nitrogen content is 0.14wt percent to 0.61wt percent, the total content of nickel and vanadium is 320 to 365 mug/g, and the condensation index CI is 0.26 to 0.35.
The inferior slag reduction can be the slag reduction of a tower river or other slag reduction meeting the property, and the inferior slag reduction is the fraction with the initial boiling point of more than 425 ℃.
Further, in the pretreatment component, the medium component refers to colloid obtained after solvent deasphalting, and has the following properties: kinematic viscosity at 100 ℃ of 50mm 2 /s～65mm 2 The flash point is 206-220 ℃, the saturated fraction accounts for 30-42%, the aromatic fraction accounts for 48-57%, the colloid accounts for 8-13% and the asphaltene content is less than 2% in terms of mass fraction; the weight average molecular weight is 1990-2140, and the molecular weight distribution width is 1.6-3.7.
Further, in the pretreatment component, the light component refers to decompressed wax oil, and the light component has the following properties: kinematic viscosity at 50 ℃ of 10mm 2 /s～16mm 2 Density at 20 deg.C of 760-900 kg/m 3 In terms of mass fraction, the saturated fraction accounts for 60% -78%, the aromatic fraction accounts for 20% -32%, and the total content of colloid and asphaltene is less than6%; the carbon residue is less than 0.15%, the sulfur content is less than 0.3%, the nitrogen content is less than 1%, and the hydrogen-carbon ratio is 1.5-1.8.
Further, in the anhydridized slag reduction, the polyphosphoric acid includes polyphosphoric acid with a low polyphosphoric acid content and polyphosphoric acid with a high phosphoric acid content.
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 (H 3 PO 4 Calculated by weight), the mass content is 105 to 125 percent, preferably 110 to 120 percent.
The high phosphoric acid content polyphosphoric acid refers to phosphoric acid (H 3 PO 4 Calculated by weight), the mass content is 130-145%, preferably 130-140%.
Further, in the anhydridization slag reduction, the anhydride modifier is one or more of maleic anhydride, polyisobutylene succinic anhydride, methyl nadic anhydride, modified methyl nadic anhydride, dodecenyl succinic anhydride, tung oil anhydride, polyazeic anhydride, polyglutaric anhydride, polyglycolic anhydride or hydrolyzed polymaleic anhydride.
Further, in the anhydrization slag reduction, the initiator is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium metabisulfite, azobisisobutyronitrile, azobisisoheptonitrile and cumene hydroperoxide.
The invention also provides a preparation method of the No. 90A grade asphalt, which comprises the following steps:
(1) Preparing anhydride slag reduction;
(2) Preparing a pretreatment component;
(3) Blending the material obtained in the step (1) and the material obtained in the step (2) and carrying out static heat preservation treatment to finally obtain the No. 90 grade A asphalt.
Further, in the step (1), the process of preparing the anhydridized slag reduction is as follows:
a. adding the inferior slag reduction and high phosphoric acid content polyphosphoric acid heated to a flowing state into a reaction kettle, heating to a reaction temperature, continuously stirring, reacting under protective gas, and carrying out heat preservation treatment after the reaction is finished;
b. and d, adding polyphosphoric acid with low phosphoric acid content into the material obtained in the step a, stirring uniformly, adding an anhydride modifier and an initiator, continuously stirring, heating to a reaction temperature, reacting under a protective gas, and obtaining the anhydride slag reduction after the reaction is finished.
In the step a, the reaction kettle is a high-pressure reaction kettle, and the initial temperature of the reaction kettle is regulated to be 115-140 ℃.
In the step a, the heating to the reaction temperature is heating to the reaction temperature by adopting temperature programming, the heating rate is 1-3 ℃/min, and the reaction temperature is 140-180 ℃, preferably 145-160 ℃. The reaction time is 3-6 h. The stirring speed is 600-800 r/min.
In the step a, the protective gas is inert gas and/or N 2 The amount of the shielding gas maintains the pressure in the reaction vessel at 0.2 to 0.9MPa, preferably 0.4 to 0.8MPa. The heat preservation treatment condition is that heat preservation is carried out for 10-16 h at 120-135 ℃.
In the step b, the polyphosphoric acid with low phosphoric acid content is added and then stirred for 30 to 50 minutes, and the stirring speed is 300 to 600r/min.
In the step b, the stirring speed after the anhydride modifier and the initiator are added is 600-800 r/min. The heating to the reaction temperature is heating to the reaction temperature by adopting temperature programming, and the heating rate is 1-3 ℃/min. The reaction temperature is 160-180 ℃ and the reaction time is 6-8 h. The shielding gas is inert gas and/or N 2 . The amount of the shielding gas maintains the pressure in the reaction kettle to be 0.3-0.9 MPa, preferably 0.5-0.9 MPa.
Further, in the step (2), the process of preparing the pretreatment component is as follows:
i. mixing the inferior slag reduction heated to a flowing state with a middle-quality component and a light component, and then carrying out hydrotreatment with hydrogen;
and ii, carrying out atmospheric and vacuum distillation on the material obtained in the step i to obtain a final pretreatment component.
In step i, the operating conditions of the hydrotreatment are as follows: the reaction temperature is 365-390 ℃, the reaction pressure is 12-22 MPa, and the volume airspeed is 0.5-1.8 h -1 The volume ratio of hydrogen to oil is 400-1500; preferred operating conditions are: the reaction temperature is 370-390 ℃, the reaction pressure is 13-20 MPa, and the volume airspeed is 0.5-1.2 h -1 The volume ratio of the hydrogen oil is 500-1100.
In step i, the reactor used for the hydrotreatment may be a fixed bed hydrogenation reactor, a ebullated bed hydrogenation reactor or a suspended bed hydrogenation reactor, preferably a ebullated bed hydrogenation reactor.
In the step i, the catalyst used for the hydrotreatment may be a commercially available catalyst, for example, a FF, FH, FZC series catalyst developed by the institute of petrochemical industry, chinese. The catalyst gradation method may be determined according to a conventional method, and is not particularly limited in the present invention.
In step ii, the atmospheric and vacuum distillation is performed in an atmospheric and vacuum still. Wherein the atmospheric distillation has no special requirements. The final temperature of the reduced pressure distillation is 465 to 540 ℃, preferably 485 to 520 ℃.
Further, in the step (3), the stirring speed in the blending process is 700-900 r/min, the stirring time is 4-6 h, and the blending temperature is 140-165 ℃.
In the step (3), the static heat preservation treatment is carried out under the condition of oxygen-enriched air (the oxygen volume content is 40% -55%), the temperature is kept at 135-150 ℃, and the heat preservation time is 6-10 h.
Compared with the prior art, the No. 90A grade asphalt and the preparation method thereof have the following advantages:
(1) The invention adopts inferior slag reduction as a raw material, which is not suitable for producing high-grade road asphalt, such as the slag reduction of a Tahe with high asphaltene content, very special existence form and extremely inferior comprehensive performance. The invention adopts the synergistic combination of the inferior slag reduction agent, the polyphosphoric acid, the initiator and the anhydride modifier, can obtain the anhydride slag reduction agent, and then is matched with the pretreatment component, thereby being capable of being used for preparing qualified grade-90A asphalt, expanding the use of the inferior slag reduction agent and improving the added value thereof.
(2) The pretreatment component is obtained by carrying out hydrotreatment and secondary distillation on inferior slag reduction, medium component and light component, the average molecular structure, molecular weight distribution and the like of the material are regulated and optimized in the treatment process, the continuity of the structure and the composition of the material is enhanced, and the inventor researches find that the pretreatment component is matched with the anhydridized slag reduction in a synergic manner, so that the defect of inferior slag reduction can be overcome.
(3) The pretreatment component introduced by the invention can be well compatible with the anhydration slag reduction, and can give consideration to the high and low temperature performance of asphalt after blending, the colloid structure can be optimized without mixing distillation, and the aging resistance of the asphalt is improved; and the low-temperature extensibility is good, the step of slightly modifying and extending the polymer is omitted, and the finally obtained high-grade road asphalt has the characteristics of high flash point, excellent high-low temperature performance and the like.
Detailed Description
The technical solutions of the present invention are further described below by examples, which are not intended to limit the scope of the present invention, but the wt% referred to is mass fraction.
Example 1
(1) 100 parts of the reduced sludge (part of the properties are shown in Table 1) of the Takara Shuzo heated to a flowing state are added to a high-pressure reaction vessel at a temperature of 120℃and stirred, and 0.2 part of phosphoric acid content (in H 3 PO 4 Calculated as 135 percent of polyphosphoric acid is slowly added into a reaction kettle (the addition is completed within 3 min), and the temperature is programmed to 145 ℃ at the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is raised 2 Carrying out reaction under atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5MPa, and the reaction time is 4 hours; after the reaction is finished, placing the mixture into a reaction kettle for heat preservation, wherein the heat preservation temperature is 120 ℃, and the heat preservation time is 10 hours.
(2) The phosphoric acid content (in H) of 0.1 part 3 PO 4 110% of polyphosphoric acid is added into the reduced slag of the tower river after the reaction in the step (1), and is stirred for 30min at a stirring speed of 600r/min, then 4 parts of maleic anhydride and 0.5 part of dicumyl peroxide are added, and the mixture is lifted according to a speed program of 2 ℃ per minute at a stirring speed of 650r/minHeating to 175 deg.C, and heating to N 2 And (3) carrying out the reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.6MPa, and the reaction time is 6h to obtain the anhydridized slag reduction.
(3) 100 parts of the Tahe slag reduction (step (1)), 30 parts of the medium component (part of the properties are shown in Table 2) and 10 parts of the light component (part of the properties are shown in Table 3) which are heated to a flowing state are heated at a reaction temperature of 380 ℃, a reaction pressure of 16MPa and a volume space velocity of 0.8h -1 The hydrogenation treatment is carried out under the condition that the volume ratio of hydrogen to oil is 900, the hydrogenation catalyst is selected from FZC series catalysts developed by China petrochemical industry institute of large company petrochemical industry, the hydrogenation product is subjected to atmospheric and vacuum distillation, and the distillation product with the temperature higher than 510 ℃ is the required pretreatment component.
(4) And (3) carrying out blending treatment on 100 parts of the anhydridized slag obtained in the step (2) and 40 parts of the pretreatment component obtained in the step (3), wherein the stirring speed is 750r/min, the temperature is 155 ℃, the stirring time is 6h, and the static heat preservation is carried out for 8h under the conditions that the oxygen volume content is 50% and the oxygen volume content is 145 ℃ after the stirring is finished, so that the final grade-A asphalt A1 No. 90 is obtained.
Example 2
(1) 100 parts of the reduced sludge (properties shown in Table 1) of the Takara Shuzo heated to a flowing state were charged into a high-pressure reaction vessel at 120℃and stirred, and 0.25 part of phosphoric acid was added as a component (in H 3 PO 4 Calculated as 135 percent of polyphosphoric acid is slowly added into a reaction kettle (the addition is completed within 3 min), and the temperature is programmed to 145 ℃ at the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is raised 2 Carrying out reaction under atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5MPa, and the reaction time is 6h; after the reaction is finished, placing the mixture into a reaction kettle for heat preservation, wherein the heat preservation temperature is 120 ℃, and the heat preservation time is 16 hours.
(2) The phosphoric acid content (in H) of 0.1 part 3 PO 4 Calculated as 110 percent, adding polyphosphoric acid into the reduced slag of the tower river after the reaction in the step (1), stirring for 30 minutes at a stirring speed of 600r/min, adding 4.75 parts of tung oil anhydride and 0.6 part of dicumyl peroxide, heating to 175 ℃ at a stirring speed of 650r/min according to a speed program of 2 ℃/min, and adding N after the heating is finished 2 The reaction is carried out in atmosphere, the pressure in the reaction kettle is maintained at 0.8MPa, and the reaction time is 6h to obtain the anhydration reductionSlag.
(3) 100 parts of the Tahe slag reduction (step (1)), 25 parts of the medium component (part of the properties are shown in Table 2) and 15 parts of the light component (part of the properties are shown in Table 3) which are heated to a flowing state are heated at a reaction temperature of 380 ℃, a reaction pressure of 16MPa and a volume space velocity of 0.8h -1 The hydrogenation treatment is carried out under the condition that the volume ratio of hydrogen to oil is 900, the hydrogenation catalyst is selected from FZC series catalysts developed by China petrochemical industry institute of great company petrochemical industry, the hydrogenation product is distilled under normal and reduced pressure, and the distilled product with the temperature higher than 515 ℃ is the required pretreatment component.
(4) And (3) carrying out blending treatment on 100 parts of the anhydridized slag obtained in the step (2) and 45 parts of the pretreatment component obtained in the step (3), wherein the stirring speed is 750r/min, the temperature is 155 ℃, the stirring time is 6h, and the static heat preservation is carried out for 8h under the conditions that the oxygen volume content is 50% and the oxygen volume content is 145 ℃ after the stirring is finished, so that the final grade-A90 asphalt A2 is obtained.
Example 3
(1) 100 parts of the reduced sludge (properties shown in Table 1) of the Takara Shuzo heated to a flowing state were charged into a high-pressure reaction vessel at 120℃and stirred, and 0.2 part of phosphoric acid was added as a content (in H 3 PO 4 Calculated as 135 percent of polyphosphoric acid is slowly added into a reaction kettle (the addition is completed within 3 min), and the temperature is programmed to 145 ℃ at the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is raised 2 Carrying out reaction under atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5MPa, and the reaction time is 4 hours; after the reaction is finished, placing the mixture into a reaction kettle for heat preservation, wherein the heat preservation temperature is 120 ℃, and the heat preservation time is 10 hours.
(2) The phosphoric acid content (in H) of 0.2 part 3 PO 4 110% of polyphosphoric acid is added into the reduced slag of the tower river after the reaction in the step (1), 5 parts of maleic anhydride, 0.5 part of dicumyl peroxide and 0.1 part of azodiisobutyronitrile are added after stirring for 30min at a stirring speed of 600r/min, the temperature is increased to 180 ℃ at a stirring speed of 650r/min according to a speed program of 2 ℃/min, and N is added after the temperature is increased 2 And (3) carrying out the reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.6MPa, and the reaction time is 6h to obtain the anhydridized slag reduction.
(3) 100 parts of the waste residue of the Tahe heated to a flowing state (step (1)),35 parts of medium component (partial properties are shown in Table 2) and 8 parts of light component (partial properties are shown in Table 3) at a reaction temperature of 385 ℃, a reaction pressure of 15MPa and a volume space velocity of 1.0h -1 The hydrogenation treatment is carried out under the condition that the volume ratio of hydrogen to oil is 1000, the hydrogenation catalyst is selected from FH series catalysts developed by China petrochemical industry institute of great company petrochemical industry, the hydrogenation product is distilled under normal and reduced pressure, and the distilled product with the temperature higher than 520 ℃ is the required pretreatment component.
(4) And (3) carrying out blending treatment on 100 parts of the anhydridized slag obtained in the step (2) and 50 parts of the pretreatment component obtained in the step (3), wherein the stirring speed is 750r/min, the temperature is 155 ℃, the stirring time is 6h, and the static heat preservation is carried out for 8h under the conditions that the oxygen volume content is 50% and the oxygen volume content is 145 ℃ after the stirring is finished, so that the final 90 # A-grade asphalt A3 is obtained.
Example 4
(1) 100 parts of the reduced sludge (properties shown in Table 1) of the Takara Shuzo heated to a flowing state were charged into a high-pressure reaction vessel at a temperature of 125℃and stirred, and 0.4 part of phosphoric acid was added as a component (in H 3 PO 4 140% of polyphosphoric acid is slowly added into a reaction kettle (the addition is completed within 5 min), the temperature is programmed to 160 ℃ at the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is raised 2 Carrying out reaction under atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5MPa, and the reaction time is 6h; after the reaction is finished, placing the mixture into a reaction kettle for heat preservation, wherein the heat preservation temperature is 120 ℃, and the heat preservation time is 16 hours.
(2) The phosphoric acid content (in H) of 0.3 part 3 PO 4 110% of polyphosphoric acid is added into the reduced slag of the tower river after the reaction in the step (1), and 4.75 parts of maleic anhydride, 0.5 part of dicumyl peroxide and 0.2 part of benzoyl peroxide are added after stirring for 30min at a stirring speed of 600r/min, and the temperature is increased to 175 ℃ according to a speed program of 2 ℃/min at a stirring speed of 700r/min, and then the mixture is heated to N after the temperature is increased 2 And (3) carrying out the reaction under the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.6MPa, and the reaction time is 8 hours, so as to obtain the anhydridized slag reduction.
(3) 100 parts of the Tahe slag reduction (step (1)), 40 parts of the medium component (part of the properties are shown in Table 2) and 15 parts of the light component (part of the properties are shown in Table 3) heated to a flowing state are reacted at a reaction temperature of 385 DEG CThe stress is 15MPa, and the volume space velocity is 1.0h -1 The hydrogenation treatment is carried out under the condition that the volume ratio of hydrogen to oil is 1000, the hydrogenation catalyst is selected from FH series catalysts developed by China petrochemical industry institute of great company petrochemical industry, the hydrogenation product is distilled under normal and reduced pressure, and the distilled product with the temperature higher than 520 ℃ is the required pretreatment component.
(4) And (3) carrying out blending treatment on 100 parts of the anhydridized slag obtained in the step (2) and 40 parts of the pretreatment component obtained in the step (3), wherein the stirring speed is 800r/min, the temperature is 160 ℃, the stirring time is 6h, and the static heat preservation is carried out for 7h under the conditions that the oxygen volume content is 45% and the temperature is 150 ℃ after the stirring is finished, so that the final 90 # A-grade asphalt A4 is obtained.
Comparative example 1
(1) An anhydrified slag reduction was prepared as in example 1.
(2) Mixing 100 parts of the Tahe slag reduction (in step (1)), 40 parts of the medium component (the partial properties are shown in table 2) and 15 parts of the light component heated to a flowing state directly to obtain a mixed material;
(3) Directly blending 100 parts of the anhydride slag reduction in the step (1) with 40 parts of the mixed material obtained in the step (2), wherein the stirring speed is 800r/min, the temperature is 160 ℃, the stirring time is 6h, and the static heat preservation is carried out for 7h under the conditions that the oxygen volume content is 45% and the temperature is 150 ℃ after the stirring is finished, so that the final asphalt B1 is obtained.
Comparative example 2
The same as in example 1, except that the slag reduction was not subjected to the acid anhydride pretreatment during the preparation process, the final asphalt B2 was obtained, specifically:
(1) 100 parts of the Tahe slag reduction (same as in example 1), 30 parts of the medium component (partial properties are shown in Table 2) and 10 parts of the light component (partial properties are shown in Table 3) heated to a flowing state are reacted at a reaction temperature of 380 ℃, a reaction pressure of 16MPa and a volume space velocity of 0.8h -1 The hydrogenation treatment is carried out under the condition that the volume ratio of hydrogen to oil is 900, the hydrogenation catalyst is selected from FZC series catalysts developed by China petrochemical industry institute of large company petrochemical industry, the hydrogenation product is subjected to atmospheric and vacuum distillation, and the distillation product with the temperature higher than 510 ℃ is the required pretreatment component.
(2) 100 parts of the Tahe slag reduction (same as in example 1) and 40 parts of the pretreatment component obtained in (1) are subjected to blending treatment, wherein the stirring speed is 750r/min, the temperature is 155 ℃, the stirring time is 6h, and the static heat preservation is carried out for 8h under the conditions that the oxygen volume content is 50% and the temperature is 145 ℃ after the stirring is finished, so that the final asphalt B2 is obtained.
Comparative example 3
As in example 1, except that polyphosphoric acid was not introduced during the slag reduction anhydrization, B3 was finally obtained. The method comprises the following steps:
(1) Adding 4 parts of maleic anhydride and 0.5 part of dicumyl peroxide into 100 parts of Tar residue (part of properties are shown in Table 1) heated to a flowing state at a stirring speed of 600r/min, stirring for 30min, heating to 175 ℃ at a stirring speed of 650r/min according to a speed program of 2 ℃/min, and adding N after heating 2 And (3) carrying out the reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.6MPa, and the reaction time is 6h to obtain the anhydridized slag reduction.
(2) 100 parts of the Tahe slag reduction (step (1)), 30 parts of the medium component (part of the properties are shown in Table 2) and 10 parts of the light component (part of the properties are shown in Table 3) which are heated to a flowing state are heated at a reaction temperature of 380 ℃, a reaction pressure of 16MPa and a volume space velocity of 0.8h -1 The hydrogenation treatment is carried out under the condition that the volume ratio of hydrogen to oil is 900, the hydrogenation catalyst is selected from FZC series catalysts developed by China petrochemical industry institute of large company petrochemical industry, the hydrogenation product is subjected to atmospheric and vacuum distillation, and the distillation product with the temperature higher than 510 ℃ is the required pretreatment component.
(3) And (3) carrying out blending treatment on 100 parts of the anhydridized slag obtained in the step (1) and 40 parts of the pretreatment component obtained in the step (2), wherein the stirring speed is 750r/min, the temperature is 155 ℃, the stirring time is 6h, and the static heat preservation is carried out for 8h under the conditions that the oxygen volume content is 50% and the temperature is 145 ℃ after the stirring is finished, so as to obtain the final asphalt B3.
Comparative example 4
As in example 1, but without introducing pretreatment components during the preparation, B4 was finally obtained. The method comprises the following steps:
(1) 100 parts of the reduced sludge (part of the properties are shown in Table 1) of the Takara Shuzo heated to a flowing state are added to a high-pressure reaction vessel at a temperature of 120℃and stirred, and 0.2 part of phosphoric acid content (in H 3 PO 4 Calculated as 135% polyphosphoric acid was slowly added to the reactionA kettle (the addition is completed within 3 min), the temperature is programmed to 145 ℃ at the speed of 2 ℃/min under the stirring speed of 600r/min, and N is added after the temperature is raised 2 Carrying out reaction under atmosphere, wherein the pressure in the reaction kettle is maintained at 0.5MPa, and the reaction time is 4 hours; after the reaction is finished, placing the mixture into a reaction kettle for heat preservation, wherein the heat preservation temperature is 120 ℃, and the heat preservation time is 10 hours.
(2) The phosphoric acid content (in H) of 0.1 part 3 PO 4 110% of polyphosphoric acid is added into the reduced slag of the tower river after the reaction in the step (1), and 4 parts of maleic anhydride and 0.5 part of dicumyl peroxide are added after stirring for 30min at a stirring speed of 600r/min, and the temperature is programmed to 175 ℃ at a speed of 2 ℃ per min at a stirring speed of 650r/min, and then N is added after the temperature is increased 2 And (3) carrying out the reaction in the atmosphere, wherein the pressure in the reaction kettle is maintained at 0.6MPa, and the reaction time is 6h to obtain the anhydridized slag reduction.
(3) And (3) carrying out blending treatment on 100 parts of the anhydration slag obtained in the step (2), wherein the stirring speed is 750r/min, the temperature is 155 ℃, the stirring time is 6h, and the static heat preservation is carried out for 8h under the conditions that the oxygen volume content is 50% and the temperature is 145 ℃ after the stirring is finished, so as to obtain the final asphalt B4.
Test case
And (3) carrying out key index tests on the reduced slag, the middle-quality component, the light component and the 90A asphalt obtained in the examples and the comparative examples (according to the highway engineering asphalt and asphalt mixture test procedure JTG E20-2011), wherein each index of the qualified 90A asphalt product is required to meet the related requirements of the technical requirement JTG F40-2004 of road petroleum asphalt.
Table 1 properties of the slag-reduced portion of the talents used in examples and comparative examples
TABLE 2 partial Properties of the mesogenic Components used in examples and comparative examples
| Saturation fraction/wt% | 32.37 |
| Fragrance fraction/wt% | 56.15 |
| Gum/wt% | 11.41 |
| Asphaltenes/wt% | 0.07 |
| Kinematic viscosity at 100 ℃ per mm 2 /s | 53 |
| Flash point/. Degree.C | 213 |
| Weight average molecular weight | 2135 |
| Width of molecular weight distribution | 2.2 |
TABLE 3 partial Properties of the light Components used in examples and comparative examples
Table 4 principal properties of examples and comparative examples
The scope of the invention is not limited by the embodiments described above, but is defined by the claims. Those skilled in the art can make appropriate modifications to these embodiments without departing from the technical spirit and scope of the present invention, and these modified embodiments are also included in the scope of the present invention.
Claims (16)
1. The No. 90A grade asphalt comprises the following raw material components in parts by weight: anhydride slag reduction: 100 parts; pretreatment components: 20 to 80 parts, preferably 40 to 60 parts; the anhydride slag reduction comprises the following raw material components in parts by weight:
inferior slag reduction: 100 parts;
anhydride modifier: 2 to 10 parts, preferably 2 to 8 parts;
polyphosphoric acid: 0.1 to 2 parts, preferably 0.2 to 1.8 parts;
and (3) an initiator: 0.08 to 0.7 part, preferably 0.15 to 0.7 part.
2. The grade 90a asphalt of claim 1, wherein the pretreatment component comprises the following raw material components by weight:
inferior slag reduction: 100 parts;
medium component: 20 to 50 parts, preferably 25 to 40 parts;
light components: 5 to 20 parts, preferably 6 to 15 parts.
3. The grade No. 90a asphalt of claim 1 or 2, wherein the inferior slag reduction has the following properties: flash point 241-256 deg.c, sulfur content 2.61-3.65 wt%, saturated fraction 26.1-37.7 wt%, aromatic fraction 20.2-34.5 wt%, colloid 18.3-24.8 wt%, asphaltene 21.3-30.1 wt% and/or,
the inferior slag reduction also has the following properties: the carbon residue value is 21wt percent to 29wt percent, the nitrogen content is 0.14wt percent to 0.61wt percent, the total content of nickel and vanadium is 320 to 365 mug/g, and the condensation index CI is 0.26 to 0.35.
4. The grade-90 a asphalt of claim 2, wherein the pretreatment component is a gum obtained after solvent deasphalting, and the pretreatment component has the following properties: kinematic viscosity at 100 ℃ of 50mm 2 /s～65mm 2 The flash point is 206-220 ℃, the saturated fraction accounts for 30-42%, the aromatic fraction accounts for 48-57%, the colloid accounts for 8-13% and the asphaltene content is less than 2% in terms of mass fraction; the weight average molecular weight is 1990-2140, and the molecular weight distribution width is 1.6-3.7.
5. The grade 90a asphalt of claim 2, wherein the light component in the treatment composition is a vacuum wax oil, and the light component has the following properties: kinematic viscosity at 50 ℃ of 10mm 2 /s～16mm 2 Density at 20 deg.C of 760-900 kg/m 3 The saturated fraction accounts for 60 to 78 percent, the aromatic fraction accounts for 20 to 32 percent, and the total content of colloid and asphaltene is less than 6 percent; the carbon residue is less than 0.15%, the sulfur content is less than 0.3%, the nitrogen content is less than 1%, and the hydrogen-carbon ratio is 1.5-1.8.
6. The grade-90 a asphalt of claim 1, wherein in the anhydrified slag reduction, the polyphosphoric acid comprises polyphosphoric acid with a low polyphosphoric acid content and polyphosphoric acid with a high phosphoric acid content; 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.
7. The grade-90 a asphalt of claim 1, wherein the anhydride modifier is one or more of maleic anhydride, polyisobutylene succinic anhydride, methylnadic anhydride, modified methylnadic anhydride, dodecenyl succinic anhydride, tung oil anhydride, polyazelaic anhydride, polyglutaric anhydride, polyglycolic anhydride, or hydrolyzed polymaleic anhydride.
8. The grade-90 a asphalt of claim 1, wherein the initiator in the anhydrization slag reduction is one or more of dicumyl peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium metabisulfite, azobisisobutyronitrile, azobisisoheptonitrile, cumene hydroperoxide.
9. A method for preparing grade 90a asphalt according to any one of claims 1-8, comprising the steps of:
(1) Preparing anhydride slag reduction;
(2) Preparing a pretreatment component;
(3) Blending the material obtained in the step (1) and the material obtained in the step (2) and carrying out static heat preservation treatment to finally obtain the No. 90 grade A asphalt.
10. The method according to claim 9, wherein in the step (1), the process of preparing the anhydridized slag reduction is as follows:
a. adding the inferior slag reduction and high phosphoric acid content polyphosphoric acid heated to a flowing state into a reaction kettle, heating to a reaction temperature, continuously stirring, reacting under protective gas, and carrying out heat preservation treatment after the reaction is finished;
b. and d, adding polyphosphoric acid with low phosphoric acid content into the material obtained in the step a, stirring uniformly, adding an anhydride modifier and an initiator, continuously stirring, heating to a reaction temperature, reacting under a protective gas, and obtaining the anhydride slag reduction after the reaction is finished.
11. The method according to claim 10, wherein in the step a, the heating to the reaction temperature is performed by adopting temperature programming, the heating rate is 1-3 ℃/min, the reaction temperature is 140-180 ℃, the reaction time is 3-6 h, and the stirring speed is 600-800 r/min.
12. The method according to claim 10, wherein in step b, the stirring speed after the addition of the anhydride-modifier and the initiator is 600 to 800r/min; the heating to the reaction temperature is heating to the reaction temperature by adopting temperature programming, and the heating rate is 1-3 ℃/min; the reaction temperature is 160-180 ℃ and the reaction time is 6-8 h; the shielding gas is inert gas and/or N 2 The method comprises the steps of carrying out a first treatment on the surface of the The amount of the protective gas maintains the pressure in the reaction kettle to be 0.3-0.9 MPa.
13. The method according to claim 9, wherein in step (2), the pretreatment component is prepared by the following steps:
i. mixing the inferior slag reduction heated to a flowing state with a middle-quality component and a light component, and then carrying out hydrotreatment with hydrogen;
and ii, carrying out atmospheric and vacuum distillation on the material obtained in the step i to obtain a final pretreatment component.
14. The process according to claim 13, wherein in step i the operating conditions of the hydrotreatment are: the reaction temperature is 365-390 ℃, the reaction pressure is 12-22 MPa, and the volume airspeed is 0.5-1.8 h -1 The volume ratio of the hydrogen oil is 400-1500.
15. The method according to claim 9, wherein in the step (3), the stirring speed of the tempering process is 700-900 r/min, the stirring time is 4-6 h, and the tempering temperature is 140-165 ℃.
16. The method according to claim 9, wherein in the step (3), the static heat preservation treatment is performed under oxygen-enriched air, and the temperature is kept at 135-150 ℃ for 6-10 h.
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