CN1415663A - Polymer modified compsn. of road bitumen and its prepn. method - Google Patents
Polymer modified compsn. of road bitumen and its prepn. method Download PDFInfo
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- CN1415663A CN1415663A CN 01133375 CN01133375A CN1415663A CN 1415663 A CN1415663 A CN 1415663A CN 01133375 CN01133375 CN 01133375 CN 01133375 A CN01133375 A CN 01133375A CN 1415663 A CN1415663 A CN 1415663A
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Abstract
A polymer modified asphalt for road is prepared through mixing the arylhydrocarbon-enriched low-wax component with thermoplastic rubber, and mixing with basic asphalt and additive. Its advantages are high storage stability and good ductility and low-temp performance.
Description
1, technical field
The present invention relates to a kind of composition and preparation method of polymer modification road bitumen of composition and preparation method, especially stable storing of polymer modification road bitumen, belong to the petroleum pitch production technical field.
2, background technology
Pitch is as a kind of binding agent, uses very generally in urban road laying, and along with the continuous expansion that is fit to produce bituminous crude oil range of choice, and to the continuing to optimize of production technique, the quality of road bitumen has had large increase.But because the continuous increase of harsh climate condition and traffic loading, bituminous temperature sensibility needs that can not conform in addition, the warm draw seam ubiquity of geographic rut of high temperature and cold district, cause the road surface early damage, have to keep in repair in advance, will drop into a large amount of maintenance costs like this to guarantee the normal operation of road.Therefore, be necessary to develop temperature sensibility and the good pitch product innovation of high temperature performance, make it to satisfy the requirement of the needed various use propertieies of motorway.
At present, with polymkeric substance pitch being carried out modification is to use more method to improve its temperature sensibility and high and low temperature performance etc., yet, because high molecular polymer and pitch all exist bigger difference at aspects such as molecular weight, density and other physics, chemical property, cause consistency between the two relatively poor, even polymkeric substance is evenly dispersed in the basic asphalt, because formation is a kind of Unstable Systems, polymkeric substance all has the tendency that segregation comes out in pitch.In case stop to stir, demixing phenomenon can appear in most polymers, therefore, most at present working-yard production polymer modified asphalts that adopt do not wait polymkeric substance to separate out promptly to mix and stir with aggregate and pave the way.This not only has relatively high expectations with power to production unit and production, and production cost is higher.
In recent years, once there were some patent documentation reports to attempt to improve polymkeric substance and bituminous consistency with different methods.As US5070123 etc. is to improve consistency by adding mineral acid (especially phosphoric acid), but the result is unsatisfactory.In patents such as EP885934, US5288773, be to handle, and then improve consistency, but its polymkeric substance process for sulfonation practical application is difficult with pitch blended method by polymkeric substance being carried out sulfonation.(as WO9845372 etc.) is to make linking agent with sulphur in some other patents, reaches the compatible purpose of polymkeric substance and pitch.But its polymkeric substance mixes with bituminous by High shear device to be realized, big to equipment requirements height, facility investment like this, and processing method and step are more loaded down with trivial details, and the used time of the course of processing is long, therefore, treatment capacity is restricted.
3, summary of the invention
The objective of the invention is to overcome the problems referred to above, a kind of composition and preparation method with polymer modification road bitumen of stability in storage is provided.
The concrete composition (weight) that the present invention has the polymer modification road bitumen of stability in storage is:
Basic asphalt 81%～97.9%;
The mother liquor 2%～18% that comprises poor wax group of Fu Fang and polymkeric substance;
Composite additive 0.1%～5%.
The preparation method that the present invention has the polymer modification road bitumen of stability in storage is:
1, with rich fragrant poor wax component polymer melt is become mother liquor;
2, above-mentioned mother liquor is added in the basic asphalt of heating and melting;
3, composite additive is joined in batches insulated and stirred certain hour in the basic asphalt that contains mother liquor in the 2nd step, the polymer modification road bitumen that promptly can obtain having good shelf-stability.
Simple, the less investment of the inventive method production unit, and owing to added the compound agent that adds, shortened the preparation feedback time greatly, product have less temperature sensibility and high and low temperature performance preferably.When being used to build high-grade highway, can resist the rut under the summer high temperature environment and the generation of the phenomenons such as cracking under the winter low temperature environment, prolong the life-span of road, can improve performances such as the abrasion performance on road surface and brake simultaneously.And, therefore, can be fit to batch production production because this bituminous composition has stability in storage well.
4, embodiment
The present invention has in the polymer modification road bitumen of stability in storage and comprises that the preferred content (weight) of the mother liquor of poor wax group of Fu Fang and polymkeric substance is 6%～12%.The extraction oil that the fragrant poor wax component of used richness can be a lubricating oil solvent can be catalytically cracked oil, can also be with the vacuum distillate (boiling point preferably is higher than 420 ℃) of naphthenic base crude, and the mixture of arbitrary proportion between them.Used polymkeric substance is the thermoplastic elastomer class that contains the conjugated diolefine hydrocarbon structure, comprises diblock copolymer SB, and triblock copolymer SBS and structure polymkeric substance similarly can be wherein a kind of polymkeric substance or several mixture of polymers, preferred SBS.Polymkeric substance accounts for 20%～70% (m) of mother liquor total amount, is suitably 30%～60%.
Used basic asphalt comprises residual oil that distil process obtains, straight-run pitch, solvent deoiling pitch, blending pitch etc., 25 ℃ of penetration degrees of pressing the basic asphalt of GB/T4509 mensuration are (30～120) 1/10mm, be preferably (40～100) 1/10mm, the softening temperature of the basic asphalt of measuring by GB/T4507 is 37 ℃～80 ℃, is preferably 43 ℃～65 ℃.
Used composite additive is made up of the inorganics or the organism that play effects such as sulfuration and promotion, comprise several compound in magnesium oxide, calcium oxide, zinc oxide, plumbous oxide, basic carbonate sodium, white lead carbonate, basic carbonate calcium, zinc subcarbonate, zinc carbonate, sulphur, sulfocompound, carbon black, the calcium hydroxide etc., the sulfur-bearing thing accounts for 10%～50% (m) in the composite additive, metal oxide accounts for 40%～70% (m), and other accounts for 10%～20% (m).
The present invention has the preparation method who contains mother liquor described in the polymer modification road bitumen of stability in storage: with rich fragrant poor wax component with polymer melt, used mixing temperature is 150 ℃～240 ℃, be preferably 170 ℃～190 ℃, mixing time is (1～5) h, preferred (2～3) h.Can continuously stirring or interruption stirring in preparation mother liquor process.
The preparation of modifying asphalt can comprise following two kinds of concrete technologies:
A. mother liquor 2%～18% is joined in 150 ℃～210 ℃ the heated bitumen in the ratio of polymkeric substance in modifying asphalt, be preferably 170 ℃～190 ℃, under common stirring, mix (10～180) min, preferred (20～100) min, when stirring, divide 2～5 addings with composite additive, be 50% of additive total amount for the first time wherein, each add-on is the five equilibrium adding of residual content later on, adds the used time to be no more than 60min at every turn, the most handy (5～40) min, each adding afterreaction time is (10～120) min, preferably adds for the first time afterreaction (20～80) min, each later on afterreaction 20～60min that adds.Can bring up to 170 ℃～230 ℃ in adding composite additive afterreaction first time temperature, preferably remain on 175 ℃～220 ℃, finish until reaction.
B. at first half of mother liquor total amount joined in 150 ℃～230 ℃ the heated bitumen, be preferably 170 ℃～190 ℃, under common stirring, mix (10～180) min, be preferably (20～100) min, when stirring, half composite additive was added with the time that is no more than 60min, the most handy (5～40) min, reaction (10～120) min, preferably (20～80) min again.Remaining half mother liquor and half additive repeat aforesaid operations, to the reaction end.
To further specify the present invention by embodiment below.
Embodiment 1
Under 175 ℃, SBS is joined in a kind of extraction oil of lubricating oil solvent, saturated minute content is that 36.62% (m), fragrance are divided into 42.00% (m), colloid is that 21.33% (m), bituminous matter are that 0.05% (m), wax content are 2.51% (m) in this extraction oil, SBS and extract oil out and respectively account for 50% (m) mixes 3h and is prepared into mother liquor to fusion under common stirring.Get this mother liquor that accounts for modifying asphalt total amount 10%, join in the heated bitumen that is in 175 ℃, this pitch penetration degree is that 97 1/10mm, softening temperature are 45.7 ℃, accounts for 88.8% of total amount, stirs 50min, add 0.5% composite additive (containing dimorpholinyl disulfide 35%, plumbous oxide 50%, carbon black 15%) afterwards with 15min, temperature is risen to 185 ℃, and reaction 50min adds remaining 0.5% composite additive at last with 5min, continue to finish behind the reaction 60min, and test its character.(the results are shown in Table 1).
Embodiment 2
Under 180 ℃, SBS is joined in the vacuum distillate of naphthenic base crude of Liaohe Oil Field, this distillate boiling spread is 430 ℃～500 ℃, the two respectively accounts for 50%, mixes 3.5h under stirring being interrupted, and is prepared into mother liquor.Get this mother liquor that accounts for modifying asphalt total amount 12%, join in the heated bitumen that is in 180 ℃, this penetration of bitumens is 60 1/10mm, softening temperature is 49.7 ℃, account for 86.5% (m) of total amount, after stirring 60min, add half of composite additive (sulfur-bearing 30%, zinc oxide 50%, basic carbonate calcium 20%) with 10min, temperature is risen to 215 ℃, reaction 60min, after this, join remaining additive etc. in the said mixture at twice, use 5min each the adding, and reaction 50min, until the character that finishes back test modifying asphalt.(the results are shown in Table 1).
Embodiment 3
Under 185 ℃, SBS is joined in a kind of catalytically cracked oil, saturated minute content is that 30.12% (m), fragrance are divided into 46.15% (m), colloid is that 21.56% (m), bituminous matter are that 2.17% (m), wax content are 1.94% (m) in this slurry oil, SBS content is 33.3% (m), under interruption stirs, mix 2.5h, be prepared into mother liquor.Get this mother liquor that accounts for modifying asphalt total amount 12%, 1/2 of this mother liquor is joined in the heated bitumen that is in 175 ℃, this penetration of bitumens is 70 1/10mm, softening temperature is 47.9 ℃, accounts for 86.5% (m) of total amount, stirs 50min, add half of composite additive (containing alkyl phenol disulfide 40%, zinc oxide 50%, basic carbonate calcium 10%) afterwards with 7min, reaction 60min, temperature keeps constant then, and remaining 1/2 mother liquor and 1/2 additive are repeated to finish behind the aforesaid operations.(the results are shown in Table 1).
Table 1 embodiment 123 mother liquor add-ons, m% 10 12 12SBS add-ons, m% 564 composite additives, m% 1.0 1.5 1.5 technology A A B penetration degrees (25 ℃), 1/10mm 88 77 103 softening temperatures, ℃ 75.6 78.0 55.95 ℃ of ductilities, cm 73 40 86 separation tests (163 ℃, 48h)
*Softening temperature is poor, ℃-0.6-1.7 1.3 recovery of elasticity (25 ℃), m% 90.3 99.9 88.2 viscosity (135 ℃), Pas 1.2 2.3 0.9 penetrative indexs (PI)
*-0.2519-0.0605-0.8492 plastic zone, ℃ 68.0 70.0 62.0
*Stability in storage among the present invention (being consistency) is to estimate by upper and lower softening temperature difference after the separation of stipulating among the ASTMD5892-96.When softening temperature difference during, think that stability in storage is qualified less than 2.2 ℃.
*Obtain calculating and getting with PI=30/ (1+50A)-10 after the A by formula 1gP=AT+K recurrence by the penetration degree under three temperature.
Can find out that from table 1 polymer modified asphalt not only stability in storage (softening temperature is poor) meets requirement less than 2.2 ℃, and have that low-temperature ductility is big, recovery of elasticity is big, temperature sensibility is little and good performance such as plastic zone is wide.
Claims (10)
1, a kind of weight with polymer modification road bitumen of stability in storage consists of:
Basic asphalt 81%～97.9%;
The mother liquor 2%～18% that comprises poor wax group of Fu Fang and polymkeric substance;
Composite additive 0.1%～5%.
2, according to the described polymer modification road bitumen of claim 1 with stability in storage, it is characterized in that the vacuum distillate of extraction oil that the rich fragrant poor wax component in the described mother liquor is a lubricating oil solvent, catalytically cracked oil, alkyl crude oil or the mixture of arbitrary proportion between them, polymkeric substance in the described mother liquor is one or more the mixture that contains in the thermoplastic elastomer class of conjugated diolefine hydrocarbon structure, and wherein polymkeric substance accounts for 20%～70% of mother liquor gross weight; 25 ℃ of penetration degrees of described basic asphalt are 30～1201/10mm, and softening temperature is 37 ℃～80 ℃; Described composite additive comprises several in magnesium oxide, calcium oxide, zinc oxide, plumbous oxide, basic carbonate sodium, white lead carbonate, basic carbonate calcium, zinc subcarbonate, zinc carbonate, sulphur, sulfocompound, carbon black and the calcium hydroxide, wherein the sulfur-bearing thing accounts for 10%～50% of gross weight, metal oxide account for must measure 40%～70%, other material accounts for 10%～20% of gross weight.
3, according to the described polymer modification road bitumen of claim 2 with stability in storage, it is characterized in that the polymkeric substance in the described mother liquor is SBS, wherein the weight content in the mother liquor is 30%～60%.
4, the described preparation method with polymer modification road bitumen of stability in storage of a kind of claim 1 is:
(1) with rich fragrant poor wax component polymer melt is become mother liquor;
(2) above-mentioned mother liquor is added in the basic asphalt of heating and melting;
(3) composite additive is joined in batches insulated and stirred certain hour in the basic asphalt that contains mother liquor in (2) step, the polymer modification road bitumen that promptly can obtain having good shelf-stability.
5, according to the described preparation method of claim 4 with polymer modification road bitumen of stability in storage, the preparation process that it is characterized in that described (1) step mother liquor is: use rich fragrant poor wax component with polymer melt, mixing temperature is 150 ℃～240 ℃, mixing time is 1～5h, and continuously stirring or interruption stir in preparation mother liquor process.
6, according to the described preparation method of claim 4 with polymer modification road bitumen of stability in storage, it is characterized in that described (2), (3) one step process is: mother liquor is joined in 150 ℃～210 ℃ the heated bitumen, under agitation, mix 10～180min, when stirring, divide 2～5 addings with composite additive, add the used time to be no more than 60min at every turn, add the afterreaction time is 10～120min at every turn.
7, according to the described preparation method of claim 6 with polymer modification road bitumen of stability in storage, it is characterized in that described (2), (3) one step process is: mother liquor is joined in 170 ℃～190 ℃ the heated bitumen, under agitation, mix 20～100min, composite additive is for the first time for adding 50% of total amount, each add-on is the five equilibrium adding of residual content later on, adds afterreaction 20～80min for the first time, each later on afterreaction 20～60min that adds.
8, according to claim 6 or 7 described preparation methods with polymer modification road bitumen of stability in storage, it is characterized in that describedly bringing up to 170 ℃～230 ℃ adding for the first time composite additive afterreaction temperature, finish until reaction.
9, according to the described preparation method of claim 4 with polymer modification road bitumen of stability in storage, it is characterized in that described (2), (3) one step process is: at first half of mother liquor total amount joined in 150 ℃～230 ℃ the heated bitumen, under agitation, mix 10～180min, when stirring, half composite additive was added with the time that is no more than 60min, react 10～120min again, remaining half mother liquor and half additive repeat aforesaid operations, to the reaction end.
10, according to the described preparation method of claim 9 with polymer modification road bitumen of stability in storage, it is characterized in that described (2), (3) one step process is: at first half of mother liquor total amount joined in 170 ℃～190 ℃ the heated bitumen, under agitation, mix 20～100min, when stirring, half composite additive with 5～40min, is reacted 20～80min again, remaining half mother liquor and half additive repeat aforesaid operations, to the reaction end.
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| CNB011333758A CN1195803C (en) | 2001-10-30 | 2001-10-30 | Polymer modified compsn. of road bitumen and its prepn. method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101007902B (en) * | 2005-12-27 | 2011-01-12 | 新日本石油株式会社 | Asphalt composition for pavement and its continuous production method |
| CN103804929A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Modified asphalt composition and preparation method thereof |
| CN103804925A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Modified asphalt and preparation method thereof |
| CN104560084A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Preparation method for blended asphalt |
| CN104962088A (en) * | 2015-06-26 | 2015-10-07 | 安徽顺驰电缆有限公司 | Preparation technology for rubber asphalt parent |
-
2001
- 2001-10-30 CN CNB011333758A patent/CN1195803C/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101007902B (en) * | 2005-12-27 | 2011-01-12 | 新日本石油株式会社 | Asphalt composition for pavement and its continuous production method |
| CN103804929A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Modified asphalt composition and preparation method thereof |
| CN103804925A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Modified asphalt and preparation method thereof |
| CN103804925B (en) * | 2012-11-07 | 2016-01-20 | 中国石油化工股份有限公司 | A kind of modifying asphalt and preparation method thereof |
| CN104560084A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Preparation method for blended asphalt |
| CN104560084B (en) * | 2013-10-22 | 2017-02-01 | 中国石油化工股份有限公司 | Preparation method for blended asphalt |
| CN104962088A (en) * | 2015-06-26 | 2015-10-07 | 安徽顺驰电缆有限公司 | Preparation technology for rubber asphalt parent |
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| Publication number | Publication date |
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| CN1195803C (en) | 2005-04-06 |
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Granted publication date: 20050406 |