CN108264721B - Preparation method of high-viscosity asphalt modifier, modified asphalt containing modifier and asphalt mixture - Google Patents
Preparation method of high-viscosity asphalt modifier, modified asphalt containing modifier and asphalt mixture Download PDFInfo
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Abstract
The invention provides a preparation method of a high-viscosity asphalt modifier, modified asphalt containing the modifier and an asphalt mixture. The preparation method of the high-viscosity asphalt modifier comprises the following steps: (1) uniformly mixing thermoplastic styrene-butadiene rubber, ethylene octene polyolefin elastomer, maleic anhydride and an initiator in a high-speed mixer, then carrying out grafting reaction in a double-screw extruder, and extruding and granulating to prepare maleic anhydride modified master batch; (2) and uniformly mixing the maleic anhydride modified master batch, styrene butadiene rubber, tackifying resin and a crosslinking agent in a high-speed mixer, then adding the mixture into a double-screw extruder for dynamic vulcanization and extrusion granulation to obtain the high-viscosity asphalt modifier.
Description
Technical Field
The invention relates to a preparation method of a high-viscosity asphalt modifier, and modified asphalt and an asphalt mixture containing the modifier.
Background
As a large-pore pavement structure, the drainage asphalt pavement has the characteristics of noise reduction, water permeability, air permeability, water drift prevention and the like, can effectively reduce road surface accidents in rainy days, and is particularly important under the large background that urban inland inundation is frequent and China advocates vigorously to build a sponge city at present. However, the general asphalt lacks certain cohesive force to the macroporous structure to influence the service performance, and in addition, the drainage asphalt pavement has the condition of poor high and low temperature resistance. The modified asphalt with high viscosity is widely noticed by introducing polymer and the like into the asphalt, so that stone material with strong adhesion can be provided, and the service performance such as high and low temperature can be improved.
SBS (thermoplastic styrene-butadiene rubber) is used as the most commonly used polymer and is much studied as an asphalt modifier. But the compatibility with asphalt is limited, the tackifying capability of the asphalt modifier needs to be improved, and the integral high-performance use requirement of the pavement is difficult to meet. Chinese patent document CN1657565A discloses a high viscosity asphalt modifier and a preparation method thereof, which is composed of SBS, petroleum resin and diatomite, and although the preparation method is simple and the high temperature storage property is good, it is difficult to consider both the high and low temperature service performance. Chinese patent document CN101457009B discloses a high viscosity asphalt modifier and a preparation method thereof, which is prepared from SIS (styrene-isoprene-styrene block copolymer), coumarone resin and oleamide, and although the asphalt modifier has good compatibility with asphalt and good adhesion and high temperature performance, the asphalt modifier does not satisfy the requirements of low temperature performance. Chinese patent document CN102268188B discloses a high-viscosity asphalt additive, a preparation method and an application thereof, which are composed of rubber powder and POE compound main agent, plasticizer, filler and stabilizer, and can improve the properties of asphalt such as softening point, viscosity and the like to a certain extent, but do not relate to the use requirements of high and low temperature resistance and the like of a pavement. Although the problems of asphalt stability, viscosity improvement, high temperature resistance and the like are solved to a certain extent by the modification technology, less high-performance use requirements on simultaneously meeting the requirements of viscosity, asphalt compatibility and high and low temperature resistance are involved.
Disclosure of Invention
Object of the Invention
The invention aims to provide a preparation method of a high-viscosity asphalt modifier, which is used for asphalt modification and can simultaneously meet the requirements of high viscosity, high adhesion and high and low temperature resistant service performance.
Another object of the present invention is to provide a modified asphalt containing the highly viscous asphalt modifier obtained by the above-mentioned production method.
The invention also aims to provide an asphalt mixture containing the high-viscosity asphalt modifier obtained by the preparation method.
Summary of The Invention
According to a first aspect of the present invention, the present invention provides a method for preparing a high-viscosity asphalt modifier, comprising the steps of:
(1) uniformly mixing thermoplastic styrene-butadiene rubber, ethylene octene polyolefin elastomer, maleic anhydride and an initiator in a high-speed mixer, then carrying out grafting reaction in a double-screw extruder, and extruding and granulating to prepare maleic anhydride modified master batch;
(2) uniformly mixing the maleic anhydride modified master batch, styrene butadiene rubber, tackifying resin and a crosslinking agent in a high-speed mixer, then adding the mixture into a double-screw extruder for dynamic vulcanization and extrusion granulation to obtain the high-viscosity asphalt modifier;
the raw materials comprise the following components in percentage by mass:
the thermoplastic styrene-butadiene rubber (SBS) is a well-known and commonly used substance in the art, and is a triblock polymer of styrene-butadiene-styrene; the styrene-butadiene rubber (SBR) is a random copolymer of styrene and butadiene, and is also well known and commonly used in the art. In the present invention, when referring to a simple "styrene-butadiene rubber", it refers to a random copolymer of styrene and butadiene, and when referring to a "thermoplastic styrene-butadiene rubber", it refers to a triblock polymer of styrene-butadiene-styrene.
Preferably, the thermoplastic styrene-butadiene rubber is a mixture of star-shaped thermoplastic styrene-butadiene rubber and linear thermoplastic styrene-butadiene rubber, and the star-shaped thermoplastic styrene-butadiene rubber accounts for 10% to 40% (e.g., 10%, 20%, 30%) of the total mass of the thermoplastic styrene-butadiene rubber.
Preferably, the styrene-butadiene rubber is at least one of solution-polymerized styrene-butadiene rubber, emulsion-polymerized styrene-butadiene rubber and powdered styrene-butadiene rubber.
Preferably, the tackifying resin is at least one of rosin resin, petroleum resin and terpene resin.
Preferably, the initiator is dicumyl peroxide and/or azobisisobutyronitrile.
Preferably, the cross-linking agent is sulfur.
The specific parameters of the grafting reaction and the extrusion granulation in the double-screw extruder can be simply determined by the skilled person through tests, preferably, the length-diameter ratio of the screw of the extruder is 36: 1-48: 1, the extrusion temperature is 120-190 ℃, and the rotating speed of the screw is 40-150 rpm;
the specific parameters of dynamic vulcanization, extrusion and granulation in the double-screw extruder can be simply determined by a person skilled in the art through tests, preferably, the length-diameter ratio of the screw of the extruder is 36: 1-48: 1, the extrusion temperature is 145-220 ℃, and the rotating speed of the screw is 40-300 rpm.
According to the second aspect of the invention, the invention also provides modified asphalt containing the high-viscosity asphalt modifier obtained by the preparation method, the raw material composition of the modified asphalt comprises the high-viscosity asphalt modifier and asphalt, and the mixing amount of the high-viscosity asphalt modifier is 1-12% of the mass of the asphalt. The asphalt is preferably 70# and 90# asphalt.
The preparation steps of the modified asphalt are as follows: (1) firstly, adding the high-viscosity asphalt modifier into No. 70 asphalt at 160-180 ℃ and stirring for half an hour; (2) and (3) stirring at high speed for 1 hour at the speed of 4000-5000 rpm at 160-180 ℃ by using a high-speed shearing machine, and then developing for half an hour to obtain the modified asphalt. Wherein the dynamic viscosity of the modified asphalt at 60 ℃ is more than 20000 Pa-s.
According to the third aspect of the invention, the invention also provides an asphalt mixture containing the high-viscosity asphalt modifier obtained by the preparation method, the raw material composition of the asphalt mixture comprises the high-viscosity asphalt modifier and asphalt, and the mixing amount of the high-viscosity asphalt modifier is 1-12% of the mass of the asphalt. The asphalt is preferably 70# and 90# asphalt.
The preparation method of the asphalt mixture can be selected from one of the following methods:
(1) the aggregate, the high-viscosity asphalt modifier, the asphalt and the mineral powder can be directly mixed to obtain the asphalt mixture.
(2) Or mixing the high-viscosity asphalt modifier with asphalt to prepare the modified asphalt, and then adding the aggregate and the mineral powder to mix to obtain the asphalt mixture.
The invention adopts SBS, POE, SBR, tackifying resin, MAH and other raw materials to prepare the high-viscosity asphalt modifier through reactive extrusion and dynamic vulcanization technology. Wherein, SBS can improve the high and low temperature resistance of the modified asphalt and the mixture; POE and SBR have excellent low temperature resistance, and moreover, the cost of POE is relatively inexpensive; the viscosity of the system can be obviously improved by adding the star SBS, the SBR and the tackifying resin; the maleic anhydride reaction extrusion can graft polar groups on the surfaces of SBS and POE polymers, so that the compatibility of the SBS and POE polymers with asphalt is improved, and the system stability is improved; the dynamic vulcanization is mainly used for overcoming the processing difficulty of the elastomer and the rubber. The asphalt and the asphalt mixture modified by the high-viscosity asphalt modifier prepared by the invention have excellent comprehensive performance, and can meet the use requirements of drainage asphalt pavement on high viscosity, high adhesion and high and low temperature resistance of asphalt.
Detailed Description
The technical scheme of the invention is further illustrated by the following embodiments.
The information on the raw materials involved in the following examples is as follows: wherein the star SBS is model 411 of Korean LG chemical company, and the linear SBS is model YH-792 of Yueyang petrochemical company; POE is model 7447 of Dow chemical company Limited; the SBR is XY-GO15 emulsion particle model number of Shandong Yinyuan chemical technology Co Ltd; the petroleum resin is C5 petroleum resin with model number of D0102 from Jitian chemical Limited of Shenzhen city; the rosin resin and the terpene resin are purchased from Zhengzhou Shengyu chemical products Co., Ltd, and the models are FS-1 and T100 respectively; maleic anhydride, dicumyl peroxide and azodiisobutyronitrile are purchased from Shanghai Feng Rui chemical Co Ltd, and have excellent grade and purity of more than 99 percent; sulfur is purchased from Lanxing Industrial technology, Inc., Liyunggang and has a purity of more than 99%.
The used aggregates are all purchased from limestone stones of Nanjing Gaojia road and bridge company, wherein the mixture consists of: 39 wt% of 10-15mm stone, 44 wt% of 5-10mm stone, 3 wt% of 3-5mm stone, 11 wt% of 0-3mm stone and 3 wt% of ore powder. The asphalt used was Tanzhou 70# asphalt and 90# asphalt, which had softening points of 47 ℃ and 45 ℃ and penetration degrees (25 ℃, 100g, 5s) of 71mm and 88mm, respectively. The test method of the mixture is carried out according to the test procedure of JTG E-20-2011 road engineering asphalt and asphalt mixture. The related test standard of the high-viscosity asphalt modifier refers to a second part of JTT 860.2-2013 asphalt mixture modified additive: the high viscosity additive protocol proceeds. The compatibility of the high-viscosity asphalt modifier and the asphalt is judged according to the existence of obvious unmelted objects after the modified asphalt is stirred, if no obvious particles exist, the compatibility is good; the reverse is true.
Example 1
The high-viscosity asphalt modifier comprises the following raw materials: 14 parts of linear SBS, 6 parts of star SBS, 30 parts of ethylene-octene polyolefin elastomer (POE), 35 parts of Styrene Butadiene Rubber (SBR), 12.49 parts of petroleum resin, 0.5 part of Maleic Anhydride (MAH), 0.01 part of dicumyl peroxide and 2 parts of sulfur.
The preparation method of the high-viscosity asphalt modifier comprises the following steps: (1) SBS, POE, MAH and dicumyl peroxide are mixed homogeneously in a high mixing machine and then extruded in a double screw extruder to pelletize. Wherein the length-diameter ratio of the screw of the extruder is 40: 1, the extrusion temperature is 120-180 ℃, and the rotation speed of the screw is 100 rpm. (2) And (3) uniformly mixing the first-step reaction master batch with SBR, petroleum resin and sulfur in a high mixing machine, and then dynamically vulcanizing, extruding and granulating in a double-screw extruder to obtain the high-viscosity asphalt modifier. Wherein the length-diameter ratio of the screw is 36: 1, the extrusion temperature is 155-200 ℃, and the rotation speed of the screw is 250 rpm.
The modified asphalt is prepared as follows: (1) firstly, 6 percent of the high-viscosity asphalt modifier is added into 70# asphalt with the temperature of 180 ℃ to be stirred for half an hour; (2) and continuously stirring at a high speed of 180 ℃ for 1 hour by using a high-speed shearing machine, and then developing for half an hour to obtain the modified asphalt.
The preparation of the asphalt mixture is as follows: and (3) firstly mixing the high-viscosity asphalt modifier and the aggregate in a stirring pot at 180 ℃ for 30s, adding asphalt, continuously mixing for 90s, finally adding mineral powder, and stirring for 90s to obtain the asphalt mixture. Wherein the oil-stone ratio is 4.4, and the high-viscosity asphalt modifier accounts for 6 percent of the asphalt by mass.
TABLE 1 Properties relating to the high-viscosity asphalt modifier, modified asphalt and asphalt mixture described in example 1
Example 2
The high-viscosity asphalt modifier comprises the following raw materials: 36 parts of linear SBS, 4 parts of star SBS, 25 parts of ethylene-octene polyolefin elastomer (POE), 27.9 parts of Styrene Butadiene Rubber (SBR), 5 parts of rosin resin, 1 part of Maleic Anhydride (MAH), 0.1 part of azobisisobutyronitrile and 1 part of sulfur.
The preparation method of the high-viscosity asphalt modifier comprises the following steps: (1) SBS, POE, MAH and azodiisobutyronitrile are mixed homogeneously in a high mixing machine and then extruded in a double screw extruder to pelletize. Wherein the length-diameter ratio of the screw of the extruder is 48: 1, the extrusion temperature is 130-185 ℃, and the rotation speed of the screw is 50 rpm. (2) And (3) uniformly mixing the first-step reaction master batch with SBR, rosin resin and sulfur in a high mixing machine, and then dynamically vulcanizing, extruding and granulating in a double-screw extruder to obtain the high-viscosity asphalt modifier. Wherein the length-diameter ratio of the screw of the extruder is 40: 1, the extrusion temperature is 145 ℃ to 210 ℃, and the rotating speed of the screw is 100 rpm.
The modified asphalt is prepared as follows: (1) firstly, adding 8% of the high-viscosity asphalt modifier into 90# asphalt at 170 ℃ and stirring for half an hour; (2) and continuously stirring at a high speed of 180 ℃ for 1 hour by using a high-speed shearing machine, and then developing for half an hour to obtain the modified asphalt.
The preparation of the asphalt mixture is as follows: and firstly mixing the high-viscosity asphalt modifier and the aggregate in a stirring pot at 170 ℃ for 30s, adding asphalt, continuously mixing for 90s, finally adding mineral powder, and stirring for 90s to obtain the asphalt mixture. Wherein the oil-stone ratio is 4.3, and the mass of the high-viscosity asphalt modifier accounts for 8 percent of that of the asphalt.
TABLE 2 Properties relating to the high-viscosity asphalt modifier, modified asphalt and asphalt mixture described in example 2
Example 3
The high-viscosity asphalt modifier comprises the following raw materials: 22 parts of linear SBS, 8 parts of star SBS, 45 parts of ethylene-octene polyolefin elastomer (POE), 15 parts of Styrene Butadiene Rubber (SBR), 6.2 parts of terpene resin, 3 parts of Maleic Anhydride (MAH), 0.3 part of dicumyl peroxide and 0.5 part of sulfur.
The preparation method of the high-viscosity asphalt modifier comprises the following steps: (1) SBS, POE, MAH and dicumyl peroxide are mixed homogeneously in a high mixing machine and then extruded in a double screw extruder to pelletize. Wherein the length-diameter ratio of the screw of the extruder is 40: 1, the extrusion temperature is 140 ℃ to 180 ℃, and the rotating speed of the screw is 40 rpm. (2) And (3) uniformly mixing the first-step reaction master batch with SBR, terpene resin and sulfur in a high-speed mixer, and then dynamically vulcanizing, extruding and granulating in a double-screw extruder to obtain the high-viscosity asphalt modifier. Wherein the length-diameter ratio of the screw of the extruder is 40: 1, the extrusion temperature is 160-210 ℃, and the rotation speed of the screw is 50 rpm.
The modified asphalt is prepared as follows: (1) firstly, adding 10% of the high-viscosity asphalt modifier into 70# asphalt at 180 ℃, stirring for half an hour (2), continuing to stir at a high speed for 1 hour at 170 ℃ by using a high-speed shearing machine, and then developing for half an hour to obtain the high-viscosity modified asphalt.
The preparation of the asphalt mixture is as follows: and (3) firstly mixing the high-viscosity asphalt modifier and the aggregate in a stirring pot at 175 ℃ for 30s, adding asphalt, continuously mixing for 90s, finally adding mineral powder, and stirring for 90s to obtain the asphalt mixture. Wherein the oil-stone ratio is 4.3, and the high-viscosity asphalt modifier accounts for 10 percent of the mass of the asphalt.
TABLE 3 Properties relating to the high-viscosity asphalt modifier, modified asphalt and asphalt mixture described in example 3
Example 4
The high-viscosity asphalt modifier comprises the following raw materials: 35 parts of linear SBS, 10 parts of star SBS, 20 parts of ethylene-octene polyolefin elastomer (POE), 15 parts of Styrene Butadiene Rubber (SBR), 13.7 parts of petroleum resin, 5 parts of Maleic Anhydride (MAH), 0.3 part of dicumyl peroxide and 1 part of sulfur.
The preparation method of the high-viscosity asphalt modifier comprises the following steps: (1) SBS, POE, MAH and dicumyl peroxide are mixed homogeneously in a high mixing machine and then extruded in a double screw extruder to pelletize. Wherein the length-diameter ratio of the screw of the extruder is 48: 1, the extrusion temperature is from 150 ℃ to 200 ℃, and the rotating speed of the screw is 100 rpm. (2) And (3) uniformly mixing the first-step reaction master batch with SBR, petroleum resin and sulfur in a high mixing machine, and then dynamically vulcanizing, extruding and granulating in a double-screw extruder to obtain the high-viscosity asphalt modifier. Wherein the length-diameter ratio of the screw of the extruder is 36: 1, the extrusion temperature is 165-220 ℃, and the rotating speed of the screw is 40 rpm.
The modified asphalt is prepared as follows: (1) firstly, adding 10% of the high-viscosity asphalt modifier into 90# asphalt at 180 ℃ and stirring for half an hour; (2) and continuously stirring at a high speed of 180 ℃ for 1 hour by using a high-speed shearing machine, and then developing for half an hour to obtain the modified asphalt.
The preparation of the asphalt mixture is as follows: firstly stirring the high-viscosity asphalt modifier and the aggregate in a stirring pot at 180 ℃ for 30s, adding asphalt, continuously stirring for 90s, and finally adding mineral powder and stirring for 90s to obtain the asphalt mixture. Wherein the oil-stone ratio is 4.2, and the mass of the high-viscosity modifier accounts for 10 percent of that of the asphalt.
TABLE 4 Properties relating to the high-viscosity asphalt modifier, modified asphalt and asphalt mixture described in example 4
In combination with tables 1-4, the present invention is excellent in that: the asphalt modifier has good compatibility with asphalt, and the modified asphalt has almost no unmelted substances; for the modified asphalt, the dynamic viscosity at 60 ℃ meets the condition and is excellent, which shows that the modified asphalt has the characteristic of high viscosity. The modified asphalt has excellent adhesion capability as shown by the adhesion grade with aggregate; ductility and low temperature bending failure strain respectively show that the modified asphalt and the mixture have good low temperature resistance. The data of softening point, dynamic stability and the like respectively show that the modified asphalt and the mixture have good high-temperature resistance; in a word, the high-viscosity asphalt modifier, the modified asphalt and the asphalt mixture prepared by the embodiment of the invention have excellent performance in all aspects, meet the standard requirements, and can meet the requirements of comprehensive use performance such as high and low temperature resistance of the drainage asphalt pavement.
Claims (8)
1. The preparation method of the high-viscosity asphalt modifier is characterized by comprising the following steps:
(1) uniformly mixing thermoplastic styrene-butadiene rubber, ethylene octene polyolefin elastomer, maleic anhydride and an initiator in a high-speed mixer, then carrying out grafting reaction in a double-screw extruder, and extruding and granulating to prepare maleic anhydride modified master batch;
(2) uniformly mixing the maleic anhydride modified master batch, styrene butadiene rubber, tackifying resin and a crosslinking agent in a high-speed mixer, then adding the mixture into a double-screw extruder for dynamic vulcanization and extrusion granulation to obtain the high-viscosity asphalt modifier;
the raw materials comprise the following components in percentage by mass:
2. the method for preparing the high-viscosity asphalt modifier according to claim 1, wherein the thermoplastic styrene-butadiene rubber is a mixture of star-shaped thermoplastic styrene-butadiene rubber and linear thermoplastic styrene-butadiene rubber, and the star-shaped thermoplastic styrene-butadiene rubber accounts for 10-40% of the total mass of the thermoplastic styrene-butadiene rubber.
3. The method for preparing the high-viscosity asphalt modifier according to claim 1, wherein the styrene-butadiene rubber is at least one of solution-polymerized styrene-butadiene rubber, emulsion-polymerized styrene-butadiene rubber and powdered styrene-butadiene rubber.
4. The method for preparing high-viscosity asphalt modifier according to claim 1, wherein the tackifying resin is at least one of rosin resin, petroleum resin and terpene resin.
5. The method of claim 1, wherein the initiator is dicumyl peroxide and/or azobisisobutyronitrile.
6. The method for preparing the high-viscosity asphalt modifier according to claim 1, wherein the crosslinking agent is sulfur.
7. Modified asphalt containing the high-viscosity asphalt modifier obtained by the preparation method of any one of claims 1 to 6, characterized in that the raw material composition comprises the high-viscosity asphalt modifier and asphalt, and the high-viscosity asphalt modifier is added in an amount of 1 to 12 percent of the mass of the asphalt.
8. The asphalt mixture containing the high-viscosity asphalt modifier obtained by the preparation method of any one of claims 1 to 6 is characterized in that the raw material composition of the asphalt mixture contains the high-viscosity asphalt modifier and asphalt, and the mixing amount of the high-viscosity asphalt modifier is 1 to 12 percent of the mass of the asphalt.
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| CN110564102A (en) * | 2019-10-28 | 2019-12-13 | 重庆重交再生资源开发股份有限公司 | Asphalt high-viscosity modifier and preparation method thereof |
| CN111621025B (en) * | 2020-06-15 | 2021-11-16 | 山东省高速路桥养护有限公司 | Solid warm-mix modified double-effect asphalt modifier and preparation method thereof |
| CN112551940A (en) * | 2020-12-10 | 2021-03-26 | 辽宁省交通科学研究院有限责任公司 | Direct-vat-set tackifying regenerative modifier and preparation and application methods thereof |
| CN113025070A (en) * | 2021-03-17 | 2021-06-25 | 山东京博石油化工有限公司 | Preparation method of high-viscosity modified asphalt |
| CN114605846A (en) * | 2022-04-26 | 2022-06-10 | 河南蓝翎环科防水材料有限公司 | Super-durable high polymer modified asphalt waterproof coiled material and preparation method thereof |
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| CN101775223B (en) * | 2009-12-24 | 2011-08-17 | 交通部公路科学研究所 | Additive for drainage asphalt mixture of high temperature heavy load road and preparation method thereof |
| CN102757655B (en) * | 2012-08-02 | 2014-04-16 | 唐山德生防水股份有限公司 | Edge sealing material for modified asphalt sealing, and preparation method and application method thereof |
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| CN104559242A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Waste rubber powder modified asphalt composition and preparation method thereof |
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