CN110229534B - Preparation method of microalgae oil modified rubber asphalt - Google Patents
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- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/28—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic compounds containing nitrogen, sulfur or phosphorus
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- C08J2419/00—Characterised by the use of rubbers not provided for in groups C08J2407/00 - C08J2417/00
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Abstract
The invention discloses a preparation method of microalgae oil modified rubber asphalt, which is prepared from raw material matrix asphalt, rubber powder, microalgae oil and a cracking agent: firstly, heating matrix asphalt to 160-170 ℃, then slowly adding rubber powder and a cracking agent into the matrix asphalt, shearing and stirring at a high speed of 3500-4000 r/min for 60-90 min at a temperature of 180-185 ℃, and then stirring and developing at a low speed of 500-1000 r/min for 40-60 min at a temperature of 160-170 ℃ to obtain rubber powder modified asphalt; preheating microalgae oil to 160-170 ℃, preheating rubber powder modified asphalt to 160-170 ℃, then slowly adding the microalgae oil into the rubber powder modified asphalt, and shearing and stirring at a high speed of 3500-4000 r/min for 10-30 min at a temperature of 160-170 ℃ to obtain a microalgae oil modified rubber asphalt finished product; according to the invention, the rubber asphalt is modified by using the microalgae oil, the high-temperature performance of the desulfurized rubber asphalt can be remarkably improved by using the stone asphalt component in the microalgae oil, and the problem of overhigh viscosity of the desulfurized rubber asphalt can be solved by using the other low-viscosity components.
Description
Technical Field
The invention relates to an auxiliary material for road engineering construction, in particular to a preparation method of microalgae oil modified rubber asphalt.
Background
The rubber asphalt is used as an auxiliary material to be mixed with the crushed stone aggregate in road engineering construction to form a rubber asphalt mixture, and then the rubber asphalt mixture is paved to form the rubber asphalt concrete pavement. In general, the rubber asphalt is suitable for being used in areas and road sections with higher air temperature, higher traffic volume and other higher requirements on road surface performance.
The waste tires can be changed into valuables by the rubber asphalt, and the harm of the waste tires to the natural environment is reduced, so that the full utilization of the rubber asphalt has great significance to the highway construction and the environmental protection. Because the common rubber asphalt has the defects of poor compatibility and high viscosity, the common rubber asphalt is easy to separate in the storage process and has the defect of difficult construction in the application process. To solve this problem, devulcanized rubber asphalt is generally used. The desulfurized rubber asphalt overcomes the defects of large viscosity and insufficient storage stability of common rubber asphalt, but the high-temperature performance of the desulfurized rubber asphalt is reduced compared with that of the common rubber asphalt, and the viscosity of the desulfurized rubber asphalt is still obviously higher than that of the conventional modified asphalt, so that the desulfurized rubber asphalt is not beneficial to construction. Therefore, it is necessary to combine the characteristics of the desulfurized rubber asphalt, further improve the high-temperature performance of the desulfurized rubber asphalt, reduce the viscosity of the desulfurized rubber asphalt and promote the further popularization and application of the rubber asphalt.
Disclosure of Invention
The invention aims to provide a preparation method of microalgae oil modified rubber asphalt, which improves the high-temperature performance of rubber asphalt and reduces the viscosity.
In order to achieve the purpose, the invention can adopt the following technical scheme:
the preparation method of the microalgae oil modified rubber asphalt comprises the following steps of preparing raw material matrix asphalt, rubber powder, microalgae oil and a cracking agent according to the following weight part ratio:
proportioning: 100 parts of matrix asphalt, 15-35 parts of rubber powder, 15-45 parts of microalgae oil and 0.2-0.6 part of cracking agent;
the preparation method comprises the following steps:
firstly, heating matrix asphalt to 160-170 ℃, then slowly adding rubber powder and a cracking agent into the matrix asphalt, shearing and stirring at a high speed of 3500-4000 r/min for 60-90 min at a temperature of 180-185 ℃, and then stirring and developing at a low speed of 500-1000 r/min for 40-60 min at a temperature of 160-170 ℃ to obtain rubber powder modified asphalt;
the second step is that: preheating microalgae oil to 160-170 ℃, preheating the rubber powder modified asphalt obtained in the first step to 160-170 ℃, then slowly adding the microalgae oil into the rubber powder modified asphalt, and shearing and stirring at a high speed of 3500-4000 r/min for 10-30 min at a temperature of 160-170 ℃ to obtain a microalgae oil modified rubber asphalt finished product.
The rubber powder is prepared by cutting, crushing, grinding and desulfurizing waste tires, and has a particle size of 60-80 meshes and an ash content of less than or equal to 8%.
The cracking agent is octyl phosphate. The octyl phosphate cracking agent can increase the surface energy and chemical energy of rubber powder, enhance the polarity and reactivity of the rubber powder, promote the full action of the rubber powder and the asphalt, improve the interface bonding performance of the rubber powder and the asphalt, decompose the rubber powder into smaller particles to the maximum extent under the high-temperature condition, and completely mix and dissolve the rubber powder into the matrix asphalt.
The microalgae oil used by the invention is prepared by the following steps:
in the first step, ultraviolet rays (0.7-0.8 mW/cm)2) Irradiating with microalgae solution (concentration of 10)4~105one/mL) for 4-6 h, adding bacillus to enable the concentration of the bacillus to reach 106~107The cfu/mL is placed for 20-24 hours at room temperature, so that the microalgae are fully degraded by bacteria; the strong ultraviolet irradiation can kill the microalgae cells, and the bacteria can fully degrade the dead microalgae cells;
the second step is that: separating water-soluble protein in the microalgae liquid obtained in the first step by using a centrifugal filter to obtain a microalgae residue solution;
the third step: putting the microalgae residue solution obtained in the second step in an oven at 100-105 ℃ until the water is completely volatilized to obtain microalgae residues;
the fourth step: adding normal hexane into the microalgae residues, stirring for 1-2 h, standing for 20-24 h, and filtering out insoluble substances in the solution to obtain a normal hexane solution containing microalgae oil;
the fifth step: and (3) heating and distilling the n-hexane solution obtained in the fourth step at 70-80 ℃ to fully volatilize the n-hexane, and extracting to obtain a microalgae oil finished product.
According to the invention, the rubber asphalt is modified by using the microalgae oil, the high-temperature performance of the desulfurized rubber asphalt can be remarkably improved by using the stone asphalt component in the microalgae oil, and the problem of overhigh viscosity of the desulfurized rubber asphalt can be solved by using the other low-viscosity components.
As the main raw material for extracting the microalgae oil, the microalgae is an autotrophic plant with wide land and ocean distribution, rich nutrition and high photosynthetic availability, has strong environmental adaptability, fast production and propagation, high photosynthetic rate and renewable biological resources, so the production cost is low; the microalgae stem cells contain more than 70% of microalgae oil, and the extracted microalgae oil is a black, opaque and asphaltic substance containing 60-70% of asphaltic stone. Compared with common asphalt, the asphalt has higher content of asphaltene and colloid, better high-temperature performance, can obviously improve the performance of the desulfurized rubber asphalt and effectively relieve the dilemma of increasing shortage of nonrenewable resources such as asphalt and the like.
Detailed Description
The present invention is described in greater detail below with reference to specific examples to facilitate understanding and application by those skilled in the art.
Example 1 preparation of crumb rubber modified asphalt as a comparative example
Heating 100 parts of matrix asphalt to 160-170 ℃, slowly adding 20 parts of rubber powder and 0.4 part of cracking agent (adopting octyl phosphate) into the matrix asphalt, shearing and stirring at a high speed of 3500-4000 r/min for 70min at 180-185 ℃, and then stirring at a low speed of 500-1000 r/min for 50min at 160-170 ℃ to obtain the rubber powder modified asphalt.
Example 2 preparation of 1# microalgal oil-modified rubber asphalt
Firstly, extracting microalgae oil
In the first step, 0.7-0.8 mW/cm is used2Ultraviolet irradiation concentration 104~105Adding bacillus into the microalgae liquid of 5h per mL to make the concentration of the bacillus reach 106~107cfu/mL, and standing for 22h at room temperature to fully degrade the microalgae by bacteria;
the second step is that: separating water-soluble protein in the microalgae liquid obtained in the first step by using a centrifugal filter to obtain a microalgae residue solution;
the third step: putting the microalgae residue solution in the second step into an oven at 100 ℃ until the water is completely volatilized to obtain microalgae residue;
the fourth step: adding n-hexane into the microalgae residues, stirring for 1.5h, standing for 22h, and filtering out insoluble substances in the solution to obtain an n-hexane solution containing microalgae oil;
the fifth step: and (3) heating and distilling the n-hexane solution obtained in the fourth step at 75 ℃ to fully volatilize the n-hexane, and extracting to obtain a microalgae oil finished product.
Secondly, preparing 1# microalgae oil modified rubber asphalt
100 parts of the rubber powder modified asphalt prepared in the example 1 and 20 parts of microalgae oil are respectively preheated to 160-170 ℃, then the microalgae oil is slowly added into the rubber powder modified asphalt, and the mixture is sheared and stirred at a high speed of 3500-4000 r/min for 20min at a temperature of 160-170 ℃, so that a finished product of the 1# microalgae oil modified rubber asphalt is obtained.
Example 3 preparation of # 2 microalgal oil-modified rubber asphalt
The extraction of microalgal oil was performed as in example 2.
The method for preparing the 2# microalgae oil modified rubber asphalt comprises the following steps: 100 parts of the rubber powder modified asphalt prepared in the example 1 and 30 parts of microalgae oil are respectively preheated to 160-170 ℃, then the microalgae oil is slowly added into the rubber powder modified asphalt, and the mixture is sheared and stirred at a high speed of 3500-4000 r/min for 20min at a temperature of 160-170 ℃, so that a finished product of the 2# microalgae oil modified rubber asphalt is obtained.
Example 4 preparation of 3# microalgal oil-modified rubber asphalt
The extraction of microalgal oil was performed as in example 2.
The method for preparing the 3# microalgae oil modified rubber asphalt comprises the following steps: 100 parts of the rubber powder modified asphalt prepared in the example 1 and 40 parts of microalgae oil are respectively preheated to 160-170 ℃, then the microalgae oil is slowly added into the rubber powder modified asphalt, and the mixture is sheared and stirred at a high speed of 3500-4000 r/min for 20min at a temperature of 160-170 ℃, so that a finished product of the 3# microalgae oil modified rubber asphalt is obtained.
Example 5 Performance testing of modified asphalts prepared separately in examples 1-4
The four asphalt softening points, brookfield viscosities at 180 ℃ and ductility were tested according to the test method in road engineering asphalt and asphalt mixture test protocol (JTG E20-2011). The test results are shown in table 1.
TABLE 1
Comparing the test results in table 1, it can be seen that the softening points of the 1-3 # microalgal oil-modified rubber asphalt prepared in examples 2-4 are all significantly higher than the comparative example of example 1, indicating that the high temperature performance of the rubber asphalt can be significantly improved after the microalgal oil is added; within a certain range, the higher the microalgae oil mixing amount is, the more obvious the improvement effect is.
The Brookfield viscosity of the 1-3 # microalgae oil modified rubber asphalt prepared in the examples 2-4 is obviously lower than that of the comparative example of the example 1, which shows that the viscosity of the rubber asphalt can be reduced by adding the microalgae oil. While the viscosity of the 3# rubber asphalt prepared in example 4 is lower than that of the comparative example but higher than that of examples 2 and 3, it is shown that the improvement effect of the excessively high microalgae oil content on the viscosity of the rubber asphalt is reduced, but still has a certain improvement effect.
The ductility of the 1-3 # microalgae oil modified rubber asphalt prepared in the embodiments 2-4 is basically equivalent to that of the comparative example in the embodiment 1, which shows that the microalgae oil does not cause obvious adverse effects on the low-temperature performance of the rubber asphalt while improving the high-temperature performance of the rubber asphalt and reducing the viscosity.
Comprehensive analysis shows that: the microalgae oil modified rubber asphalt can obviously improve the high-temperature performance of the rubber asphalt, and simultaneously, the viscosity is reduced, thereby being beneficial to construction; while not significantly degrading low temperature performance.
Claims (3)
1. A preparation method of microalgae oil modified rubber asphalt is characterized by comprising the following steps: the asphalt is prepared from raw material matrix asphalt, rubber powder, microalgae oil and octyl phosphate according to the following weight part ratio and method:
proportioning: 100 parts of matrix asphalt, 15-35 parts of rubber powder, 15-45 parts of microalgae oil and 0.2-0.6 part of octyl phosphate;
the preparation method comprises the following steps:
firstly, heating matrix asphalt to 160-170 ℃, slowly adding rubber powder and octyl phosphate into the matrix asphalt, shearing and stirring at a high speed of 3500-4000 r/min for 60-90 min at a temperature of 180-185 ℃, and then stirring and developing at a low speed of 500-1000 r/min for 40-60 min at a temperature of 160-170 ℃ to obtain rubber powder modified asphalt;
the second step is that: preheating microalgae oil to 160-170 ℃, preheating the rubber powder modified asphalt obtained in the first step to 160-170 ℃, then slowly adding the microalgae oil into the rubber powder modified asphalt, and shearing and stirring at a high speed of 3500-4000 r/min for 10-30 min at a temperature of 160-170 ℃ to obtain a microalgae oil modified rubber asphalt finished product.
2. The method for preparing microalgae oil modified rubber asphalt according to claim 1, which is characterized in that: the rubber powder is prepared by cutting, crushing, grinding and desulfurizing waste tires, and has a particle size of 60-80 meshes and an ash content of less than or equal to 8%.
3. The method for preparing microalgae oil modified rubber asphalt according to claim 1, which is characterized in that: the microalgae oil is prepared by the following steps:
firstly, irradiating microalgae liquid for 4-6 hours by using ultraviolet rays, adding bacillus, and standing for 20-24 hours at room temperature to fully degrade the microalgae by bacteria;
the second step is that: centrifugally filtering the water-soluble protein in the microalgae liquid obtained in the first step to obtain a microalgae residue solution;
the third step: putting the microalgae residue solution obtained in the second step in an oven at 100-105 ℃ until the water is completely volatilized to obtain microalgae residues;
the fourth step: adding normal hexane into the microalgae residues, stirring for 1-2 h, standing for 20-24 h, and filtering out insoluble substances in the solution to obtain a normal hexane solution containing microalgae oil;
the fifth step: and (3) heating and distilling the n-hexane solution obtained in the fourth step at 70-80 ℃ to fully volatilize the n-hexane, and extracting to obtain a microalgae oil finished product.
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| CN101613618A (en) * | 2008-06-27 | 2009-12-30 | 新奥科技发展有限公司 | A kind of is the feedstock production method of bio-diesel oil with the microalgae grease |
| WO2011153152A3 (en) * | 2010-06-01 | 2012-03-29 | Iowa State University Research Foundation, Inc. | Bio-oil formulation as an asphalt substitute |
| CN108329702A (en) * | 2018-01-18 | 2018-07-27 | 广西大学 | A kind of preparation method of algal oil Biological asphalt and algal oil Biological asphalt mixture |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101613618A (en) * | 2008-06-27 | 2009-12-30 | 新奥科技发展有限公司 | A kind of is the feedstock production method of bio-diesel oil with the microalgae grease |
| WO2011153152A3 (en) * | 2010-06-01 | 2012-03-29 | Iowa State University Research Foundation, Inc. | Bio-oil formulation as an asphalt substitute |
| CN108329702A (en) * | 2018-01-18 | 2018-07-27 | 广西大学 | A kind of preparation method of algal oil Biological asphalt and algal oil Biological asphalt mixture |
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| Title |
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