CN103396818A - Biological asphalt and its preparation method - Google Patents
Biological asphalt and its preparation method Download PDFInfo
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- CN103396818A CN103396818A CN2013102547738A CN201310254773A CN103396818A CN 103396818 A CN103396818 A CN 103396818A CN 2013102547738 A CN2013102547738 A CN 2013102547738A CN 201310254773 A CN201310254773 A CN 201310254773A CN 103396818 A CN103396818 A CN 103396818A
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Abstract
The invention relates to a biological asphalt. Specifically, its needle penetration is 30-150dmm at 25DEG C, the softening point is 40-80DEG C, the 15DEG C ductility is 5-25cm, the 90DEG C Brookfield rotary viscosity growth rate is 0.1-0.5pa.s/h, the 120DEG C Brookfield viscosity growth rate is 0.07-1.5pa.s/h, the alcohol content is 5-30% by mass. The invention also provides a preparation method of the biological asphalt. The preparation method disclosed in the invention is simple and practicable, the production process has small pollution, and the raw materials are easily available. The obtained biological asphalt has greatly improved thermal stability, and can be directly used in production of road asphalt mixture for road paving.
Description
Technical field
The invention belongs to road engineering bituminous material technical field, relate to particularly a kind of biological pitch with the bio oil preparation.
The invention still further relates to a kind of method for preparing above-mentioned biological pitch.
Background technology
Biomass contain heavy component and the resistates of 20%-40% in the bio oil of the methods such as pyrolysis preparation, be the starting material of the biological bituminous material of a kind of reasonable preparation.These heavy components and resistates can make the mixture material that high-molecular hydrocarbons with agglutinate performance and nonmetal derivative thereof form-be biological pitch through separation and deep processing, modification.
Directly pyrolysis is considered to the most promising biomass liquefying technology, and its development is very rapid.Pyrolytic process is substantially all that the mode by rapid heating makes the high molecular polymer that forms biomass be cracked into low molecule organic matter steam, and adopts the method for quenching, and it is condensed into liquid-bio oil.Because this process does not reach thermodynamic(al)equilibrium, so bio oil with and the physicochemical property of separated portion usually unstable, main manifestations is that bio oil is with storage time and temperature change, cause it that physicochemical change occurs, viscosity increase etc., also there is similar problem in biological pitch, has greatly hindered the use of biological pitch.
Summary of the invention
The object of the present invention is to provide a kind of heat-staple biological pitch.
Another purpose of the present invention is to provide a kind of method for preparing biological pitch.
For achieving the above object, biological pitch provided by the invention, wherein, 25 ℃ of penetration degrees are 30-150dmm, softening temperature is 40-80 ℃, and 15 ℃ of ductilities are 5-25cm, and 90 ℃ of Bu Shi rotation viscosity rates of rise are 0.1-0.5pa.s/h, 120 ℃ of Bu Shi viscosity rates of rise are 0.07-1.5pa.s/h, and the mass ratio of pure content is 5-30% (preferably pure content is 10-20%).
In described biological pitch, alcohol is for containing the material of oh group.
In described biological pitch, alcohol is one or more in ethylene glycol, glycerol, 1,2-PD, polyoxyethylene glycol, phenylcarbinol.
The method of the above-mentioned biological pitch of preparation provided by the invention, the steps include:
Bio oil and solvent, filter, centrifugation obtains indissolvable component, and indissolvable component is mixed with pure, directly contacts that to be stirred to softening temperature be 40 ℃-80 ℃ under 80 ℃-120 ℃ with air.Preferably preparation condition is that bio oil and solvent were mixed in 1: 5 by volume, and stirs in 5 ℃-15 ℃.
In described method, bio oil is that biomass are through pyrogenically prepared oily liquids product.
In described method, bio oil is one or more in maize straw, oak, switchgrass, rice husk.
In described method, solvent is water or organic solvent.
In described method, solvent is deionized water or methylene dichloride.
Effect of the present invention is:
1) can solve the present known biological pitch unstable properties problem of being heated.
2) in the biological pitch course of processing by adding the method for alcohols chemical, make the active substance in biological pitch be transformed into inactive substance, greatly improved the stability of biological pitch, be conducive to biological pitch and partially or completely replace petroleum pitch, reduced the dependency to petroleum resources.
3) starting material of the present invention derive from cheap biomass resource, utilize the biological bituminous material of heavy component processing in bio-oil to improve and take full advantage of biomass energy, improve the additional utility value of biomass energy.
4) the present invention has that technique is simple, cost is low, the characteristics of excellent performance.
Description of drawings
Fig. 1 is biological pitch of the present invention in the Bu Shi viscosity of 90 ℃-soaking time curve.
Fig. 2 is biological pitch of the present invention in the Bu Shi viscosity of 120 ℃-soaking time curve.
Embodiment
The present invention is take bio oil as raw material, mix with solvent (water or methylene dichloride), filtration, centrifugation obtain indissolvable component, (mass ratio of pure content is 5-30% with alcohol with indissolvable component, preferably pure content is 10-20%) mix, directly contacting and constantly be stirred to softening temperature with air under 80 ℃ of-120 ℃ of conditions is 40 ℃-80 ℃.The bio oil that the present invention adopts is by solvent extraction, can effectively remove the light constituent of bio oil system, acquisition is fit to prepare the active principle of pitch, but still there are the reactive behavior materials such as carboxylic-acid in these components, by adding alcohol, effectively the reactive behavior material in the removal system or with the high reactivity Substance Transformation, be the low activity material, improve the stability of biological pitch.
Preferably described bio oil is mixed and put into a container by 1: 5 (volume ratio) with solvent, this container is placed in 5 ℃ of-15 ℃ of circulator baths, constantly stir 30min-50min, then container is placed in standing 0.5-1h under normal temperature, filtration, drying are reacted with alcohol again.
The bio oil that the present invention adopts is the pyrogenically prepared oily liquids product of biomass process, and wherein said biomass comprise one or more in maize straw, oak, switchgrass, rice husk.
The stable biological pitch of thermal characteristics by aforesaid method preparation of the present invention, 25 ℃ of penetration degrees are 30-150dmm, softening temperature is 40-80 ℃, 15 ℃ of ductilities are 5-25cm, 90 ℃ of Bu Shi rotation viscosity rates of rise are in the 0.1-0.5pa.s/h scope, and 120 ℃ of Bu Shi viscosity rates of rise are in the 0.07-1.5pa.s/h scope.
Below will embodiment of the present invention be described by embodiment and comparative example, but the present invention is not limited to these specific embodiment.
The starting material that use in each embodiment are known products.
Embodiment 1:
Cornstalk biological oil is mixed with water, in 5 ℃ of circulator baths, stir 30min, then container is placed in standing 0.5h under normal temperature, filtration, centrifugation, add 10% glycerol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 35min, obtain biological pitch 1.
Embodiment 2:
Cornstalk biological oil is mixed with water, in 5 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, add 20% glycerol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 65min, obtain biological pitch 2.
Embodiment 3:
Cornstalk biological oil is mixed with methylene dichloride, in 15 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, add 30% glycerol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 70min, obtain biological pitch 3.
Embodiment 4:
The rice husk bio oil is mixed with water, in 10 ℃ of circulator baths, stir 40min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, add 10% ethylene glycol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 80min, obtain biological pitch 4.
Embodiment 5:
The oak bio oil is mixed with methylene dichloride, in 13 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, add 20%1,2-propylene glycol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 60min, obtain biological pitch 5.
Embodiment 6:
The oak bio oil is mixed with water, in 15 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, add 10%1,2-propylene glycol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 85min, obtain biological pitch 5.
Embodiment 7:
The oak bio oil is mixed with methylene dichloride, in 5 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, add 10% polyoxyethylene glycol in indissolvable component, directly contact with air under 95 ℃ of conditions, stir oxidation 100min, obtain biological pitch 6.
Comparative example 1:
The rice husk bio oil is mixed with water, in 5 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, indissolvable component directly contacts with air under 100 ℃, stir oxidation 0.5h.
Comparative example 2:
The rice husk bio oil is mixed with methylene dichloride, in 5 ℃ of circulator baths, stir 50min, then container is placed in standing 1h under normal temperature, filtration, centrifugation, indissolvable component directly contacts with air under 100 ℃ of conditions, stir oxidation 1h.
The biological pitch of embodiment gained has been carried out respectively the traditional performance test, and the several embodiment that choose in embodiment 1-6 have carried out the Bu Shi rotation viscosity test of the biological pitch of different soaking times from comparative example.Test result in Table 1, table 2 and table 3 and Fig. 1 and Fig. 2.
Can be reached a conclusion by data variation trend in data and figure in table, with known biological pitch, compare, biological asphalt viscosity rate of rise of the present invention obviously diminishes, and performance is more stable.
Table 1: three norms
| Sequence | Penetration degree (25 ℃, dmm) | Softening temperature (℃) | Ductility (15 ℃, cm) |
| |
98.6 | 49 | 19.8 |
| |
45.4 | 54.6 | 5.2 |
| |
123 | 47.4 | 23.8 |
| |
120.4 | 48.6 | 22.2 |
| |
95.2 | 49.6 | 25.5 |
| Embodiment 6 | 27.4 | 58.4 | - |
| Comparative example 1 | 51.7 | 51.7 | 1.8 |
| Comparative example 2 | - | 55.8 | - |
Show 2:90 ℃ of Bu Shi rotation viscosity
| Soaking time (h) | |
|
|
|
Comparative example 1 |
| 0.5 | 7.213 | 2.51 | 3.74 | 3.453 | 2.483 |
| 1 | 7.777 | 2.593 | 3.942 | 3.536 | 2.664 |
| 1.5 | 8.26 | 2.7 | 4.016 | 3.622 | 2.846 |
| 2 | 8.515 | 2.77 | 4.239 | 3.718 | 2.880 |
| 2.5 | 8.782 | 2.744 | 4.285 | 3.751 | 2.955 |
| 3 | 8.956 | 2.845 | 4.445 | 3.851 | 3.125 |
Show 3:120 ℃ of Bu Shi rotary viscosity
| | Embodiment | 4 | Embodiment 6 | Embodiment 7 | Comparative example 2 |
| 0.5 | 0.3947 | 0.615 | 2.326 | 5.525 | |
| 1 | 0.4422 | 0.695 | 2.55 | 7.25 | |
| 1.5 | 0.5023 | 0.845 | 2.988 | 9.533 | |
| 2 | 0.5377 | 0.888 | 3.264 | 12.53 | |
| 2.5 | 0.5564 | 1.008 | 3.488 | 14.65 | |
| 3 | 0.5942 | 1.131 | 3.822 | 19.06 | |
| 3.5 | 0.6474 | 1.237 | 4.492 | 22.19 |
Claims (10)
1. biological pitch, wherein, 25 ℃ of penetration degrees are 30-150dmm, softening temperature is 40-80 ℃, and 15 ℃ of ductilities are 5-25cm, and 90 ℃ of Bu Shi rotation viscosity rates of rise are 0.1-0.5pa.s/h, 120 ℃ of Bu Shi viscosity rates of rise are 0.07-1.5pa.s/h, and the mass ratio of pure content is 5-30%.
2. biological pitch according to claim 1, wherein, the mass ratio of pure content is 10-20%.
3. biological pitch according to claim 1 and 2, wherein, pure for containing the material of oh group.
4. biological pitch according to claim 3, wherein, alcohol is one or more in ethylene glycol, glycerol, 1,2-PD, polyoxyethylene glycol, phenylcarbinol.
5. prepare the method for the described biological pitch of claim 1, the steps include:
Bio oil and solvent, filter, centrifugation obtains indissolvable component, and indissolvable component is mixed with pure, directly contacts that to be stirred to softening temperature be 40 ℃-80 ℃ under 80 ℃-120 ℃ with air.
6. method according to claim 5, wherein, bio oil is that biomass are through pyrogenically prepared oily liquids product.
7. method according to claim 6, wherein, bio oil is one or more in maize straw, oak, switchgrass, rice husk.
8. method according to claim 5, wherein, the volume ratio of bio oil and solvent is 1: 5, is uniformly mixed in 5 ℃-15 ℃.
9. method according to claim 5, wherein, solvent is water or organic solvent.
10. method according to claim 9, wherein, solvent is deionized water or methylene dichloride.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194363A (en) * | 2014-09-02 | 2014-12-10 | 汪青 | Maize-based alcohol still residue modified pavement petroleum asphalt and preparation method thereof |
| CN104388107A (en) * | 2014-11-03 | 2015-03-04 | 交通运输部公路科学研究所 | Esterified biological asphalt and preparation method thereof |
| CN104388108A (en) * | 2014-11-03 | 2015-03-04 | 交通运输部公路科学研究所 | Method for preparing catalytically hydrogenated biological asphalt |
| CN105038832A (en) * | 2015-07-31 | 2015-11-11 | 长安大学 | Biological asphalt for road as well as preparation device and preparation method of biological asphalt |
| CN106336673A (en) * | 2016-08-25 | 2017-01-18 | 深圳市市政设计研究院有限公司 | Biological oil compounded nanometer diatomite modified asphalt and preparation method thereof |
| 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 |
| CN110183868A (en) * | 2019-06-24 | 2019-08-30 | 长安大学 | Application and sustainable modified pitch and preparation method of the Poplar Powder liquefaction products as sustainable asphalt modifier |
| CN112080314A (en) * | 2019-06-14 | 2020-12-15 | 北京三聚绿能科技有限公司 | Modified biological asphalt and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194363A (en) * | 2014-09-02 | 2014-12-10 | 汪青 | Maize-based alcohol still residue modified pavement petroleum asphalt and preparation method thereof |
| CN104388107A (en) * | 2014-11-03 | 2015-03-04 | 交通运输部公路科学研究所 | Esterified biological asphalt and preparation method thereof |
| CN104388108A (en) * | 2014-11-03 | 2015-03-04 | 交通运输部公路科学研究所 | Method for preparing catalytically hydrogenated biological asphalt |
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| CN105038832B (en) * | 2015-07-31 | 2017-08-08 | 长安大学 | A kind of road Biological asphalt and its preparation facilities and preparation method |
| CN106336673A (en) * | 2016-08-25 | 2017-01-18 | 深圳市市政设计研究院有限公司 | Biological oil compounded nanometer diatomite modified asphalt and preparation method thereof |
| 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 |
| CN112080314A (en) * | 2019-06-14 | 2020-12-15 | 北京三聚绿能科技有限公司 | Modified biological asphalt and preparation method thereof |
| CN112080314B (en) * | 2019-06-14 | 2022-04-19 | 北京三聚绿能科技有限公司 | Modified biological asphalt and preparation method thereof |
| CN110183868A (en) * | 2019-06-24 | 2019-08-30 | 长安大学 | Application and sustainable modified pitch and preparation method of the Poplar Powder liquefaction products as sustainable asphalt modifier |
| CN110183868B (en) * | 2019-06-24 | 2021-11-19 | 长安大学 | Application of poplar powder liquefied product as sustainable asphalt modifier, sustainable modified asphalt and preparation method |
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