CN103396818B - Biological asphalt and its preparation method - Google Patents

Biological asphalt and its preparation method Download PDF

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Publication number
CN103396818B
CN103396818B CN201310254773.8A CN201310254773A CN103396818B CN 103396818 B CN103396818 B CN 103396818B CN 201310254773 A CN201310254773 A CN 201310254773A CN 103396818 B CN103396818 B CN 103396818B
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biological asphalt
bio oil
asphalt
alcohol
biological
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CN103396818A (en
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曹东伟
何敏
吴小维
张海燕
宋昭睿
赵立东
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Research Institute of Highway Ministry of Transport
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Research Institute of Highway Ministry of Transport
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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

A kind of Biological asphalt and preparation method thereof
Technical field
The invention belongs to road engineering asphalt material technical field, relate to Biological asphalt prepared by a kind of bio oil particularly.
The invention still further relates to a kind of method preparing above-mentioned Biological asphalt.
Background technology
Heavy component containing 20%-40% in the bio oil that biomass are prepared through methods such as pyrolysis and resistates are a kind of starting material of reasonable preparation Biological asphalt material.These heavy components and resistates can obtain the mixture material-i.e. Biological asphalt of high-molecular hydrocarbons and the nonmetal derivative composition thereof with agglutinate performance through separation and deep processing, modification.
Direct pyrolysis is considered to the most promising biomass liquefying technology, and its development is very rapid.Pyrolytic process is substantially all make the high molecular polymer of composition biomass be cracked into low molecule organic matter steam by the mode of rapid heating, and adopts the method for quenching, is condensed into liquid-bio oil.Because this process does not reach thermodynamic(al)equilibrium, so the physicochemical property of bio oil and its separated portion are 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 asphalt, greatly hinders the use of Biological asphalt.
Summary of the invention
The object of the present invention is to provide a kind of heat-staple Biological asphalt.
Another object of the present invention is to provide a kind of method preparing Biological asphalt.
For achieving the above object, Biological asphalt provided by the invention, wherein, 25 DEG C of penetration degrees are 30-150dmm, softening temperature is 40-80 DEG C, and 15 DEG C of ductilities are 5-25cm, and it is 0.1-0.5pa.s/h that 90 DEG C of Bu Shi rotate viscosity rate of rise, 120 DEG C of Bu Shi viscosity rates of rise are 0.07-1.5pa.s/h, and the mass ratio of alcohol content is 5-30% (preferably alcohol content is 10-20%).
In described Biological asphalt, alcohol is the material containing oh group.
In described Biological asphalt, alcohol is one or more in ethylene glycol, glycerol, 1,2-PD, polyoxyethylene glycol, phenylcarbinol.
The method of the above-mentioned Biological asphalt of preparation provided by the invention, the steps include:
Bio oil and solvent, filtration, centrifugation obtain indissolvable component, and mixed with alcohol by indissolvable component, directly contacting with air at 80 DEG C-120 DEG C and being stirred to softening temperature is 40 DEG C-80 DEG C.Preferably preparation condition to be mixed at 1: 5 by volume bio oil and solvent, and stir in 5 DEG C-15 DEG C.
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) current known Biological asphalt can be solved to be heated unstable properties problem.
2) in the Biological asphalt course of processing by adding the method for alcohols chemical, the active substance in Biological asphalt is made to be transformed into inactive substance, substantially increase the stability of Biological asphalt, be conducive to Biological asphalt and partially or completely replace petroleum pitch, reduce the dependency to petroleum resources.
3) raw material sources of the present invention is in cheap biomass resource, utilizes the processing of the heavy component in bio-oil Biological asphalt material to improve and makes full use of biomass energy, improve the additional utility value of biomass energy.
4) the present invention has that technique is simple, cost is low, the feature of excellent performance.
Accompanying drawing explanation
Fig. 1 is that Biological asphalt of the present invention is in the Bu Shi viscosity-soaking time curve of 90 DEG C.
Fig. 2 is that Biological asphalt of the present invention is in the Bu Shi viscosity-soaking time curve of 120 DEG C.
Embodiment
The present invention take bio oil as raw material, mix with solvent (water or methylene dichloride), filtration, centrifugation obtain indissolvable component, by indissolvable component and alcohol, (mass ratio of alcohol content is 5-30%, preferably alcohol content is 10-20%) mixing, directly contacting with air and be constantly stirred to softening temperature under 80 DEG C of-120 DEG C of conditions is 40 DEG C-80 DEG C.The bio oil that the present invention adopts passes through solvent extraction, effectively can remove the light constituent of bio oil system, obtain and be applicable to the active principle preparing pitch, but still there is the reactive behavior materials such as carboxylic-acid in these components, by adding alcohol, reactive behavior material in effective removal system or high active substance is converted into low activity material, improves the stability of Biological asphalt.
Preferably described bio oil and solvent are mixed by 1: 5 (volume ratio) and put into a container, this container is placed in 5 DEG C of-15 DEG C of circulator baths, continuous stirring 30min-50min, leave standstill 0.5-1h under then container being placed in normal temperature, filtration, drying are reacted with alcohol again.
The present invention adopt bio oil be biomass through pyrogenically prepared oily liquids product, wherein said biomass comprise one or more in maize straw, oak, switchgrass, rice husk.
The Biological asphalt that the thermal characteristics prepared by aforesaid method of the present invention is stable, 25 DEG C of penetration degrees are 30-150dmm, softening temperature is 40-80 DEG C, 15 DEG C of ductilities are 5-25cm, 90 DEG C of Bu Shi rotate viscosity rate of rise within the scope of 0.1-0.5pa.s/h, and 120 DEG C of Bu Shi viscosity rates of rise are within the scope of 0.07-1.5pa.s/h.
Below by embodiment and comparative example, embodiment of the present invention will be described, but the present invention is not limited to these specific embodiments.
The starting material used in each embodiment are known products.
Embodiment 1:
Cornstalk biological oil is mixed with water, in 5 DEG C of circulator baths, stirs 30min, then leave standstill 0.5h under container being placed in normal temperature, filtration, centrifugation, add 10% glycerol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 35min, obtain Biological asphalt 1.
Embodiment 2:
Cornstalk biological oil is mixed with water, in 5 DEG C of circulator baths, stirs 50min, then leave standstill 1h under container being placed in normal temperature, filtration, centrifugation, add 20% glycerol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 65min, obtain Biological asphalt 2.
Embodiment 3:
Cornstalk biological oil is mixed with methylene dichloride, in 15 DEG C of circulator baths, stirs 50min, then leave standstill 1h under container being placed in normal temperature, filtration, centrifugation, add 30% glycerol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 70min, obtain Biological asphalt 3.
Embodiment 4:
Rice husk bio oil is mixed with water, in 10 DEG C of circulator baths, stirs 40min, then leave standstill 1h under container being placed in normal temperature, filtration, centrifugation, add 10% ethylene glycol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 80min, obtain Biological asphalt 4.
Embodiment 5:
Oak bio oil is mixed with methylene dichloride, in 13 DEG C of circulator baths, stirs 50min, under then container being placed in normal temperature, leave standstill 1h, filtration, centrifugation, add 20%1,2-propylene glycol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 60min, obtain Biological asphalt 5.
Embodiment 6:
Oak bio oil is mixed with water, in 15 DEG C of circulator baths, stirs 50min, under then container being placed in normal temperature, leave standstill 1h, filtration, centrifugation, add 10%1,2-propylene glycol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 85min, obtain Biological asphalt 5.
Embodiment 7:
Oak bio oil is mixed with methylene dichloride, in 5 DEG C of circulator baths, stirs 50min, then leave standstill 1h under container being placed in normal temperature, filtration, centrifugation, add 10% polyoxyethylene glycol in indissolvable component, directly contact with air under 95 DEG C of conditions, stir oxidation 100min, obtain Biological asphalt 6.
Comparative example 1:
Rice husk bio oil mixed with water, in 5 DEG C of circulator baths, stir 50min, leave standstill 1h under then container being placed in normal temperature, filtration, centrifugation, indissolvable component directly contacts with air at 100 DEG C, stirs oxidation 0.5h.
Comparative example 2:
Rice husk bio oil mixed with methylene dichloride, in 5 DEG C of circulator baths, stir 50min, leave standstill 1h under then container being placed in normal temperature, filtration, centrifugation, indissolvable component directly contacts with air under 100 DEG C of conditions, stirs oxidation 1h.
Respectively traditional performance test is carried out to embodiment gained Biological asphalt, and has chosen Bu Shi that several embodiment in embodiment 1-6 and comparative example carried out different soaking time Biological asphalt and rotate viscosity and test.Test result is 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 in table and figure, compared with known Biological asphalt, 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 DEG C, dmm) Softening temperature (DEG C) Ductility (15 DEG C, cm)
Embodiment 1 98.6 49 19.8
Embodiment 2 45.4 54.6 5.2
Embodiment 3 123 47.4 23.8
Embodiment 4 120.4 48.6 22.2
Embodiment 5 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 DEG C of Bu Shi and rotate viscosity
Soaking time (h) Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 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 DEG C of Bu Shi rotary viscosity
Soaking time 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 (4)

1. a Biological asphalt, wherein, 25 DEG C of penetration degrees are 30-150dmm, softening temperature is 40-80 DEG C, and 15 DEG C of ductilities are 5-25cm, and it is 0.1-0.5pa.s/h that 90 DEG C of Bu Shi rotate viscosity rate of rise, 120 DEG C of Bu Shi viscosity rates of rise are 0.07-1.5pa.s/h, and the mass ratio of alcohol content is 5-30%; Wherein, alcohol is one or more in ethylene glycol, glycerol, 1,2-PD, polyoxyethylene glycol, phenylcarbinol.
2. Biological asphalt according to claim 1, wherein, the mass ratio of alcohol content is 10-20%.
3. prepare the method for Biological asphalt described in claim 1, the steps include:
Bio oil and solvent, filtration, centrifugation obtain indissolvable component, and mixed with alcohol by indissolvable component, directly contacting with air at 80 DEG C-120 DEG C and being stirred to softening temperature is 40 DEG C-80 DEG C; Wherein:
Alcohol is one or more in ethylene glycol, glycerol, 1,2-PD, polyoxyethylene glycol, phenylcarbinol;
Bio oil is that biomass are through pyrogenically prepared oily liquids product;
The volume ratio of bio oil and solvent is 1:5, is uniformly mixed in 5 DEG C-15 DEG C;
Solvent is deionized water or methylene dichloride.
4. method according to claim 3, wherein, biomass are one or more in maize straw, oak, switchgrass, rice husk.
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Publication number Priority date Publication date Assignee Title
CN104194363B (en) * 2014-09-02 2016-04-13 汪青 Utilize residual modification bi tumenf orr oad of corn-based alcohols still and preparation method thereof
CN104388107B (en) * 2014-11-03 2017-02-15 交通运输部公路科学研究所 Esterified biological asphalt and preparation method thereof
CN104388108B (en) * 2014-11-03 2017-05-03 交通运输部公路科学研究所 Method for preparing catalytically hydrogenated biological asphalt
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
CN106336673B (en) * 2016-08-25 2019-02-01 深圳市市政设计研究院有限公司 A kind of bio oil compounding nano diatomite modified pitch 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
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

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