CN107916122A - A kind of Biological asphalt and preparation method thereof - Google Patents
A kind of Biological asphalt and preparation method thereof Download PDFInfo
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- CN107916122A CN107916122A CN201610881684.XA CN201610881684A CN107916122A CN 107916122 A CN107916122 A CN 107916122A CN 201610881684 A CN201610881684 A CN 201610881684A CN 107916122 A CN107916122 A CN 107916122A
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- glycerine
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- thermal decomposition
- decomposition product
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/002—Working-up pitch, asphalt, bitumen by thermal means
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The present invention relates to a kind of Biological asphalt and preparation method thereof.The preparation method includes the following steps：1) inorganic salts are mixed in bio oil, mixed；Crude glycerine is added, is mixed；2) air-distillation is carried out to step 1) products therefrom, isolates light components and the blending ingredients including glycerine and lignin thermal decomposition product；3) add water into the blending ingredients, mix, stand, filtering, removes water glycerine mixed phase therein, obtain rugose wood element thermal decomposition product；4) the rugose wood element thermal decomposition product is heated to constant weight state, obtains Biological asphalt；The water glycerine mixed phase is subjected to air-distillation, the glycerine isolated recycles.Wherein lignin thermal decomposition product can be efficiently separated out by carrying out pretreatment to biomass pyrolysis oil, while this separating technology is improved so that the asphalt component in biomass pyrolysis oil can have more preferably performance and anti-aging property while being sufficiently separated out to conventional distil-lation.
Description
Technical field
The present invention relates to a kind of Biological asphalt and preparation method thereof, belongs to recyclable organism-based road asphalt material and prepares skill
Art field.
Background technology
At present, both at home and abroad to bio oil it is refined using be concentrated mainly on by chemical process by cellulose in biomass with
The light components that hemicellulose is pyrolyzed are converted into emulsion fuel, fuel oil additive and high valuable chemicals, by wood
What quality was pyrolyzed accounts for the bio oil heavy constituent of bio oil larger proportion because more difficult conversion is not utilized effectively always.
In order to more fully utilize the potential alternate resources of this fossil energy of bio oil and alleviate asphalt supply
Increasingly intense situation, both at home and abroad correlation scholar started to prepare the trial and of road asphalt material using biomass resource
Through achieving certain progress, the bio-based road asphalt material prepared using biomass resource is defined as biology by the country
Asphalt material.
With reference to CN102796547A《Biological asphalt, biological asphalt composition and preparation method thereof》With CN103396818A
《A kind of Biological asphalt and preparation method thereof》Etc. scheme it can be concluded that main problem existing for Biological asphalt material at this stage
Have：1) due to containing substantial amounts of water-soluble substances in biomass pyrolysis oil, thus it is suitable for use as the lignin pyrolysis of asphalt material
Product can be with there is asphalt performance the water-soluble component of larger negative effect to form emulsion so that more difficult separate；2) Biological asphalt
Material is because thus there are the poor spy of cryogenic property and anti-aging property there are the oxygen-containing functional group such as more carboxyl and aldehyde radical
Property；3) there are easily make it when process conditions are harsh, financial cost is high and separates for the separation of current biological pitch and preparation method
The characteristics of structural change or introducing other impurities.
The content of the invention
The object of the present invention is to provide a kind of Biological asphalt and preparation method thereof.By being located in advance to biomass pyrolysis oil
Reason then effectively can easily isolate the component for being wherein suitable for use as bio-based road asphalt material, at the same to conventional distil-lation this
One separating technology is improved so that the asphalt component in biomass pyrolysis oil can have more while being sufficiently separated out
Excellent performance and anti-aging property, for promoting the further exploitation of bio-based road asphalt material and applying and renewable
The structure of resource oriented economy has positive effect.
To achieve these goals, the present invention provides a kind of preparation method of Biological asphalt, include the following steps：
1) inorganic salts are mixed in bio oil, mixed；Crude glycerine is added, is mixed；
2) air-distillation is carried out to step 1) products therefrom, isolates light components and be pyrolyzed including glycerine and lignin
The blending ingredients of product；
3) add water into the blending ingredients, mix, stand, filtering, removes water-glycerol mixed phase therein, obtains thick
Lignin thermal decomposition product；
4) the rugose wood element thermal decomposition product is heated to constant weight state, obtains Biological asphalt；The water-glycerol is mixed
Air-distillation is mutually carried out, the glycerine isolated recycles.
In Biological asphalt preparation method of the present invention, in step 1), the bio oil is by pine, willow or poplar
Pyrogenically prepared.The crude glycerine is preferably the accessory substance of biodiesel.
In Biological asphalt preparation method of the present invention, in step 1), the inorganic salts are Cacl2, Fecl3Or Licl
In one or more, preferably Cacl2；The incorporation of the inorganic salts is the 1~10% of biological oil quality, preferably 2~
4%, more preferably 3%.
In Biological asphalt preparation method of the present invention, in step 1), the mass ratio of the bio oil and crude glycerine is
1：2~4, it is preferably 1:2~3, more preferably 1:2.
In Biological asphalt preparation method of the present invention, in step 2), it is described distillation to gas phase final temperature for 200 DEG C~
250 DEG C, preferably 225 DEG C~250 DEG C.
In Biological asphalt preparation method of the present invention, in step 3), (glycerine is pyrolyzed the blending ingredients with lignin
Product) with mixing the mass ratio of water therein as 1：4~7, it is preferably 1:4.5~5.5, more preferably 1:5.
In Biological asphalt preparation method of the present invention, in step 4), the rugose wood element thermal decomposition product in 100~
105 DEG C are heated to constant weight state.
As one of preferred embodiment of the present invention, the preparation method of the Biological asphalt includes the following steps：
1) by Cacl2With the incorporation of mass percent 2~4% by pine, poplar or the pyrogenically prepared bio oil of willow, mixing
It is even；Add the accessory substance crude glycerine of biodiesel, the mass ratio of the bio oil and crude glycerine is 1：2~4, mix；It is described
Bio oil is pyrogenically prepared by pine, willow or poplar；
2) by step 1) products therefrom air-distillation to gas phase final temperature be 225 DEG C~250 DEG C, isolate light components and
Blending ingredients including glycerine and lignin thermal decomposition product；
3) with mass ratio 1：4~7 into the blending ingredients plus water, mixing, 2~2.5h of standing, filtering, removing are therein
Water-glycerol mixed phase, obtains rugose wood element thermal decomposition product；
4) the rugose wood element thermal decomposition product is heated to constant weight state in 100~105 DEG C, obtains Biological asphalt；By institute
State water-glycerol mixed phase and carry out air-distillation, the glycerine isolated recycles.
The present invention also provides the Biological asphalt as made from the above method.
Beneficial effects of the present invention are as follows：
(1) present invention use derive from a wealth of sources, be of low cost, environmentally protective and reproducible biomass resource for raw material, its
Cost has a clear superiority relative to conventional asphalt.
(2) present invention is also improved the distillation technique of bio oil, innovatively by the pair of industrial production biodiesel
Product-nontoxic, harmless, inexpensive and high boiling crude glycerine introduce distillation system as the diluent distilled, not only effectively
Avoid the lignin thermal decomposition product in bio oil that coking occurs so as to improve its performance as bio-based asphalt material,
Also utilize the hydroxy functional group in crude glycerine esterification can occur with the part carboxyl functional group in lignin thermal decomposition product
Characteristic improve the anti-aging property of Biological asphalt, crude glycerine used can be steamed after the completion of whole preparation process by normal pressure
Evaporate recycling.
(3) present invention originally introduces inorganic salts conduct before the separation of lignin thermal decomposition product and helps release agent, it is intended to
Realize to the water-dissolving phase in bio oil and the demulsification of non-aqueous phase so that the water-soluble substances being harmful to asphalt performance is follow-up
Separated to a greater degree in distillation technique.
In conclusion the present invention has the characteristics that preparation process is simple, easily operated and of low cost, and can be certain
Degree improves the performance and anti-aging property of Biological asphalt material.
Brief description of the drawings
Fig. 1 is that the Bu Shi viscositys of 1~3 gained Biological asphalt of comparative example and embodiment change over time curve.
Embodiment
Following embodiments are used to illustrate the present invention, but are not limited to the scope of the present invention.
Raw materials used present embodiment is commercial product.
A kind of preparation method of 1 Biological asphalt of embodiment
The present embodiment provides a kind of preparation method of Biological asphalt, include the following steps：
1) by 30gCacl2Mix in 1000g pine pyrolysis oils, 600r/min stirrings 20min；
2) by obtained by step 1) mixed with Cacl2The pine pyrolysis oil of inorganic salts is (thick sweet with 2060g biological diesel oil byproducts
Oil) mixing, 1000r/min stirrings 30min；
3) mixed system of pine pyrolysis oil and inorganic salts and glycerine is subjected to air-distillation, is 225 DEG C to gas phase temperature
~250 DEG C；
4) the isolated 2396g crude glycerines positioned at cucurbit bottom-lignin thermal decomposition product mixed phase is collected, toward it
Middle incorporation 11980g water, stands 120min；Filtering, obtains remaining the rugose wood element thermal decomposition product and crude glycerine of a small amount of impurity
With the mixing filtrate of water；
5) until constant weight state, this is Biological asphalt at a temperature of gained lignin thermal decomposition product being placed in 100 DEG C；Gained
It is 100 DEG C that the mixing filtrate of crude glycerine and water, which carries out air-distillation to gas phase temperature, and recycling crude glycerine recycles.
A kind of preparation method of 2 Biological asphalt of embodiment
The present embodiment provides a kind of preparation method of Biological asphalt, and difference lies in by embodiment 1 with embodiment 1
Pine pyrolysis oil replaces with poplar pyrolysis oil.
A kind of preparation method of 3 Biological asphalt of embodiment
The present embodiment provides a kind of preparation method of Biological asphalt, and difference lies in by embodiment 1 with embodiment 1
Pine pyrolysis oil replaces with willow pyrolysis oil.
Comparative example
Air-distillation is directly carried out to pine pyrolysis oil to 135 DEG C, obtains lignin thermal decomposition product, then by gained lignin
Until constant weight state, obtains Biological asphalt at a temperature of thermal decomposition product is placed in 100-105 DEG C.
The performance testing experiment method of Biological asphalt and comparative example Biological asphalt obtained by embodiment 1-3 is transported according to traffic
Defeated portion's professional standard highway engineering pitch and Asphalt Mixture Experiment code (JTG-E 20-2011) are measured.
The anti-aging property of Biological asphalt changes over time curve come table with Biological asphalt brookfield viscosity under the conditions of 120 DEG C
Sign.
The Biological asphalt performance data of the embodiment of the present invention 1~3 and comparative example are as shown in table 1, embodiment 1~3 with
The anti-aging property characterization of the Biological asphalt of comparative example is as shown in Figure 1.
The pavement performance of 1 Biological asphalt of table
From the data of table 1,1~3 gained Biological asphalt of the embodiment of the present invention is substantially better than in cryogenic property to be passed through
Biological asphalt that conventional distil-lation process is isolated, thus patent of the present invention is carried out for biomass pyrolysis oil distillation technique
Originality is improved to have a significant effect to improving the hard brittleness of Biological asphalt low temperature.
Fig. 1 reflects the Bu Shi viscositys of 1~3 gained Biological asphalt of comparative example and embodiment at a temperature of 120 DEG C with the time
The relation curve of change.As seen from Figure 1, the present invention is attached to bio oil by being improved to effectively reduce to distillation technique
The cellulose and hemicellulose thermal decomposition product of middle asphalt component, and the crude glycerine introduced is produced as diluent and lignin pyrolysis
Part carboxyl functional group in thing is there occurs esterification, thus the Bu Shi viscositys of 1~3 gained Biological asphalt of embodiment are 120
Versus time curve is substantially than the change curve by Biological asphalt obtained by the isolated comparative example of conventional distil-lation at DEG C
Gently, the Bu Shi viscositys of this explanation 1~3 gained Biological asphalt of embodiment are significantly less than comparative example with the growth rate of time, thus
Had a clear superiority by the ageing resistance of Biological asphalt produced by the present invention.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (9)
1. a kind of preparation method of Biological asphalt, it is characterised in that include the following steps：
1) inorganic salts are mixed in bio oil, mixed；Crude glycerine is added, is mixed；
2) air-distillation is carried out to step 1) products therefrom, isolates light components and including glycerine and lignin thermal decomposition product
Blending ingredients；
3) add water into the blending ingredients, mix, stand, filtering, removes water-glycerol mixed phase therein, obtain rugose wood
Plain thermal decomposition product；
4) the rugose wood element thermal decomposition product is heated to constant weight state, obtains Biological asphalt；By the water-glycerol mixed phase into
Row air-distillation, the glycerine isolated recycle.
2. the preparation method of Biological asphalt according to claim 1, it is characterised in that in step 1), the bio oil is
It is pyrogenically prepared by pine, willow or poplar；
And/or the accessory substance that the crude glycerine is biodiesel.
3. the preparation method of Biological asphalt according to claim 1 or 2, it is characterised in that in step 1), the inorganic salts
For Cacl2, Fecl3Or the one or more in Licl, preferably Cacl2。
4. the preparation method of Biological asphalt according to claim 3, it is characterised in that in step 1), the inorganic salts
Incorporation is the 1~10% of biological oil quality, is preferably 2~4%.
5. the preparation method of the Biological asphalt according to Claims 1 to 4 any one, it is characterised in that in step 1), institute
The mass ratio for stating bio oil and crude glycerine is 1：2~4, preferably 1:2~3.
6. the preparation method of Biological asphalt according to claim 1, it is characterised in that in step 2), the distillation to gas
Phase final temperature is 200 DEG C~250 DEG C, preferably 225 DEG C~250 DEG C.
7. the preparation method of Biological asphalt according to claim 1, it is characterised in that in step 3), the blending ingredients
The mass ratio of water with being added thereto is 1:4~7, preferably 1:4.5~5.5.
8. the preparation method of Biological asphalt according to claim 1, it is characterised in that the preparation method of the Biological asphalt
Include the following steps：
1) by Cacl2With the incorporation of mass percent 2~4% by pine, poplar or the pyrogenically prepared bio oil of willow, mixing；Again
The mass ratio of the accessory substance crude glycerine of addition biodiesel, the bio oil and crude glycerine is 1：2~4, mix；The bio oil
It is pyrogenically prepared by pine, willow or poplar；
2) by step 1) products therefrom air-distillation to gas phase final temperature be 225 DEG C~250 DEG C, isolate light components and including
The blending ingredients of glycerine and lignin thermal decomposition product；
3) with mass ratio 1：4~7 into the blending ingredients plus water, mix, and stand 2~2.5h, filtering, remove water therein-
Glycerine mixed phase, obtains rugose wood element thermal decomposition product；
4) the rugose wood element thermal decomposition product is heated to constant weight state in 100~105 DEG C, obtains Biological asphalt；By the water-
Glycerine mixed phase carries out air-distillation, and the glycerine isolated recycles.
9. Biological asphalt made from any one of claim 1~8 the method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610881684.XA CN107916122A (en) | 2016-10-09 | 2016-10-09 | A kind of Biological asphalt and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610881684.XA CN107916122A (en) | 2016-10-09 | 2016-10-09 | A kind of Biological asphalt and preparation method thereof |
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| CN107916122A true CN107916122A (en) | 2018-04-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518583A (en) * | 2020-04-20 | 2020-08-11 | 华中科技大学 | Solid waste pyrolysis liquid phase product fused salt gradient treatment impurity removal and quality improvement device |
| CN116589868A (en) * | 2023-05-19 | 2023-08-15 | 湖南师范大学 | Biological asphalt and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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2016
- 2016-10-09 CN CN201610881684.XA patent/CN107916122A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| DENG L，YAN Z，FU Y等: ""Green Solvent for Flash Pyrolysis Oil Separation"", 《ENERGY & FUELS》 * |
| QIN-HUA SONG,* JUN-QI NIE, MING-GUANG REN,QING-XIANG GUO: ""Effective Phase Separation of Biomass Pyrolysis Oils by Adding"", 《ENERGY & FUELS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111518583A (en) * | 2020-04-20 | 2020-08-11 | 华中科技大学 | Solid waste pyrolysis liquid phase product fused salt gradient treatment impurity removal and quality improvement device |
| CN111518583B (en) * | 2020-04-20 | 2021-03-05 | 华中科技大学 | Solid waste pyrolysis liquid phase product fused salt gradient treatment impurity removal and quality improvement device |
| CN116589868A (en) * | 2023-05-19 | 2023-08-15 | 湖南师范大学 | Biological asphalt and preparation method and application thereof |
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Application publication date: 20180417 |
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