CN107118575A - Azotized carbon nano piece improves the application of pitch ageing resistace - Google Patents
Azotized carbon nano piece improves the application of pitch ageing resistace Download PDFInfo
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- CN107118575A CN107118575A CN201710245086.8A CN201710245086A CN107118575A CN 107118575 A CN107118575 A CN 107118575A CN 201710245086 A CN201710245086 A CN 201710245086A CN 107118575 A CN107118575 A CN 107118575A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention provides a kind of application of azotized carbon nano piece in pitch ageing resistace is improved, and the preparation method of the azotized carbon nano piece includes：By melamine, urea or dimerization cdicynanmide carry out 550 DEG C~600 DEG C, 4h~5h high temperature thermopolymerizations react, obtain layered nitride toner body, it is added to after ground 200~500 mesh sieve in stabilizer, carries out 2h~4h, centrifugation after 6000r/min~8000r/min high speed shears, dry azotized carbon nano piece.Azotized carbon nano piece and the matrix pitch stirring of melting are mixed to get modified pitch.Compared with prior art, azotized carbon nano piece of the present invention is two-dimension nano materials, and slabbing is melted with pitch, and pitch composite is mutually made using azotized carbon nano sheet material as enhancing, pitch composite material exhibits can be made to go out good ageing resistace.
Description
Technical field
The invention belongs to pavement material field, it is related to modified asphalt material, and in particular to the modification of nitrogen carbon nanosheet
Pitch.
Background technology
Pitch is modified as one of effective measures for improving asphalt material performance using inorganic nano material.It is existing
In technology, the inorganic nano material of researcher's selection mainly has titanium oxide, zinc oxide and calcium carbonate etc..These nano materials grain
Footpath is small, mostly spherical in shape, it is easy to reunite, and is difficult to effectively disperse in pitch, so that the advantage of nano material can not be played.Example
Such as, sword English, Wu Shaopeng, once rotation etc. carry out fusion intercalation by modifying agent of organic layered silicate salt to pitch more than Wuhan University of Technology
It is modified, as a result show the addition of phyllosilicate, improve high temperature complex modulus and Rutting parameter, illustrate that pitch can be improved
High-temperature behavior and rutting resistance, but phyllosilicate is to press from both sides one layer of magnalium oxygen octahedra is constituted 2 by two layers of silicon-oxy tetrahedron:
Silicate mineral of 1 type containing the crystallization water, it is poor with bitumen compatibility due to the characteristic of inorganic material, so in phyllosilicate
Need to carry out organic-treating to it in modified pitch to use, troublesome poeration.Therefore well dispersed nano material is found
It is of great significance applied to having in asphalt material for inorganic nanometer modified pitch.
The content of the invention
In view of the deficienciess of the prior art, a kind of it is an object of the present invention to provide modification of nitrogen carbon nanosheet
Pitch, significantly improves the ageing resistace of pitch.
In order to solve the above-mentioned technical problem, the present invention, which is adopted the following technical scheme that, is achieved：
Application of the azotized carbon nano piece in pitch ageing resistace is improved, the azotized carbon nano piece lamellar spacing is
1.5~3.5nm.The azotized carbon nano piece is obtained by high speed shear layered nitride toner body；The nitridation toner body is stone
Black phase carbon nitride, 25~75 μm of particle diameter.
The preparation method of the azotized carbon nano piece includes：By melamine, urea or dimerization cdicynanmide carry out 550 DEG C~
600 DEG C, the reaction of 4h~5h high temperature thermopolymerizations is added to stabilizer after obtaining layered nitride toner body, ground 200~500 sieve
In, carry out 2h~4h, centrifugation after 6000r/min~8000r/min high speed shears, dry azotized carbon nano piece.
The stabilizer includes isopropanol, methanol, ethanol or dimethyl sulfoxide (DMSO).
The present invention also provides a kind of modified pitch, including matrix pitch and azotized carbon nano piece.
The mass percent of the azotized carbon nano piece and matrix pitch is 5~20：80~95, azotized carbon nano piece and base
The mass percent sum of matter pitch is 100%.
The preparation method of the modified pitch includes：By azotized carbon nano piece in 120 DEG C of temperature~140 DEG C, 3000r/min
Under~5000r/min rotating speeds, 60~120min is mixed with the matrix pitch stirring of melting, modified pitch is obtained.
The present invention compared with prior art, has the following technical effect that：
(1) compared with prior art, azotized carbon nano piece of the present invention is two-dimension nano materials, slabbing and drip
Green grass or young crops melting, is mutually made pitch composite using azotized carbon nano sheet material as enhancing, can go out pitch composite material exhibits good
Good anti-aging characteristic, significantly improves the performance of pitch composite.
(2) present invention uses azotized carbon nano piece, has C-N keys composition, has compatibility well with the organic matter in pitch,
Compared with other inorganic laminated silicate materials, azotized carbon nano piece can be uniformly dispersed in pitch, so as to be more beneficial for nitrogen
Change the raising of carbon nanosheet performance of modified bitumen.
(3) azotized carbon nano piece of the present invention can be made by melamine heat polymerization, with low cost, with higher
Cost performance, while preparation technology is simple, is not required to by other dispersing apparatus, therefore azotized carbon nano piece modified pitch can be used as one
Plant new asphalt pavement material.
Brief description of the drawings
Fig. 1 is azotized carbon nano piece scanning electron micrographs.
Fig. 2 is the transmission electron micrograph of azotized carbon nano piece.
Fig. 3 is complex modulus and temperature relation figure before and after asphalt sample aging.
Fig. 4 is phase angle and temperature relation figure before and after asphalt sample aging.
Explanation is further explained in detail to the particular content of the present invention with reference to embodiments.
Embodiment
Inventor's research finds that nano particle diameter is small, and specific surface area is big so that their own is easy to reunite, in drip
Be difficult to be uniformly dispersed in green grass or young crops, this is the biggest obstacle that current inorganic nano-material modified asphalt runs into, graphite phase carbon nitride be by
The organic polymer of two kinds of element compositions of carbon and nitrogen, it has and interlayer structure as graphite-phase, and interlayer spacing is 0.326nm.
With excellent physical and chemical performance, high heat endurance simultaneously can absorb ultraviolet-visible.In fields such as electricity, optics, catalysis
With widely applying.Lamellar graphite phase carbon nitride can by peel off the C-N keys that be formed in nanometer chip architecture, lamellar structure with
Other polymer have compatibility well.
Specific embodiment of the invention given below, it is necessary to explanation be the invention is not limited in following examples, it is all
The equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
The trade mark of matrix pitch of the present invention is No. 70 bi tumenf orr oads.
Embodiment 1：The present embodiment provides a kind of modified pitch, and preparation method includes：By melamine, 550 DEG C of urea enters
Row high temperature thermopolymerization reacts 4h, is added to after obtaining layered nitride toner body, ground 200 sieve in stabilizer alcohol, progress 2h,
After 6000r/min high speed shears centrifugation, dry azotized carbon nano piece as depicted in figs. 1 and 2, it will be seen from figure 1 that carbonitride
Typical laminated structure is presented；Azotized carbon nano piece is transparent in Fig. 2, and lamellar spacing is in 2nm or so.By 25 grams of azotized carbon nano pieces
In No. 70 heavy-duty road asphalts for being added to 475 grams of meltings, keeping temperature is 140 DEG C, under 3000r/min shear rate at a high speed
60min is stirred, is well mixed it, you can to obtain modified pitch.
According to《Highway engineering pitch and Asphalt Mixture Experiment code》T0610-2011 asphalt rotating thin-film heat runs
Standard prepares test specimen, using dynamic shear rheometer (DSR), determine pitch complex modulus and phase angle with temperature change
Change situation, test result as shown in Figure 3 and Figure 4, short ageing experiment, penetration test, ductility test and the softening point of pitch
Experimental test result is as shown in table 1.
Embodiment 2：
The present embodiment provides a kind of modified pitch, preparation method be the same as Example 1, and difference is, 50 grams of carbonitrides are received
Rice piece is added in No. 70 heavy-duty road asphalts of 450 grams of meltings, and keeping temperature is 120 DEG C, under 5000r/min shear rate
High-speed stirred 70min, is well mixed it, you can to obtain modified pitch.
The present embodiment method of testing is same as Example 1, and test result is as shown in Fig. 3, Fig. 4 and table 1.
Embodiment 3：
The present embodiment provides a kind of modified pitch, preparation method be the same as Example 1, and difference is, 75 grams of carbonitrides are received
Rice piece is added in No. 70 heavy-duty road asphalts of 425 grams of meltings, and keeping temperature is 140 DEG C, under 3000r/min shear rate
High-speed stirred 80min, is well mixed it, you can to obtain modified pitch.
The present embodiment method of testing is same as Example 1, and test result is as shown in Fig. 3, Fig. 4 and table 1.
Embodiment 4：
The present embodiment provides a kind of modified pitch, preparation method be the same as Example 1, and difference is, 100 grams of carbonitrides are received
Rice piece is added in No. 70 heavy-duty road asphalts of 400 grams of meltings, and keeping temperature is 130 DEG C, under 4000r/min shear rate
High-speed stirred 120min, is well mixed it, you can to obtain modified bitumen product.
The present embodiment method of testing is same as Example 1, and test result is as shown in Fig. 3, Fig. 4 and table 1.
Comparative example 1：
This comparative example provides a kind of pitch, for No. 70 matrix pitches of no addition azotized carbon nano piece.This comparative example is surveyed
Method for testing is same as Example 1, and test result is as shown in Fig. 3, Fig. 4 and table 1.
Comparative example 2：
This comparative example provides a kind of pitch, and No. 70 matrix pitches for no addition azotized carbon nano piece rotate by pitch
No. 70 aging matrix pitches that film experiment is obtained.
This comparative example method of testing is same as Example 1, and test result is as shown in Figure 3 and Figure 4.
Effect analysis：
The change at the complex modulus of pitch and phase angle at different temperatures can be characterized using dynamic shear rheometer, when
When aging occurs for pitch, the complex modulus of pitch can become big, and its phase angle can reduce.Fig. 3 and Fig. 4 show：No. 70 matrix pitches
After generation aging, complex modulus numerical value increase, phase angle diminishes, and obvious aging character occurs；And add the nitrogen of different proportion
The complex modulus increasing degree for changing carbon modified pitch diminishes, and the amplitude that phase angle reduces also substantially diminishes, and degree of aging subtracts significantly
It is slow.As a result show the pitch that with the addition of azotized carbon nano piece in ageing process, prevent infiltration of the oxygen in pitch so that pitch
Component keeps relatively stable, so as to also greatly slow down the speed of ageing of asphalt.
Azotized carbon nano piece modified pitch obtained by embodiment 1-4, and the matrix pitch of comparative example 1 are used into Rotational Thin
Film baking oven (RTFO) carry out short ageing experiment, experiment according to《Highway engineering pitch and Asphalt Mixture Experiment code》In
T0610-2011 bars regulation carry out, asphalt penetration test according to《Highway engineering pitch and Asphalt Mixture Experiment code》The
T0604-2011 bars regulation carry out, bitumen ductility experiment according to《Highway engineering pitch and Asphalt Mixture Experiment code》The
T0605-2011 bars regulation carry out, bituminous softening-point test according to《Highway engineering pitch and Asphalt Mixture Experiment code》The
T0606-2011 bars regulation is carried out.Result of the test is as shown in table 1.
Azotized carbon nano piece modified pitch prepared by the present invention of table 1 and performance comparison before and after matrix pitch aging
By table 1 it can be found that matrix pitch and azotized carbon nano piece modified pitch are after short ageing is tested, its pin
In-degree diminishes, and softening point becomes big, and ductility reduces.Compared with matrix pitch aging, the residual pin of azotized carbon nano piece modified pitch
In-degree is enhanced；Softening point rate of change is being gradually reduced；Remain ductility and become big.Remain needle penetration bigger, softening point
Rate of change is smaller, and residual ductility is bigger, and the ageing resistace of pitch is better.Test result indicates that azotized carbon nano piece is added to drip
In green grass or young crops, the ageing resistace of matrix pitch is substantially improved.
Claims (10)
1. azotized carbon nano piece improves the application of pitch ageing resistace.
2. application as claimed in claim 1, it is characterised in that the preparation method of the azotized carbon nano piece includes：By melamine
Amine, urea or dimerization cdicynanmide carry out high temperature thermopolymerization reaction, obtain layered nitride toner body, stabilization is added to after grinding sieving
In agent, centrifugation after high speed shear, dry azotized carbon nano piece are carried out.
3. application as claimed in claim 2, it is characterised in that the high speed shear time is 2h~4h, and speed is 6000r/min
~8000r/min.
4. application as claimed in claim 2, it is characterised in that the reaction temperature of the high temperature thermopolymerization reaction is 550 DEG C~600
DEG C, the reaction time is 4h~5h.
5. application as claimed in claim 2, it is characterised in that described to sieve with 200~500 mesh sieve.
6. application as claimed in claim 2, it is characterised in that it is sub- that the stabilizer includes isopropanol, methanol, ethanol or dimethyl
Sulfone.
7. application as claimed in claim 2, it is characterised in that the nitridation toner body is graphite phase carbon nitride, particle diameter is 25 μm
~75 μm.
8. a kind of modified pitch, it is characterised in that the modified pitch preparing raw material includes matrix pitch and azotized carbon nano piece.
9. modified pitch as claimed in claim 8, it is characterised in that the quality percentage of the azotized carbon nano piece and matrix pitch
Than for 5~20：80~95, the mass percent sum of azotized carbon nano piece and matrix pitch is 100%.
10. modified pitch as claimed in claim 8, it is characterised in that the preparation method of the modified pitch includes：By carbonitride
Nanometer sheet is mixed at 120 DEG C~140 DEG C of temperature, 3000r/min~5000r/min rotating speeds with the matrix pitch stirring of melting
60min~120min, obtains modified pitch.
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| CN201710245086.8A CN107118575B (en) | 2017-04-14 | 2017-04-14 | The application of azotized carbon nano piece raising pitch anti-aging property |
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| CN201710245086.8A CN107118575B (en) | 2017-04-14 | 2017-04-14 | The application of azotized carbon nano piece raising pitch anti-aging property |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108752944A (en) * | 2018-05-22 | 2018-11-06 | 山东交通学院 | A kind of graphite phase carbon nitride modified emulsifying asphalt and its photocatalytic applications |
| CN111218082A (en) * | 2020-02-28 | 2020-06-02 | 江苏凯信环保材料有限公司 | Carbon-based composite anti-aging modifier suitable for asphalt and preparation method thereof |
| CN112047311A (en) * | 2020-09-09 | 2020-12-08 | 天津工业大学 | Stripping method of graphite phase carbon nitride |
| CN115394888A (en) * | 2022-06-13 | 2022-11-25 | 武汉中科先进材料科技有限公司 | Blue-violet light carbon nitride nanosheet, preparation method thereof and blue-violet light LED device |
| CN115710432A (en) * | 2022-12-15 | 2023-02-24 | 中路交科科技股份有限公司 | Hydrophobic durable high-viscosity modified asphalt and preparation method thereof |
| CN115710432B (en) * | 2022-12-15 | 2024-04-19 | 中路交科科技股份有限公司 | Hydrophobic durable high-viscosity modified asphalt and preparation method thereof |
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| CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
| CN106496701A (en) * | 2016-12-20 | 2017-03-15 | 佛山市高明区塑料行业协会 | A kind of modified abrasion resistant high impact-resistant butadiene-styrene rubber |
| CN106542509A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of efficient method for preparing class Graphene carbonitride |
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2017
- 2017-04-14 CN CN201710245086.8A patent/CN107118575B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104401948A (en) * | 2014-11-17 | 2015-03-11 | 长安大学 | Preparation method for single-layer graphite-type carbon nitride nanosheet solution |
| CN106542509A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of efficient method for preparing class Graphene carbonitride |
| CN106496701A (en) * | 2016-12-20 | 2017-03-15 | 佛山市高明区塑料行业协会 | A kind of modified abrasion resistant high impact-resistant butadiene-styrene rubber |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108752944A (en) * | 2018-05-22 | 2018-11-06 | 山东交通学院 | A kind of graphite phase carbon nitride modified emulsifying asphalt and its photocatalytic applications |
| CN111218082A (en) * | 2020-02-28 | 2020-06-02 | 江苏凯信环保材料有限公司 | Carbon-based composite anti-aging modifier suitable for asphalt and preparation method thereof |
| CN112047311A (en) * | 2020-09-09 | 2020-12-08 | 天津工业大学 | Stripping method of graphite phase carbon nitride |
| CN115394888A (en) * | 2022-06-13 | 2022-11-25 | 武汉中科先进材料科技有限公司 | Blue-violet light carbon nitride nanosheet, preparation method thereof and blue-violet light LED device |
| CN115394888B (en) * | 2022-06-13 | 2024-02-09 | 武汉中科先进材料科技有限公司 | Blue-violet light carbon nitride nanosheet, preparation method thereof and blue-violet light LED device |
| CN115710432A (en) * | 2022-12-15 | 2023-02-24 | 中路交科科技股份有限公司 | Hydrophobic durable high-viscosity modified asphalt and preparation method thereof |
| CN115710432B (en) * | 2022-12-15 | 2024-04-19 | 中路交科科技股份有限公司 | Hydrophobic durable high-viscosity modified asphalt and preparation method thereof |
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