CN106675049A - Method for preparing tetrahydrofuran soluble substance-modified asphalt in direct coal liquefaction residues - Google Patents
Method for preparing tetrahydrofuran soluble substance-modified asphalt in direct coal liquefaction residues Download PDFInfo
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- CN106675049A CN106675049A CN201610894152.XA CN201610894152A CN106675049A CN 106675049 A CN106675049 A CN 106675049A CN 201610894152 A CN201610894152 A CN 201610894152A CN 106675049 A CN106675049 A CN 106675049A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to a method for preparing tetrahydrofuran soluble (THFS) substance-modified asphalt in direct coal liquefaction residues (DCLR). The method comprises the following steps: 1) detecting each performance of THFS AND matrix asphalt in DCLR; 2) detecting an orthogonal test scheme in three factors and three levels, 3) using a penetration grading system to determining the preparation technology of THFS asphalt; 4) determining the preparation technology of the THFS-modified asphalt by a grey relational analysis method; 5) comparing the penetration grading system and the grey relational analysis, and determining the optimum preparation technology of the THFS-modified asphalt; 6) preparing the modified asphalt under different THFS doping amounts according to the optimum preparation technology of the THFS-modified asphalt; and 7) by using the penetration grading system and a SHRP PG grading system to evaluate each performance of the THFS-modified asphalt, and determining the optimum doping amount of THFS. The method is characterized in that DCLR is extracted as a modifier, and then is added into the asphalt, which overcome the defect in the prior art, and the invention also provides the improved preparation method for the THFS-modified asphalt in DCLR, and the added value of the DCLR is increased.
Description
Technical field
The present invention relates to pavement construction material preparing technical field, more particularly to using coal directly-liquefied residue (Direct
Coal Liquefaction Residue, DCLR) in tetrahydrofuran DDGS (tetrahydrofuran soluble,
THFS) come prepare modified pitch with and preparation method thereof field.
Background technology
DCLR is that the accessory substance produced in direct coal liquefaction process accounts for feed coal total amount 30%, its be a kind of high ash,
The material of high-sulfur, high charcoal and golf calorific value, by asphaltene, preasphaltene, 4 component groups of mink cell focus and tetrahydrofuran insoluble
Into wherein mink cell focus and pitch alkenes material account for 30~50%
From the seventies, people just set about studying impacts of the DCLR as modifying agent to asphalt performance.
King stockaded village rosy clouds are mixed with different types of DCLR different proportions, are found with the increase of DCLR content of modifier, are modified
The softening point of pitch gradually rises, and needle penetration and ductility are decreased obviously, when finding to add 7%DCLR in pitch, modified pitch
Correlated performance meet the rank of 40-55 needle penetrations in U.S.'s ASTM D5710-95 standards, it is proposed that DCLR can be used as a kind of drip
Blue or green modifying agent is used.
Zhu Weiping DCLR have studied volume, compounding process and the compounding temperature of DCLR to pitch as asphalt modifier
The impact of performance.
He Liang is tested the needle penetration of the adulteration modified pitches of different DCLR, softening point and ductility, is as a result shown, its property
Can close 5%SBS modified pitch.With the increase of DCLR volumes, the viscosity of modified pitch is in rising trend.
Zhang Yanrong inquires into the factors such as modification temperature, modification time, DCLR volumes and adding mode to performance of modified bitumen
Affect, find, when DCLR volumes are 5%, the standard of No. 50 pitch can be met.
Season is studied DCLR with the performance of bitumen blend, it is found that DCLR has very well to the high-temperature behavior of pitch
Improvement result, but the cryogenic property and fatigue behaviour to pitch has damage.
In terms of the recycling of DCLR, it has been recognized that the asphaltogenic modifying agent of its secondary development, mesophase can be dripped
Green grass or young crops etc., but the tetrahydrofuran insoluble in DCLR has a strong impact on the cryogenic property of modified pitch.
A kind of method for preparing modified pitch of the disclosure of the invention of Application No. 201110393394.8, it is characterised in that
Room temperature in the range of 100 DEG C, with the organic solvent that the ability of dispersing or dissolving is respectively provided with to coal liquefaction heavy product and matrix pitch
And/or mixed solvent oil, coal liquefaction heavy product and matrix pitch mixing are made, it is then peeled off, recycling design, you can be modified
Pitch, it is 5-50% that the addition of wherein coal liquefaction heavy product accounts for the percentage by weight of modified pitch.The invention has preparation
Temperature is low, the good advantage of performance of modified bitumen.
A kind of road asphalt modifier of the disclosure of the invention of application number 200610012547.9 is coal directly-liquefied residue, its
Consist of:Tetrahydrofuran insoluble content is 10-50wt%, and tetrahydrofuran is solvable-and toluene insolubles content is 0-40wt%, four
Hydrogen furans is solvable-and xylene solubles content is 20-60wt%.The application process of road asphalt modifier is that DCL/Direct coal liquefaction is residual
Ground-slag is broken to below 100 mesh, with pitch 100-250 DEG C of scope by coal directly-liquefied residue account for modified pitch weight ratio be 5-
30% is well mixed.The invention enables that coal directly-liquefied residue is simple, Optimum utilization, can effectively improve DCL/Direct coal liquefaction process
Economy.A kind of new, cheap road asphalt modifier is generated simultaneously.
Tetrahydrofuran insoluble has a strong impact on to modified pitch cryogenic property in order to overcome prior art, and the present invention will
DCLR is extracted, and extracts THFS, and is added in pitch as modifying agent.Research to DCLR modified pitch at present
Also in the experimental study stage, without a kind of perfect preparation method.Therefore, the invention provides THFS is modified in a kind of DCLR
The perfect preparation method of pitch, to improve the added value of DCLR.
The content of the invention
The invention provides a kind of coal directly-liquefied residue (direct coal liquefaction residue, DCLR)
The method that middle tetrahydrofuran DDGS (tetrahydrofuran soluble, THFS) prepares modified pitch, including following step
Suddenly：
Step one：THFS, the properties of matrix pitch in test DCLR；
Step 2：Determine orthogonal test scheme；
Step 3：Determine the preparation technology of THFS pitches using needle penetration staging hierarchy；
Step 4：The preparation technology of THFS modified pitch is determined according to grey relation analysis method；
Step 5：The preparation technology of the THFS modified pitch that step 3 and step 4 are determined is contrasted, and determines THFS
The optimal preparation technology of modified pitch；
Step 6：Modified pitch under difference THFS volumes is prepared according to the optimal preparation technology of THFS modified pitch；
Step 7：The properties of THFS modified pitch are evaluated, THFS the optimum mix amounts are determined.
The step 3 and step 4 are in no particular order sequentially.
Such scheme is preferably, and in step one, the TFHS is the extract of DCLR.
In any of the above-described scheme preferably, in step 2, the orthogonal test is Three factors-levels orthogonal test.Adopt
With the orthogonal experiment of Three factors-levels, a kind of preparation method of THFS modified pitch in DCLR is determined.
In any of the above-described scheme preferably, three factor is shear temperature, shear time, shear rate.Shearing temperature
Degree, shear time, shear rate are to affect the most important factor of THFS performance of modified bitumen.
In any of the above-described scheme preferably, three levels of the shear temperature are 150 DEG C, 160 DEG C, 170 DEG C.From temperature
Degree is less than 150 DEG C, the excessively sticky operation for being unfavorable for testing of THFS modified pitch；Temperature is easily aging higher than 170 DEG C of pitches.
In any of the above-described scheme preferably, three levels of the shear time are 30min, 45min, 60min.From
The shear time of 30min, 45min, 60min is because that shear time is too short causes THFS modified pitch uneven, shear time
More than the poor-performing that 60min causes THFS modified pitch, thus from 30min, 45min, 60min shear time as examination
Three levels tested.
In any of the above-described scheme preferably, three levels of the shear rate be 2000r/min, 4000r/min,
6000r/min。
In any of the above-described scheme preferably, using needle penetration staging hierarchy, the preparation technology of THFS modified pitch is determined.
In any of the above-described scheme preferably, according to grey relation analysis method, the preparation technology of THFS modified pitch is determined.
In any of the above-described scheme preferably, the utilization needle penetration staging hierarchy determines the preparation work of THFS modified pitch
In the step of skill, 10 DEG C of ductilities of THFS modified pitch are tested.
In any of the above-described scheme preferably, the utilization needle penetration staging hierarchy determines the preparation work of THFS modified pitch
In the step of skill, 25 DEG C of needle penetrations of THFS modified pitch are tested.
In any of the above-described scheme preferably, the utilization needle penetration staging hierarchy determines the preparation work of THFS modified pitch
In the step of skill, the softening point of THFS modified pitch is tested.
In any of the above-described scheme preferably, the utilization needle penetration staging hierarchy determines the preparation work of THFS modified pitch
In the step of skill, 135 DEG C of brookfield viscosities of THFS modified pitch are tested.
In any of the above-described scheme preferably, the utilization needle penetration staging hierarchy determines the preparation work of THFS modified pitch
In the step of skill, penetration index PI is calculated.
In any of the above-described scheme preferably, shear temperature 150- in the optimal preparation technology of the THFS modified pitch
160℃
In any of the above-described scheme preferably, shear time 30- in the optimal preparation technology of the THFS modified pitch
60min
In any of the above-described scheme preferably, the optimal preparation technology medium shear rate 2000- of the THFS modified pitch
4000r/min。
In any of the above-described scheme preferably, in step 6, THFS volumes are added to be 4-10% in matrix pitch.
In the range of 4-10%, choose several volumes, such as 4%, 6%, 8%, 10% etc. THFS be added separately to base
In matter pitch, shearing is uniform, prepares several THFS modified pitch, tests the technical indicator of above-mentioned THFS modified pitch, it is ensured that its
Technical indicator meets《Standard specification for construction and acceptance of highway asphalt pavement》It is comprehensive about the technical standard of pitch in (JTG F40-2004)
Properties, determine the optimum mix amount of THFS.
In any of the above-described scheme preferably, in step 6, the heating-up temperature of matrix pitch is 110-130 DEG C.The temperature
Under degree, matrix pitch can be completely melt, and uniformly, good fluidity.
In any of the above-described scheme preferably, in step 6, the heating-up temperature of THFS is 150-160 DEG C.At this temperature,
THFS can melt completely, and uniformly.
In any of the above-described scheme preferably, in step 6, matrix pitch is 150-160 with the shear temperature of THFS
℃.At this temperature, matrix pitch can be sufficiently mixed with THFS, and be well mixed.
In any of the above-described scheme preferably, in step 6, matrix pitch is 0.5-1h with the shear time of THFS.Should
In time, matrix pitch can be sufficiently mixed with THFS, and be well mixed.
In any of the above-described scheme preferably, in step 6, matrix pitch is 2000- with the shear rate of THFS
4000r/min.Under the speed, matrix pitch can be sufficiently mixed with THFS, and be well mixed.
In any of the above-described scheme preferably, step 7 is to be commented using needle penetration staging hierarchy and SHRP PG staging hierarchies
The properties of valency THFS modified pitch, determine THFS the optimum mix amounts.
In any of the above-described scheme preferably, in step 7, the optimum mix amount of THFS is 4-6%.
The present invention adopts the orthogonal experiment of Three factors-levels, it is determined that the preparation of THFS modified pitch in a kind of DCLR
Method.
Grey correlation analysis are a kind of new factor approach, and it is all to investigate system to system dynamic course quantitative analysis
Degree of correlation between factor, is a kind of analysis method of fixed guantity combining with fixed quality, its basic skills be according to things or because
The similarity degree of the sequence curve of element is judging its correlation degree.
Needle penetration classification performance appraisement system, is to determine the weather conditions that pitch is adapted to according to the size of Asphalt Penetration
And load-up condition.The main body of needle penetration classification performance appraisement system is ductility, needle penetration, softening point, is aided with the security of pitch
Energy index flash-point, the purity index solubility of pitch, ageing resistace index Thin Film Oven Test TFOT of pitch etc., constitute pitch
Needle penetration classification performance system.
SHRP PG classification performance appraisement systems, are U.S. SHRP (Strategic Highway Research
Program) pavement performance grade scale is planned, it is desirable to which cementitious matter meets at different temperatures same performance requirement, is according to drip
Method of the temperature on blue or green road surface to select pitch.
DSR is tested, i.e. DSR test, for determining the viscoplasticity of pitch.Pitch as viscoelastic material, it
There is the characteristic of elastomeric material and the characteristic of cohesive material simultaneously, the relation between both characteristics is used to evaluate cementitious matter
Permanent deformation resistance and antifatigue cracking ability.For Rut resistance, cementitious matter needs hard and flexible；Open in order to antifatigue
Split, cementitious matter needs flexible and viscosity.Balance between the elasticity of pitch and viscosity is very important.
BBR is tested, i.e. bent beam rheological test, for determining stiffness of the pitch girder test specimen under creep loading effect.
The technical indicator of matrix pitch should meet《Standard specification for construction and acceptance of highway asphalt pavement》Have in (JTG F40-2004)
Close the technical standard of pitch.
The performance of THFS modified pitch is influenced by many factors, such as shear temperature, shear time, shear rate, examination
The factors such as the selection of instrument are tested, wherein shear temperature, shear time, shear rate is three factors for playing a decisive role.This
Invention adopts Three factors-levels orthogonal experiment design method, by test the ductility of its pitch, needle penetration, softening point test,
The analysis shear temperature such as kinematic viscosity, shear time, the factor of shear rate three are under varying level to THFS performance of modified bitumen
Impact, and then determine affect asphalt performance key factor and level.Orthogonal test is with efficiency high, speed is fast, cost
Low test design method.Using Three factors-levels Orthogonal Experiment and Design, test according to orthogonal arrage arrangement, only need to do nine examinations
Test, can so greatly reduce workload, and be able to ensure that the accuracy of result of the test, while can be from nine tests
Find the optimum matching relation of three factors and three levels.
Present invention also offers THFS modified pitch in a kind of DCLR, using coal directly-liquefied residue composition and matrix pitch
Prepare, the modified pitch is prepared by the method for any of the above-described.
In any of the above-described scheme preferably, the extract THFS of the DCLR.
The invention has the beneficial effects as follows：The preparation method of THFS modified pitch in a kind of DCLR of the present invention, to improving DCLR
Added value and its secondary reasonable development is significant into asphalt modifier, therefore, preparation method Jing of the present invention
Ji is practical, simple, easily operate, the low, low cost that consumes energy, beneficial to environmental protection.
Description of the drawings
Fig. 1 is the preferred of the preparation method of tetrahydrofuran DDGS modified pitch in a kind of coal directly-liquefied residue of the invention
In the step of determining the preparation technology of THFS modified pitch using needle penetration staging hierarchy in embodiment 5 indexs and value with because
The change curve of element and level, Fig. 1 a be in the preferred embodiment of the present invention 25 DEG C of needle penetration and value with factor and level change
Change curve map, Fig. 1 b be in the preferred embodiment 10 DEG C of ductilities and value with factor and the change curve of level, Fig. 1 c are this
In invention preferred embodiment softening point and value with factor and the change curve of level, Fig. 1 d are in the preferred embodiment of the present invention
Brookfield viscosity and value with factor and the change curve of level, Fig. 1 e be in the preferred embodiment of the present invention PI values and be worth with because
The change curve of element and level.
Specific embodiment
Below in conjunction with instantiation, the present invention will be further described, but present disclosure be not limited solely to it is following
Embodiment.
Embodiment
DCLR, from the by-product of China Shenhua Coal to Liquid and Chemical Co., Ltd.'s Inner Mongol production, is powder.Using Soxhlet
Extractor is extracted using tetrahydrofuran solvent to DCLR, obtains THFS.According to《Highway engineering pitch and asphalt are tried
Test code》Relevant regulations in (JTG E20-2011) are tested THFS performances, are shown in Table 1.
The technical indicator of the THFS of table 1
Matrix pitch adopts Korea's import SK-90 pitches, according to《Highway engineering pitch and Asphalt Mixture Experiment code》
Relevant regulations in (JTG E20-2011) have carried out performance test to it, are shown in Table 2, and the PG of wherein SK-90 pitches is classified as 58-
22。
The performance of the SK-90 pitches of table 2
The performance of SK-90 pitches meets《Standard specification for construction and acceptance of highway asphalt pavement》It is relevant No. 90 in (JTG F40-2004)
The technical standard of pitch.
The orthogonal test of Three factors-levels is determined herein, and table 3 is three factors and its three levels in orthogonal test, orthogonal
Testing program is shown in Table 4.
The Three factors-levels table of table 3
The orthogonal test scheme of table 4
The THFS modified pitch under 9 groups of Different Preparations is prepared according to table 4, according to《Highway engineering pitch and pitch are mixed
Close material testing regulations》Relevant regulations in (JTG E20-2011) carry out needle penetration, ductility, softening point, 135 DEG C of Bu Shi to it and glue
The test of degree and the calculating of penetration index PI, calculate respectively above-mentioned 5 indexs and value and extreme difference, it is shown in Table 5 and Fig. 1.
The range analysis table of table 5
As can be seen from Table 5, the master of THFS modified pitch is affected by wanting influence factor to be shear time, next to that shearing temperature
Degree, is finally shear rate.
As shown in Figure 1：
(1) knowable to Fig. 1 (a), with the increase of shear time, the needle penetration of pitch first increases and declines afterwards, when shearing temperature
Spend for 60min when, needle penetration is minimum, and asphalt high-temperature stability is optimum.Shear temperature is secondary cause, with shear temperature
Raise, the needle penetration of pitch is on a declining curve, when shear temperature is higher than 160 DEG C, the reduction amplitude of Asphalt Penetration and value subtracts
It is little.
(2) from Fig. 1 (b), with the increase of shear temperature, its ductility and value are being gradually reduced, it is seen that shear temperature
Increase, making the cryogenic property of DCLR modified pitch reduces.With the increase of shear time, ductility and value straight line are reduced；With
The increase of shear time, the cryogenic property for making DCLR modified pitch drastically declines；With the increase of shear rate, the modified drips of DCLR
Blue or green ductility is also what is be gradually reduced, but rate of change slows down, and illustrates that rotating speed 2000r/min and 4000r/min are direct to coal
The cryogenic property of liquefied residue modified pitch affects larger.
(3) from Fig. 1 (c), with the increase of shear time and shear temperature, asphalt softening point is dramatically increased, and is shown
The high-temperature behavior of pitch is improved.Increase with shear rate, the softening point first increases and then decreases of pitch, when shear rate is
During 4000r/min, the softening point of pitch is maximum, and when illustrating 4000r/min, its high-temperature stability is optimal.
(4) from Fig. 1 (d), asphalt viscosity after first dramatically increasing and is strongly reduced with the increase of shear time, when cutting
Cut the time for 45min when, asphalt viscosity reaches maximum, illustrates that its high-temperature behavior is most strong.Asphalt viscosity with shear temperature liter
Height, linearly increases.
(5) from Fig. 1 (e), pitch PI first reduces increasing afterwards with the increase of shear time, with the increase of shear rate,
Pitch PI first increases and then decreases, when shear time be 60min, shear rate be 4000r/min when, pitch PI reaches maximum, says
Bright its temperature sensitivity is minimum.
Impact and value of the comprehensive each factor to asphalt performance changes with extreme difference, and the preparation technology for determining THFS modified pitch is
A2B2C2。
According to the calculation procedure of Grey Incidence Analysis, above-mentioned 5 indexs are calculated in THFS modified pitch preparation technologies
Middle proportion, and comprehensive grading is carried out to it, it is shown in Table 6.
The grey correlation analysis of table 6
As shown in Table 6：5 indexs differ to the weighing factor of THFS performance of modified bitumen, and primary and secondary order respectively softens
Point>Ductility>135 DEG C of brookfield viscosities>Needle penetration>PI.According to comprehensive grading, 2 highest scorings are combined, illustrate the THFS under the combination
The best performance of modified pitch is got over.Therefore, the THFS modified pitch preparation technology for being determined by grey correlation analysis is A1B2C2。
Two kinds of THFS modified pitch preparation technologies that above-mentioned employing orthogonal test and grey relation analysis method determine are carried out
Contrast, so as to the optimal preparation technology of optimization design THFS modified pitch, is shown in Table 7.
The performance comparison of the Different Preparation THFS modified pitch of table 7
As known from Table 7, THFS modified pitch high-temperature behaviors (needle penetration, softening point, viscosity), the cryogenic property of technique two
(ductility) and temperature-sensitive performance (PI) are superior to technique one, illustrate that using technique two the more excellent THFS of performance can be prepared
Modified pitch, is (the A of technique two so as to optimize the optimal preparation technology for determining THFS modified pitch1B2C2), i.e., shear temperature is
150 DEG C, shear time is 45min, and shear rate is 4000r/min.
Optimal preparation technology according to above-mentioned determination prepares THFS modified pitch：
(1) matrix pitch is heated into 120-130 DEG C；
(2) THFS is heated into 150-160 DEG C；
(3) in mass ratio it is respectively 4 by the THFS of molten condition and matrix pitch：100,6：100,8：100,10：100 enter
Row blending, in order to ensure the uniformity of THFS modified pitch, adopt boxshear apparatus by THFS modified pitch at 150 DEG C with 4000r/
Min low velocity shear 45min.
According to《Highway engineering pitch and Asphalt Mixture Experiment code》Relevant regulations in (JTG E20-2011), according to
SHRPPG and needle penetration staging hierarchy carry out performance test to modified pitch under different THFS volumes respectively, are shown in Table 8.
The performance of modified pitch under the difference THFS volumes of table 8
As shown in Table 8：
(1) addition of THFS and being continuously increased with THFS volumes, modified pitch high-temperature behavior is become better and better and (is softened
The raising of point, viscosity), but cryogenic property is worse and worse (reduction of 10 DEG C of ductilities), it means that and pitch is with THFS volumes
Increase and be constantly hardened, become fragile.When THFS volumes are more than 6%, the cryogenic property of THFS modified pitch can not meet《Highway
Asphalt Pavement Construction Technique specification》To the requirement of 10 DEG C of ductilities (>=10cm) of No. 50 pitch in (JTG F40-2004).
(2) THFS addition and being continuously increased with THFS volumes, THFS modified pitch compared with matrix pitch, its PG
High thermal level is constantly declining in continuous improvement, but PG low-temperature grades, and this point keeps with the result of the test of needle penetration appraisement system
Unanimously.When THFS volumes are more than 6%, the low-temperature grade of THFS modified pitch have dropped 1 grade.
(3) the high and low temperature performance of synthesis THFS modified pitch, recommends THFS the optimum mix amounts to be 4-6%.
It will be apparent to those skilled in the art that the preparation method of THFS modified pitch is including upper in a kind of DCLR of the present invention
The content of the invention of description of the invention and any combination of specific embodiment part are stated, as space is limited and to make specification simple and clear
Do not have the scheme for constituting these combinations to describe one by one.All any modifications within the spirit and principles in the present invention, made, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of coal directly-liquefied residue（Direct coal liquefaction residue, DCLR）Middle tetrahydrofuran is solvable
Thing（Tetrahydrofuran soluble, THFS）The method for preparing modified pitch, comprises the steps：
Step one：The properties of THFS and matrix pitch in test DCLR；
Step 2：Determine orthogonal test scheme；
Step 3：Determine the preparation technology of THFS pitches using needle penetration staging hierarchy；
Step 4：The preparation technology of THFS modified pitch is determined according to grey relation analysis method；
Step 5：The preparation technology of the THFS modified pitch that step 3 and step 4 are determined is contrasted, and determines that THFS is modified
The optimal preparation technology of pitch；
Step 6：Modified pitch under difference THFS volumes is prepared according to the optimal preparation technology of THFS modified pitch；
Step 7：The properties of THFS modified pitch are evaluated, THFS the optimum mix amounts are determined；
The step 3 and step 4 are in no particular order sequentially.
2. in a kind of DCLR as claimed in claim 1 THFS modified pitch preparation method, it is characterised in that：In step one,
The TFHS is the extract of DCLR.
3. in a kind of DCLR as claimed in claim 1 THFS modified pitch preparation method, it is characterised in that：In step 2,
The orthogonal test is Three factors-levels orthogonal test.
4. in a kind of DCLR as claimed in claim 3 THFS modified pitch preparation method, it is characterised in that：Three factor
For shear temperature, shear time and shear rate.
5. in a kind of DCLR as claimed in claim 4 THFS modified pitch preparation method, it is characterised in that：The shearing temperature
Three levels of degree are 150 DEG C, 160 DEG C and 170 DEG C.
6. in a kind of DCLR as claimed in claim 4 THFS modified pitch preparation method, it is characterised in that：During the shearing
Between three levels be 30min, 45min and 60min.
7. in a kind of DCLR as claimed in claim 4 THFS modified pitch preparation method, it is characterised in that：The shearing speed
Three levels of rate are 2000r/min, 4000r/min and 6000r/min.
8. in a kind of DCLR as claimed in claim 1 THFS modified pitch preparation method, it is characterised in that：The utilization pin
In the step of in-degree staging hierarchy determines the preparation technology of THFS modified pitch, 10 DEG C of ductilities of THFS modified pitch are tested.
9. in a kind of DCLR as claimed in claim 1 THFS modified pitch preparation method, it is characterised in that：The utilization pin
In the step of in-degree staging hierarchy determines the preparation technology of THFS modified pitch, 25 DEG C of needle penetrations of THFS modified pitch are tested.
10. THFS modified pitch in a kind of DCLR, is prepared using coal directly-liquefied residue composition and matrix pitch, its feature
Be the modified pitch be to be prepared by the method for any one of claim 1-25.
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|---|---|---|---|---|
| CN108613945A (en) * | 2018-04-10 | 2018-10-02 | 北京建筑大学 | A method of based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property |
| CN109142148A (en) * | 2018-07-27 | 2019-01-04 | 北京建筑大学 | A method of based on CAM model analysis THFS modified pitch temperature-sensitive performance |
| CN112415180A (en) * | 2020-12-10 | 2021-02-26 | 广西交科集团有限公司 | Method for selecting base asphalt for rubber asphalt based on ash correlation analysis |
| CN112666105A (en) * | 2020-12-04 | 2021-04-16 | 武汉科技大学 | Asphalt high-temperature performance detection method based on gray entropy correlation |
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- 2016-10-13 CN CN201610894152.XA patent/CN106675049A/en active Pending
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| 季节 等: "THFS 改性沥青制备工艺的优化设计及性能评价", 《北京建筑大学学报》 * |
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| CN108613945A (en) * | 2018-04-10 | 2018-10-02 | 北京建筑大学 | A method of based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property |
| CN109142148A (en) * | 2018-07-27 | 2019-01-04 | 北京建筑大学 | A method of based on CAM model analysis THFS modified pitch temperature-sensitive performance |
| CN112666105A (en) * | 2020-12-04 | 2021-04-16 | 武汉科技大学 | Asphalt high-temperature performance detection method based on gray entropy correlation |
| CN112415180A (en) * | 2020-12-10 | 2021-02-26 | 广西交科集团有限公司 | Method for selecting base asphalt for rubber asphalt based on ash correlation analysis |
| CN112415180B (en) * | 2020-12-10 | 2021-09-10 | 广西交科集团有限公司 | Method for selecting base asphalt for rubber asphalt based on ash correlation analysis |
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