CN107955382A - A kind of high viscosity modified pitch and preparation method thereof - Google Patents

A kind of high viscosity modified pitch and preparation method thereof Download PDF

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Publication number
CN107955382A
CN107955382A CN201711227788.XA CN201711227788A CN107955382A CN 107955382 A CN107955382 A CN 107955382A CN 201711227788 A CN201711227788 A CN 201711227788A CN 107955382 A CN107955382 A CN 107955382A
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durability
temperature stabilizer
modifying agent
modified pitch
high viscosity
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裴建中
蔡军
任鑫
宋晨
李蕊
张久鹏
温永
刘卧龙
刘涛
罗青辉
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Changan University
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Changan University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Civil Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of high viscosity modified pitch and preparation method thereof, it is 65% 75% matrix pitch by mass percent, 5% 15% high-temperature stabilizer I, 8% 14% durability modifying agent I, 2% 6% durability modifying agent II, 2% 6% low temperature stabilizer, the bulking agent of 0.1% 0.3% high-temperature stabilizer II and 0.1% 0.3% be prepared, the modified pitch coheres ability and high stability, excellent road performance, cost is low, while preparation process is relatively simple.

Description

A kind of high viscosity modified pitch and preparation method thereof
Technical field
The invention belongs to field of road, is related to a kind of high viscosity modified pitch and preparation method thereof.
Background technology
Sponge urban construction is the important points of departure of Urban Construction in China Development Transformation, it is solved to building ecocity Urban waterlogging problem is significant.Sponge city need to from ooze, it is stagnant, store, net, use, row's links consider, plan as a whole to grind Study carefully, and " oozing " is the key link of town road.In order to reach its requirement, scholars propose the concept of porous pavement, and make Standby have the modified pitch cementitious matter that height coheres ability and high-temperature stability to improve the performance of water-permeating pitch mixed material.
With China's expanding economy, the vehicle travelled on road dramatically increases, and axis carries increase;The change of global climate is led The extreme weather for causing the temperature difference larger frequently occurs;And the voidage of water-permeating pitch mixed material is generally 15%-20%, therefore its is easy Intensity and durability is caused to decline by the erosion of load, water, air and sunlight.For China's early stage extensive use and enjoy The TPS modified asphalt mixtures of accreditation, using the result shows that, during road long-time service, porous pavement is mainly shown The shortcomings of high temperature performance is poor, durability is general, and intensity is relatively low.These shortcomings significantly limit porous pavement in the road The scope of application, be generally applicable only in pavement, non-motorized lane and light automotive track.And cause the weight of disadvantages mentioned above Want one of reason be exactly as cementitious matter TMA high temperature performance is poor, endurance quality is general and releases the time more long cannot Meet prevailing traffic conditions, it is therefore desirable to a kind of modified pitch is developed, which coheres ability and high stability, Excellent road performance, cost is low, while preparation process is relatively simple.
The content of the invention
The shortcomings that it is an object of the invention to overcome the above-mentioned prior art, there is provided a kind of high viscosity modified pitch and its system Preparation Method, the modified pitch cohere ability and high stability, and excellent road performance, cost is low, while preparation process is more Simply.
To reach above-mentioned purpose, a kind of high viscosity modified pitch of the present invention is 65%-75%'s by mass percent Matrix pitch, 5%-15% high-temperature stabilizer I, 8%-14% durability modifying agent I, 2%-6% durability modifying agent The low temperature stabilizer of II, 2%-6%, the high-temperature stabilizer II and 0.1%-0.3% of 0.1%-0.3% bulking agent prepare and Into.
Matrix pitch is that the one or more in No. 70 matrix pitches, No. 90 matrix pitches and No. 110 pitches press any ratio The mixture of example mixing.
High-temperature stabilizer I is C5 Petropols, C5/C9 copolymerized petroleum resins, dicyclopentadiene petroleum resin, oxireme The mixture that one or more in base resin, rosin resin and superchlorinated polyvinyl chloride resin mix in any proportion.
High-temperature stabilizer II resists for RA anti-rut agents, road spy LT anti-rut agents, lufu 8000, PR anti-rut agents and Domix The mixture that one or more in rut agent mix in any proportion.
Durability modifying agent I is the mixture of one or both of waste bias tires rubber powder and waste radial tire rubber powder, Wherein, the particle diameter of waste bias tires rubber powder and waste radial tire rubber powder is -100 mesh of 40 mesh.
Durability modifying agent II mixes mixed in any proportion for the one or more in SBS, SIS, IR, CK, SBK and NR Compound.
Bulking agent is one in polyamide-based, polyurethanes, benzoyl peroxide, dithiocar-bamate and sulfur The mixture that kind or both mixes in any proportion.
Low temperature stabilizer is dioctyl phthalate, citroflex A-4, sebacic acid dioctyl ester, O-phthalic The mixing that one or more in dibutyl phthalate, n-butyl stearate and dioctyl adipate copolymer mix in any proportion Thing.
The preparation method of high viscosity modified pitch of the present invention comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch being preheated to 150-165 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, Durability modifying agent I is added after being warming up to 150-190 DEG C again, durability modifying agent II is added after standing, increase-volume is added after standing Agent, is then sheared, and low temperature stabilizer is added after being cooled to 150-165 DEG C, carries out pouring film after stirring, obtains high viscosity modification Pitch.
The concrete operations of step 2) are:Matrix pitch is preheated to 150-165 DEG C, adds high-temperature stabilizer I, stirring makes High-temperature stabilizer I melts, then adds durability modifying agent I after being warming up to 150-190 DEG C, and addition durability changes after standing 20min Property agent II, stand 20min after add bulking agent, then sheared by cutter, wherein, shear rate 3000r/min, Shear time is 30min-50min, develops 20min, and low temperature stabilizer is added after being cooled to 150-165 DEG C, stirs 15- Carry out pouring film after 20min, obtain high viscosity modified pitch.
The invention has the advantages that:
High viscosity modified pitch of the present invention is by matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability Modifying agent II, low temperature stabilizer, high-temperature stabilizer II and bulking agent are prepared, wherein, by mixing high-temperature stabilizer I and low Warm stabilizer, to improve the high-temperature behavior of pitch and cryogenic property, durability modifying agent I and durability modifying agent II are dripped with improving Blue or green resistance to ag(e)ing and cohesiveness, by adding high-temperature stabilizer II, to improve the medium temperature modulus of pitch, increases the glutinous of pitch Degree, high-temperature stability and pavement performance, in addition, when prepared by the present invention, it is only necessary to each raw material is heated, stirred and sheared, High viscosity modified pitch is can obtain, preparation method is relatively simple.The high viscosity modified pitch being prepared through experiment, the present invention Relative to TMA, chronic anti-aging performance has obvious advantage, while viscosity difference is smaller under 175 DEG C and temperatures above, It can preferably meet construction requirement, while recovery compliance at 64 DEG C and stickiness stiffness modulus are higher than TPS modified pitch, can not Recover creep compliance index and be less than TPS modified pitch, high-temperature behavior is more excellent compared with TPS modified pitch;Temperature stability at the same time I.e. storage stability is superior to traditional TMA.
Embodiment
The present invention is described in further detail with reference to embodiment:
Embodiment one
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 65%, 12.6% high-temperature stable Agent I, 14% durability modifying agent I, 2% durability modifying agent II, 6% low temperature stabilizer, 0.1% high-temperature stabilizer The bulking agent of II and 0.3% is prepared.
Matrix pitch is No. 70 matrix pitches.
High-temperature stabilizer I is C5 Petropols.
High-temperature stabilizer II is RA anti-rut agents.
Durability modifying agent I is the waste bias tires rubber powder of 80 mesh.
Durability modifying agent II is SBS.
Bulking agent is the mixture of sulfur.
Low temperature stabilizer is adjacent phenylacetyl group tributyl citrate.
The preparation method of high viscosity modified pitch of the present invention comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 150 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 190 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 30min, development 20min, adds low temperature stabilizer after being cooled to 165 DEG C, carry out pouring film after stirring 15min, obtain high viscosity modified pitch.
The performance of high viscosity modified pitch D-I prepared by embodiment one and TMA progress contrast tests, comparing result such as table 1, Shown in table 2, table 3, table 4 and table 5:
Table 1
As shown in Table 1, after aging 5h, the penetration values of TMA are lower slightly, but softening point and ductility numerical value are still notable Higher than D-I, show that TMA still has best anti-aging property after aging 5h;But after aging 10h, its softening point and ductility Numerical value significantly declines, and shows that the advantage in its comprehensive performance has been not present after aging 10h.
Table 2
For TMA and D-I after aging 5h, test temperature is that less than 165 DEG C of viscosity result rising by a small margin occurs, Declining occurs in viscosity result higher than 165 DEG C;After aging 10h, viscosity has the decline of certain amplitude in whole test scope; The viscosity of the glutinous pitch of height with 180 DEG C its Bu Shi viscosity be advisable no more than 1000mPs, and the present invention can at 175 DEG C Reach requirement, viscosity difference is smaller at the temperature and higher temperature, can preferably meet construction requirement.
Table 3
, should in two kinds of creeps of 0.1kPa and 3.2kPa in experience aging 5h and aging 10h compared with result when unaged Power is horizontal to carry out follow-on test, and the situation of change of recovery rate (R) and irrecoverable compliance (Jnr) from MSCR experiments can Go out:The R indexs of TMA are respectively less than D- I, and Jnr is all higher than D- I, and therefore, compared to TMA, the elasticity of D- I is stronger, and Rut resistance level is higher; In addition, high stress level would generally reduce R indexs and increase Jnr, so as to more be also easy to produce permanent deformation.
Table 4
Table 5
The complex modulus G on TMA tops at -20 DEG C*The about half of lower part, the complex modulus both at 10 DEG C are poor Different G*Just it is gradually reduced;At -20 DEG C, the phase angle δ of TMA modified pitch lower part is about 10 DEG C lower than upper part, but to 30 DEG C When, the phase angle δ of lower part is than upper part but greatly close to 10 DEG C;Two parts complex modulus G above and below 30~80 DEG C of temperature, TMA* Become readily apparent from the difference of phase angle δ.Two parts up and down of D-I test knot at a temperature of -20~30 DEG C and 30~80 DEG C Seemingly, temperature scanning result difference is smaller for fruit, the complex modulus G of top and the bottom*Relatively, phase angle differences smaller, therefore The storage stability of D-I has advantage compared with TMA.
Embodiment two
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 75%, 8.6% high-temperature stable Agent I, 8% durability modifying agent I, 6% durability modifying agent II, 2% low temperature stabilizer, 0.3% high-temperature stabilizer The bulking agent of II and 0.1% is prepared.
Matrix pitch is No. 90 matrix pitches.
High-temperature stabilizer I is dicyclopentadiene petroleum resin.
High-temperature stabilizer II is PR anti-rut agents.
Durability modifying agent I is the waste radial tire rubber powder of 40 mesh.
Durability modifying agent II is SBK.
Bulking agent is polyamide-based.
Low temperature stabilizer is dibutyl phthalate.
The preparation method of high viscosity modified pitch of the present invention comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 165 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 150 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 50min, development 20min, adds low temperature stabilizer after being cooled to 150 DEG C, carry out pouring film after stirring 20min, obtain high viscosity modified pitch D-II.
High viscosity modified pitch D-II and TMA prepared by embodiment two carry out the performance of contrast test for example table 6, table 7, table 8, Shown in table 9 and table 10:
Table 6
As shown in Table 6, after aging 5h, the penetration values of TMA are lower slightly, but softening point and ductility numerical value are still notable Higher than D-II, show that TMA still has best anti-aging property after aging 5h;But after aging 10h is undergone, its softening point and Ductility numerical value significantly declines, and shows that the advantage in its comprehensive performance has been not present after aging 10h is undergone.
Table 7
For TMA and D-II after aging 5h, there is by a small margin upper in viscosity result of the test temperature below 165 DEG C Rise, declining occurs in the viscosity result higher than 165 DEG C, and viscosity has certain amplitude in whole test scope after aging 10h Decline.The viscosity of the glutinous pitch of height with 180 DEG C its Bu Shi viscosity be advisable no more than 1000mPs, and the D- in the present invention II can reach requirement at 175 DEG C, and viscosity difference is smaller at the temperature and higher temperature, can preferably meet that construction will Ask.
Table 8
, should in two kinds of creeps of 0.1kPa and 3.2kPa in experience aging 5h and aging 10h compared with result when unaged Power is horizontal to carry out follow-on test, can be seen in the recovery rate (R) of MSCR experiments and the situation of change of irrecoverable compliance (Jnr) Go out:The R indexs of TMA are respectively less than D-II, and Jnr is all higher than D-II, and therefore, compared to TMA, the elasticity of D- II is stronger, Rut resistance level compared with It is high;In addition, high stress level would generally reduce R indexs and increase Jnr, so as to more be also easy to produce permanent deformation.
Table 9
Table 10
At -20 DEG C, the complex modulus G on TMA tops*The about half of lower part, to the complex modulus G both at 10 DEG C*Difference Exceptional talents are gradually reduced;At -20 DEG C, the phase angle δ of TMA modified pitch lower part is about 10 DEG C lower than upper part, but during to 30 DEG C, The phase angle δ of lower part is than upper part but greatly close to 10 DEG C;Two parts complex modulus G above and below 30~80 DEG C of temperature, TMA*With The difference of phase angle δ becomes readily apparent from.Two parts up and down of D-II result of the test at a temperature of -20~30 DEG C and 30~80 DEG C Similar, temperature scanning result difference is smaller, the complex modulus G of top and the bottom*Relatively, phase angle δ differences smaller, therefore D- The storage stability of II has advantage compared with TMA.
Embodiment three
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 72%, 5% high-temperature stabilizer I, 12.6% durability modifying agent I, 5% durability modifying agent II, 5% low temperature stabilizer, 0.2% high-temperature stabilizer The bulking agent of II and 0.2% is prepared.
Matrix pitch is No. 70 matrix pitches.
High-temperature stabilizer I is rosin resin.
High-temperature stabilizer II is Domix anti-rut agents.
Durability modifying agent I is the waste bias tires rubber powder of 60 mesh.
Durability modifying agent II is SIS.
Bulking agent is benzoyl peroxide.
Low temperature stabilizer is n-butyl stearate.
The preparation method of high viscosity modified pitch of the present invention comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 160 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 170 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 40min, development 20min, adds low temperature stabilizer after being cooled to 160 DEG C, carry out pouring film after stirring 18min, obtain high viscosity modified pitch D- III。
High viscosity modified pitch D-III and TMA prepared by embodiment three carry out the performance of contrast test for example table 11, table 12, Shown in table 13, table 14 and table 15:
Table 11
By table 11, after aging 5h, the penetration values of TMA are lower slightly, but softening point and ductility numerical value are still significantly high In D-III, show that TMA still has best anti-aging property after aging 5h;But after aging 10h is undergone, its softening point and Ductility numerical value significantly declines, and shows that the advantage in its comprehensive performance has been not present after aging 10h is undergone.
Table 12
For TMA and D-III after aging 5h, there is by a small margin upper in viscosity result of the test temperature below 165 DEG C Rise, declining occurs in the viscosity result higher than 165 DEG C, and viscosity has certain amplitude in whole test scope after aging 10h Decline.The viscosity of the glutinous pitch of height with 180 DEG C its Bu Shi viscosity be advisable no more than 1000mPs, and the D- in the present invention III can reach requirement at 175 DEG C, and viscosity difference is smaller at the temperature and higher temperature, can preferably meet that construction will Ask.
Table 13
Compared with result when unaged, in experience aging 5h and aging 10h, in two kinds of creeps of 0.1kPa and 3.2k Pa Stress level carries out follow-on test, and the situation of change of recovery rate (R) and irrecoverable compliance (Jnr) from MSCR experiments can Go out:The R indexs of TMA are respectively less than D-III, and Jnr is all higher than D-III, and therefore, compared to TMA, D-III elasticity is stronger, and Rut resistance is horizontal It is higher;In addition, high stress level would generally reduce R indexs and increase Jnr, so as to more be also easy to produce permanent deformation.
Table 14
Table 15
The complex modulus G on TMA tops at -20 DEG C*The about half of lower part, to the complex modulus G both at 10 DEG C* Difference is just gradually reduced;At -20 DEG C, the phase angle δ of TMA modified pitch lower part is about 10 DEG C lower than upper part, but to 30 DEG C When, the phase angle δ of lower part is than upper part but greatly close to 10 DEG C;Two parts complex modulus G above and below 30~80 DEG C of temperature, TMA* Become readily apparent from the difference of phase angle δ.Two parts up and down of D-III are tested at a temperature of -20~30 DEG C and 30~80 DEG C As a result similar, temperature scanning result difference is smaller, the complex modulus G of top and the bottom*Relatively, phase angle δ differences smaller, Therefore the storage stability of D-III has advantage compared with TMA.
Example IV
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 69.7%, 15% high-temperature stable Agent I, 9% durability modifying agent I, 3% durability modifying agent II, 3% low temperature stabilizer, 0.15% high-temperature stabilizer The bulking agent of II and 0.15% is prepared.
Matrix pitch is No. 110 pitches.
High-temperature stabilizer I is epoxy vingl ester resin.
High-temperature stabilizer II is road spy's LT anti-rut agents.
Durability modifying agent I is the waste radial tire rubber powder of 80 mesh.
Durability modifying agent II is IR.
Bulking agent is polyurethanes.
Low temperature stabilizer is sebacic acid dioctyl ester.
The preparation method of high viscosity modified pitch of the present invention comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 155 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 180 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 45min, development 20min, adds low temperature stabilizer after being cooled to 160 DEG C, carry out pouring film after stirring 16min, obtain high viscosity modified pitch.
High viscosity modified pitch D-IV prepared by example IV and TMA carries out performance such as table 16, table 17, the table of contrast test 18th, shown in table 19 and table 20:
Table 16
As shown in Table 16, after aging 5h, the penetration values of TMA are lower slightly, but softening point and ductility numerical value are still aobvious Work is higher than D-IV, shows that TMA still has best anti-aging property after aging 5h;But after aging 10h is undergone, its softening point Significantly decline with ductility numerical value, show that the advantage in its comprehensive performance has been not present after aging 10h is undergone.
Table 17
For TMA and D-IV after aging 5h, there is rising by a small margin in the viscosity test result less than 165 DEG C, is higher than Declining occurs in 165 DEG C of viscosity result, and viscosity has the decline of certain amplitude in whole test scope after aging 10h. The viscosity of the glutinous pitch of height with 180 DEG C its Bu Shi viscosity be advisable no more than 1000mPs, and the D-IV in the present invention is 175 DEG C when can reach requirement, viscosity difference is smaller at the temperature and higher temperature, can preferably meet construction requirement.
Table 18
Compared with result when unaged, in experience aging 5h and aging 10h, in two kinds of creeps of 0.1k Pa and 3.2k Pa Stress level carries out follow-on test, and the situation of change of recovery rate (R) and irrecoverable compliance (Jnr) from MSCR experiments can Go out:The R indexs of TMA are respectively less than D-IV, and Jnr is all higher than D-IV, and therefore, compared to TMA, the elasticity of D-IV is stronger, and Rut resistance is horizontal It is higher;In addition, high stress level would generally reduce R indexs and increase Jnr, so as to more be also easy to produce permanent deformation.
Table 19
Table 20
At -20 DEG C, the complex modulus G on TMA tops*The about half of lower part, during to 10 DEG C, the complex modulus of the two G*Difference is just gradually reduced;At -20 DEG C, the phase angle δ of TMA modified pitch lower part is about 10 DEG C lower than upper part, but to 30 DEG C When, the phase angle δ of lower part is than upper part but greatly close to 10 DEG C;Two parts complex modulus G above and below 30~80 DEG C of temperature, TMA* Become readily apparent from the difference of phase angle δ.Two parts up and down of D-IV test knot at a temperature of -20~30 DEG C and 30~80 DEG C Seemingly, temperature scanning result difference is smaller for fruit, the complex modulus G of top and the bottom*Relatively, phase angle δ differences smaller, therefore The storage stability of D-IV has advantage compared with TMA.
Embodiment five
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 68.7%, 15% high-temperature stable Agent I, 9% durability modifying agent I, 4% durability modifying agent II, 3% low temperature stabilizer, 0.15% high-temperature stabilizer The bulking agent of II and 0.15% is prepared.
Matrix pitch is No. 110 pitches.
High-temperature stabilizer I is C5/C9 copolymerized petroleum resins.
High-temperature stabilizer II is lufu 8000.
Durability modifying agent I is waste bias tires rubber powder, wherein, the particle diameter of waste bias tires rubber powder is 100 mesh.
Durability modifying agent II is CK.
Bulking agent is dithiocar-bamate.
Low temperature stabilizer is dibutyl phthalate.
The preparation method of the high viscosity modified pitch comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 155 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 160 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 35min, development 20min, adds low temperature stabilizer after being cooled to 160 DEG C, carry out pouring film after stirring 16min, obtain high viscosity modified pitch.
Embodiment six
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 69.7%, 15% high-temperature stable Agent I, 9% durability modifying agent I, 3% durability modifying agent II, 3% low temperature stabilizer, 0.15% high-temperature stabilizer The bulking agent of II and 0.15% is prepared.
Matrix pitch is the mixture that No. 90 matrix pitches and No. 110 pitch mix in any proportion.
High-temperature stabilizer I is superchlorinated polyvinyl chloride resin.
High-temperature stabilizer II is Domix anti-rut agents.
Durability modifying agent I is the mixture of waste bias tires rubber powder and waste radial tire rubber powder, wherein, waste bias tires The particle diameter of rubber powder and waste radial tire rubber powder is 40 mesh.
Durability modifying agent II is NR.
Bulking agent is dithiocar-bamate.
Low temperature stabilizer is dioctyl adipate copolymer.
The preparation method of the high viscosity modified pitch comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 150 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 180 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 45min, development 20min, adds low temperature stabilizer after being cooled to 160 DEG C, carry out pouring film after stirring 16min, obtain high viscosity modified pitch.
Embodiment seven
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 69.7%, 15% high-temperature stable Agent I, 9% durability modifying agent I, 3% durability modifying agent II, 3% low temperature stabilizer, 0.15% high-temperature stabilizer The bulking agent of II and 0.15% is prepared.
The mixture that matrix pitch is No. 70 matrix pitches, No. 90 matrix pitches and No. 110 pitch mix in any proportion.
High-temperature stabilizer I is superchlorinated polyvinyl chloride resin.
High-temperature stabilizer II resists for RA anti-rut agents, road spy LT anti-rut agents, lufu 8000, PR anti-rut agents and Domix The mixture that rut agent mixes in any proportion.
Durability modifying agent I is the mixture of waste bias tires rubber powder and waste radial tire rubber powder, wherein, waste bias tires The particle diameter of rubber powder and waste radial tire rubber powder is 80 mesh.
Durability modifying agent II is NR.
Bulking agent is dithiocar-bamate.
Low temperature stabilizer is dioctyl adipate copolymer.
The preparation method of the high viscosity modified pitch comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 160 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 180 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 45min, development 20min, adds low temperature stabilizer after being cooled to 155 DEG C, carry out pouring film after stirring 18min, obtain high viscosity modified pitch.
Embodiment eight
High viscosity modified pitch of the present invention is by matrix pitch of the mass percent for 69.7%, 15% high-temperature stable Agent I, 9% durability modifying agent I, 3% durability modifying agent II, 3% low temperature stabilizer, 0.15% high-temperature stabilizer The bulking agent of II and 0.15% is prepared.
Matrix pitch is the mixture that No. 90 matrix pitches and No. 110 pitch mix in any proportion.
High-temperature stabilizer I is C5 Petropols, C5/C9 copolymerized petroleum resins, dicyclopentadiene petroleum resin, oxireme The mixture that base resin, rosin resin and superchlorinated polyvinyl chloride resin mix in any proportion.
High-temperature stabilizer II resists for RA anti-rut agents, road spy LT anti-rut agents, lufu 8000, PR anti-rut agents and Domix The mixture that rut agent mixes in any proportion.
Durability modifying agent I is waste bias tires rubber powder, wherein, the particle diameter of waste bias tires rubber powder is 40 mesh.
Durability modifying agent II is the mixture that SBS, SIS, IR, CK, SBK and NR are mixed in any proportion.
Bulking agent is polyamide-based, polyurethanes, benzoyl peroxide, dithiocar-bamate and sulfur by any The mixture of ratio mixing.
Low temperature stabilizer is dioctyl phthalate, citroflex A-4, sebacic acid dioctyl ester, O-phthalic The mixture that dibutyl phthalate, n-butyl stearate and dioctyl adipate copolymer mix in any proportion.
The preparation method of the high viscosity modified pitch comprises the following steps:
1) it is steady that matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high temperature are weighed Determine agent II and low temperature stabilizer;
2) matrix pitch is preheated to 150 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Temperature adds durability modifying agent II after standing 20min, increasing is added after standing 20min to addition durability modifying agent I after 155 DEG C Hold agent, then sheared by cutter, wherein, shear rate 3000r/min, shear time 40min, development 20min, adds low temperature stabilizer after being cooled to 160 DEG C, carry out pouring film after stirring 20min, obtain high viscosity modified pitch.
, wherein it is desired to explanation, high-temperature stabilizer I can also be C5 Petropols, C5/C9 copolymerized petroleum resins, double Several in cyclopentadiene petroleum resin, epoxy vingl ester resin, rosin resin and superchlorinated polyvinyl chloride resin mix in any proportion Mixture;High-temperature stabilizer II can also be RA anti-rut agents, road spy LT anti-rut agents, lufu 8000, PR anti-rut agents And the mixture that Domix anti-rut agents mix in any proportion.Durability modifying agent II is in SBS, SIS, IR, CK, SBK and NR Several mixtures mixed in any proportion.Bulking agent can also be polyamide-based, polyurethanes, benzoyl peroxide, two Several mixtures mixed in any proportion in thiocarbamate and sulfur.

Claims (10)

1. a kind of high viscosity modified pitch, it is characterised in that by matrix pitch, the 5%- that mass percent is 65%-75% Durability modifying agent II, 2%-6%'s of durability modifying agent I, 2%-6% of 15% high-temperature stabilizer I, 8%-14% is low Warm stabilizer, the bulking agent of high-temperature stabilizer II and 0.1%-0.3% of 0.1%-0.3% are prepared.
2. high viscosity modified pitch according to claim 1, it is characterised in that matrix pitch is No. 70 matrix pitches, 90 The mixtures that one or more in number matrix pitch and No. 110 pitches mix in any proportion.
3. high viscosity modified pitch according to claim 1, it is characterised in that high-temperature stabilizer I for C5 Petropols, In C5/C9 copolymerized petroleum resins, dicyclopentadiene petroleum resin, epoxy vingl ester resin, rosin resin and superchlorinated polyvinyl chloride resin The mixtures that mix in any proportion of one or more.
4. high viscosity modified pitch according to claim 1, it is characterised in that high-temperature stabilizer II for RA anti-rut agents, One or more in road spy LT anti-rut agents, lufu 8000, PR anti-rut agents and Domix anti-rut agents mix in any proportion Mixture.
5. high viscosity modified pitch according to claim 1, it is characterised in that durability modifying agent I is waste bias tires The mixture of one or both of rubber powder and waste radial tire rubber powder, wherein, waste bias tires rubber powder and waste radial tire glue The particle diameter of powder is -100 mesh of 40 mesh.
6. high viscosity modified pitch according to claim 1, it is characterised in that durability modifying agent II for SBS, SIS, The mixture that one or more in IR, CK, SBK and NR mix in any proportion.
7. high viscosity modified pitch according to claim 1, it is characterised in that bulking agent for polyamide-based, polyurethanes, The mixture that one or both of benzoyl peroxide, dithiocar-bamate and sulfur mix in any proportion.
8. high viscosity modified pitch according to claim 1, it is characterised in that low temperature stabilizer is pungent for phthalic acid two Ester, citroflex A-4, sebacic acid dioctyl ester, dibutyl phthalate, n-butyl stearate and adipic acid two are pungent The mixture that one or more in ester copolymer mix in any proportion.
9. the preparation method of the high viscosity modified pitch described in a kind of claim 1, it is characterised in that comprise the following steps:
1) matrix pitch, high-temperature stabilizer I, durability modifying agent I, durability modifying agent II, bulking agent, high-temperature stabilizer are weighed II and low temperature stabilizer;
2) matrix pitch is preheated to 150-165 DEG C, adds high-temperature stabilizer I, stirring melts high-temperature stabilizer I, then rises Durability modifying agent I is added after warm to 150-190 DEG C, durability modifying agent II is added after standing, adds bulking agent after standing, so After sheared, low temperature stabilizer is added after being cooled to 150-165 DEG C, carries out pouring film after stirring, obtains high viscosity modified pitch.
10. the preparation method of high viscosity modified pitch according to claim 9, it is characterised in that it is characterized in that, step 2) concrete operations are:Matrix pitch is preheated to 150-165 DEG C, adds high-temperature stabilizer I, stirring makes high-temperature stabilizer I Melt, then durability modifying agent I is added after being warming up to 150-190 DEG C, add durability modifying agent II after standing 20min, stand Bulking agent is added after 20min, is then sheared by cutter, wherein, shear rate 3000r/min, shear time is 30min-50min, develops 20min, and low temperature stabilizer is added after being cooled to 150-165 DEG C, is poured after stirring 15-20min Film, obtains high viscosity modified pitch.
CN201711227788.XA 2017-11-29 2017-11-29 A kind of high viscosity modified pitch and preparation method thereof Pending CN107955382A (en)

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