CN108059840A - A kind of modified pitch and preparation method thereof - Google Patents
A kind of modified pitch and preparation method thereof Download PDFInfo
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- CN108059840A CN108059840A CN201610983418.8A CN201610983418A CN108059840A CN 108059840 A CN108059840 A CN 108059840A CN 201610983418 A CN201610983418 A CN 201610983418A CN 108059840 A CN108059840 A CN 108059840A
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- molecular sieve
- mesopore molecular
- pitch
- modified pitch
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
- C08K5/372—Sulfides, e.g. R-(S)x-R'
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
Abstract
The invention discloses a kind of modified pitch and preparation method thereof.The modified pitch includes following raw material components by weight：100 parts of matrix pitch；0.1~1 part of surface modification mesopore molecular sieve；0.1~1 part of antioxidant；Wherein, the surface modification mesopore molecular sieve is the mesopore molecular sieve that hydrosulphonyl silane is modified.The present invention is using the mesopore molecular sieve using hydrosulphonyl silane surface modification come modified pitch, synergistic effect is generated with primary antioxidant, anti-aging property has been significantly increased, and it can also make pitch that there is 60 DEG C of higher viscosity and very high low-temperature ductility, so summer is less prone to track, and winter is not easy bursting by freezing.
Description
Technical field
The present invention relates to a kind of modified pitch and preparation method thereof, more particularly to a kind of modified asphalt for road and its preparation
Method.
Background technology
Pitch is a kind of important road pavement material, but is limited by its own performance, and the high and low temperature performance of pitch is not
Stablize.Summer, pitch easily softened, and track occurs, gathers around phenomena such as bag under sunburst irradiation；Cold winter is easily split
Line seriously affects the comfort and Road Service Life of road surface running vehicle.As communications and transportation is to high speed, heavy duty, big flow, channel
The direction of change is developed, and it is solid, secured not require nothing more than highway subgrade, and highway pavement is required to possess wear-resisting, high temperature resistant, anti-soft
The functions such as change, smooth.The research of high performance modified bitumen has become an urgent demand of current road construction with application.
In existing technology, most developers improve drip by selecting suitable organic polymer modifying agent
Blue or green high-temperature stability and low-temperature cracking-resistance, but it is mainly manifested in there are limitation：（1）The stability of polymer is poor, and poly-
It is poor to the resistance to ag(e)ing of oxygen, ozone and ultraviolet light to close object；（2）Although the incorporation of polymer effectively improves the low temperature of pitch
Performance but weakens its high-temperature behavior.To solve the above problems, some developers are attempted on the basis of polymer modifiers,
Some other inorganic filler is added in, plays the comprehensive effect of organic/inorganic modifying agent to further improve the comprehensive performance of pitch.
As CN101481504A describes a kind of active nano calcium carbonate composite modified asphalt material and preparation method thereof.It should
Active nano-calcium carbonate can significantly improve the high-temperature behavior and kinetic stability of pitch, but the low temperature for reducing pitch prolongs
Degree, and antioxygenic property is still apparent insufficient.
CN102408730A discloses a kind of inorganic nano-material modified asphalt and preparation method thereof.The modified pitch is by carbon
The modifying agent and pitch of nanotube and nano ceric oxide composition are made.The modification of carbon nanotubes and nano ceric oxide composition
Agent makes pitch have preferable resistance to high and cryogenic property, but is that nano ceric oxide has ultraviolet light as anti-aging property
Stronger absorbability can significantly improve the anti-uv-ray of bituminous paving, prevent the aging of pitch, but to oxygen, ozone
Etc. antioxidations it is weaker, promoted antiageing effect it is poor.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of modified pitch and preparation method thereof.Use of the invention is adopted
With the mesopore molecular sieve of hydrosulphonyl silane surface modification come modified pitch, synergistic effect is generated with primary antioxidant, is significantly increased
Anti-aging property, and can also make pitch that there is higher 60 DEG C of viscosity and very high low-temperature ductility, such summer to be not easy
There is track, winter is not easy bursting by freezing.
The present invention provides a kind of modified pitch, which is characterized in that by weight including following raw material components：
（1）Matrix pitch：100 parts；
（2）Surface modification mesopore molecular sieve：0.1~1 part；
（3）Antioxidant：0.1~1 part；
Wherein, the surface modification mesopore molecular sieve is the mesopore molecular sieve that hydrosulphonyl silane is modified.
The hydrosulphonyl silane dosage is the 2%~15% of mesopore molecular sieve quality, is preferably 5%~10%.
The matrix pitch can be various pitches commonly used in the art, can be asphalt, coal tar asphalt,
One or more of oil sands bitumen, bitumen.The needle penetration of the matrix pitch can be 80~100 1/10mm.Oil
Pitch can be selected from one or more of straight asphalt, solvent deoiling pitch, oxidized asphalt, semi-oxidized pitch, straight asphalt
Can be the decompression residuum that the reduced crude that crude oil atmospheric distillation obtains or crude oil are obtained through vacuum distillation.
The antioxidant can be hindered phenol type antioxidant.The antioxidant is 2,6- toluene di-tert-butyl phenols, right
Tert-butyl catechol, 3,5- di-tert-butyl-4-hydroxyl benzyls diethyl phosphonate, β-（3,5- di-t-butyl -4- hydroxy benzenes
Base）The positive octadecanol ester of propionic acid, β-(3,5- di-tert-butyl-hydroxy phenyls）Propionic acid isooctanol ester, 4,4'- thiobis (uncles 6-
Butyl -3- methylphenols）, four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester, 1,3,5- trimethyls-
2,4,6- tri-（3,5- di-tert-butyl-4-hydroxyl benzyls）One or more of benzene.
The mesopore molecular sieve is one in MCM-41, MCM-22, MCM-48, SBA-15, SBA-16, HMS molecular sieve
Kind or several, one or more of prioritizing selection MCM-41, SBA-15 and MCM-48 molecular sieve.
The specific surface area of the mesopore molecular sieve is 600~1250 m2/g。
The hydrosulphonyl silane is γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane and γ-mercapto propyl
One or more of methyldiethoxysilane.
The present invention also provides a kind of preparation methods of modified pitch described above, include the following steps：
（1）Mesopore molecular sieve, hydrosulphonyl silane are added in toluene, reaction is surface modified under heated reflux condition, it is cold
But using filter, washing, drying after, surface modification mesopore molecular sieve is obtained.
（2）Surface modification mesopore molecular sieve and antioxidant are added in the matrix pitch of melting, condition of heating and stirring is equal
It is even to get to the modified pitch.
The weight ratio of the mesopore molecular sieve and toluene is 1：（10~30）.
In step（1）In, the temperature of the surface modification reaction is 100 DEG C~120 DEG C, and the time is 1~3h.
In step（1）In, conventional method may be employed in the filtering, washing, drying.Washing can use ethyl alcohol, chlorine
Imitative, acetone equal solvent is washed, and drying vapors away solvent, and dry temperature can be 80 DEG C~120 DEG C, and the time is
0.5~5.0h.
In step（2）In, the temperature of the heating stirring is 130 DEG C~150 DEG C, and the time is 0.5~1.0h.
Compared with prior art, modified pitch of the invention and preparation method thereof has the following advantages that：
（1）For the present invention using the mesopore molecular sieve of hydrosulphonyl silane surface modification come modified pitch, sulfydryl can be used as auxiliary antioxygen
Agent can be with hydroperoxide decomposition, and is converted into no free radical, the product of stabilization, so as to avoid the freedom that hydroperoxides generate
The reaction for the free radical chain that base further triggers, and free radical present in pitch can be eliminated by resistance type antioxidant, so as to
Avoid the free chain reaction of organic matter in pitch, such sulfydryl and primary antioxidant（Hindered phenol type antioxidant）Generate collaboration
Effect, has been significantly increased anti-aging property.
（2）The mesopore molecular sieve of hydrosulphonyl silane surface modification of the present invention, can not only improve antioxygenic property, but also carry
High 60 DEG C of viscosity of pitch, in summer under sunburst irradiation, pitch does not soften, and is less prone to track, gathers around phenomena such as bag；
Low-temperature ductility is also improved, therefore crackle is less prone in cold winter, so as to extend the service life of road.
Specific embodiment
The technical characterstic that the invention is further illustrated by the following examples, but these embodiments cannot limit the present invention,
The wt% being related to is mass fraction.
Embodiment 1
（1）By 1 parts by weight MCM-41 mesopore molecular sieves（Specific surface area is 1000 m2/g）, account for MCM-41 mesopore molecular sieves 5wt%
γ-mercaptopropyl trimethoxysilane be added in 20 parts by weight of toluene.The constant temperature at 110 DEG C, it is lasting to stir, it is heated to reflux
3h, cooled and filtered are washed with a large amount of ethyl alcohol, and 100 DEG C of dry 5h obtain surface modification mesopore molecular sieve.
（2）0.8 parts by weight surface modification mesopore molecular sieve and 0.2 parts by weight 2,6- toluene di-tert-butyl phenols are added to
The matrix pitch of 100 parts by weight melting（Decompression residuum, 25 DEG C of needle penetrations are 93 1/10mm）In, it is lasting to stir at 140 DEG C
0.75h makes the two uniformly be scattered in matrix pitch, you can to obtain surface modification mesopore molecular sieve modified pitch.
Embodiment 2
（1）By 1 parts by weight MCM-48 mesopore molecular sieves（Specific surface area is 800 m2/g）, account for MCM-48 mesopore molecular sieves 8wt%'s
Gamma-mercaptopropyltriethoxysilane is added in 20 parts by weight of toluene.The constant temperature at 120 DEG C, it is lasting to stir, 2h is heated to reflux,
Cooled and filtered is washed with a large amount of ethyl alcohol, and 100 DEG C of dry 5h obtain surface modification mesopore molecular sieve.
（2）By 0.5 parts by weight surface modification mesopore molecular sieve and 0.5 parts by weight 4,4'- thiobis (6- tertiary butyl -3- first
Base phenol）It is added to the matrix pitch of 100 parts by weight melting（Decompression residuum, 25 DEG C of needle penetrations are 93 1/10mm）In, 130
At DEG C, 1h is persistently stirred, the two is made uniformly to be scattered in matrix pitch, you can obtains surface modification mesopore molecular sieve and is modified drip
It is blue or green.
Embodiment 3
（1）By 1 parts by weight SBA-15 mesopore molecular sieves（Specific surface area is 1100 m2/g）, account for SBA-15 mesopore molecular sieves 10wt%
γ-mercapto hydroxypropyl methyl diethoxy silane be added in 20 parts by weight of toluene.The constant temperature at 120 DEG C, it is lasting to stir, it heats back
3h is flowed, cooled and filtered is washed with a large amount of ethyl alcohol, and 100 DEG C of dry 5h obtain surface modification mesopore molecular sieve.
（2）By 0.2 parts by weight surface modification mesopore molecular sieve and 0.8 parts by weight β-（3,5- di-t-butyl -4- hydroxy benzenes
Base）It is added to the matrix pitch of 100 parts by weight melting（Decompression residuum, 25 DEG C of needle penetrations are 93 1/10mm）In, at 140 DEG C,
0.75h is persistently stirred, the two is made uniformly to be scattered in matrix pitch, you can obtains surface modification mesopore molecular sieve and is modified drip
It is blue or green.
Comparative example 1
By 0.8 parts by weight without the MCM-41 mesopore molecular sieves of surface modification（With embodiment 1）With 0.2 parts by weight 2,6-, bis- uncles
Butyl p-cresol is added to the matrix pitch of 100 parts by weight melting（Decompression residuum, 25 DEG C of needle penetrations are 93 1/10mm）In,
At 140 DEG C, 0.75h is persistently stirred, the two is made uniformly to be scattered in matrix pitch, obtains non-surface modification mesoporous molecular
Sieve modified pitch.
Test case
The modified pitch of embodiment 1-3 and comparative example 1 are tested, the result is shown in tables 1.Wherein, Thin Film Oven Test TFOT according to
Standard GB/T5304-2001 is tested.
Matrix pitch, the property of modified pitch of 1 present invention of table and comparative example
| Matrix pitch | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| Modified pitch | |||||
| Needle penetration（25℃）, 0.1mm | 93 | 92 | 92 | 93 | 92 |
| 10 DEG C of ductilities, cm | 85 | 87 | 86 | 85 | 85 |
| Softening point, DEG C | 45.4 | 46.8 | 46.5 | 46.0 | 45.7 |
| 60 DEG C of viscosity, Pa.s | 210 | 223 | 218 | 215 | 213 |
| After Thin Film Oven Test TFOT | |||||
| Penetration ratio, % | 63 | 68 | 66 | 65 | 65 |
| 10 DEG C of ductilities, cm | 27 | 50 | 46 | 45 | 38 |
| Remain Ductility ratio, % | 32 | 57 | 53 | 50 | 45 |
By, as it can be seen that after Thin Film Oven Test TFOT, the needle penetration loss of surface modification mesopore molecular sieve modified pitch is less than base in table 1
Matter pitch, ductility value also apparently higher than matrix pitch, show that the addition of surface modification mesopore molecular sieve and antioxidant improves
The ageing resistance and stability of pitch.It is compatible with pitch that the hydrosulphonyl silane that mesopore molecular sieve surface introduces effectively improves it
Property enhances the combination power of itself and pitch, reduces the volatilization of light components in pitch, while sulfydryl and primary antioxidant cooperate with
Effect significantly improves the anti-aging property of pitch.After Thin Film Oven Test TFOT, surface modification mesopore molecular sieve modified pitch and
Non- surface modification mesopore molecular sieve modified pitch is compared, the former has higher ductility, illustrates sulfydryl as auxiliary antioxidant,
The synergistic effect of itself and primary antioxidant effectively increases the anti-aging property of pitch.
Claims (13)
1. a kind of modified pitch, which is characterized in that by weight including following raw material components：
Matrix pitch：100 parts；
Surface modification mesopore molecular sieve：0.1~1 part；
Antioxidant：0.1~1 part；
Wherein, the surface modification mesopore molecular sieve is the mesopore molecular sieve that hydrosulphonyl silane is modified.
2. modified pitch according to claim 1, it is characterised in that：The hydrosulphonyl silane dosage is mesopore molecular sieve quality
2%~15%, be preferably 5%~10%.
3. modified pitch according to claim 1, it is characterised in that：The matrix pitch is asphalt, coal tar drips
One or more of green grass or young crops, oil sands bitumen, bitumen.
4. modified pitch according to claim 1, it is characterised in that：The needle penetration of the matrix pitch is 80~100 1/
10mm。
5. modified pitch according to claim 1, it is characterised in that：The antioxidant is hindered phenol type antioxidant.
6. modified pitch according to claim 1 or 5, it is characterised in that：The antioxidant is 2,6- di-t-butyls to first
Phenol, p-tert-Butylcatechol, 3,5- di-tert-butyl-4-hydroxyl benzyls diethyl phosphonate, β-（3,5- di-t-butyls -4-
Hydroxy phenyl）The positive octadecanol ester of propionic acid, β-(3,5- di-tert-butyl-hydroxy phenyls）Propionic acid isooctanol ester, 4,4'- thiobis
(6- tertiary butyl -3- methylphenols）, four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester, 1,3,5- tri-
Methyl -2,4,6- three（3,5- di-tert-butyl-4-hydroxyl benzyls）One or more of benzene.
7. modified pitch according to claim 1, it is characterised in that：The mesopore molecular sieve for MCM-41, MCM-22,
One or more of MCM-48, SBA-15, SBA-16, HMS molecular sieve is preferably MCM-41, SBA-15 and MCM-48 molecule
One or more of sieve.
8. the modified pitch according to claim 1 or 7, it is characterised in that：The specific surface area of the mesopore molecular sieve is 600
~1250 m2/g。
9. modified pitch according to claim 1, it is characterised in that：The hydrosulphonyl silane is γ-mercapto propyl trimethoxy
One or more of silane, gamma-mercaptopropyltriethoxysilane and γ-mercapto hydroxypropyl methyl diethoxy silane.
10. the preparation method of the modified pitch as described in any in a kind of 1-9 such as claim, which is characterized in that it includes as follows
Step：
（1）Mesopore molecular sieve, hydrosulphonyl silane are added in toluene, reaction is surface modified under heated reflux condition, it is cold
But using filter, washing, drying after, surface modification mesopore molecular sieve is obtained.
（2）Surface modification mesopore molecular sieve and antioxidant are added in the matrix pitch of melting, heating stirring uniformly to get to
The modified pitch.
11. preparation method according to claim 10, it is characterised in that：The weight ratio of the mesopore molecular sieve and toluene
For 1：（10~30）.
12. the preparation method according to claim 10 or 11, it is characterised in that：In step（1）In, the surface modification is anti-
The temperature answered is 100 DEG C~120 DEG C, and the time is 1~3h.
13. the preparation method according to claim 10 or 11, it is characterised in that：In step（2）In, the heating stirring
Temperature is 130 DEG C~150 DEG C, and the time is 0.5~1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610983418.8A CN108059840B (en) | 2016-11-09 | 2016-11-09 | Modified asphalt and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610983418.8A CN108059840B (en) | 2016-11-09 | 2016-11-09 | Modified asphalt and preparation method thereof |
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| CN108059840A true CN108059840A (en) | 2018-05-22 |
| CN108059840B CN108059840B (en) | 2020-11-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636785A (en) * | 2021-07-26 | 2021-11-12 | 温州市凯安建设有限公司 | Permeable asphalt mixture |
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