CN106750699A - Shoddy prepares the conversion ratio assay method and rubber asphalt preparation method of rubber asphalt - Google Patents
Shoddy prepares the conversion ratio assay method and rubber asphalt preparation method of rubber asphalt Download PDFInfo
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- CN106750699A CN106750699A CN201611144944.1A CN201611144944A CN106750699A CN 106750699 A CN106750699 A CN 106750699A CN 201611144944 A CN201611144944 A CN 201611144944A CN 106750699 A CN106750699 A CN 106750699A
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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
- C08L19/00—Compositions of rubbers not provided for in groups C08L7/00 - C08L17/00
- C08L19/003—Precrosslinked rubber; Scrap rubber; Used vulcanised rubber
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The present invention relates to a kind of preparation of the asphalt material for pavement engineering, specifically a kind of shoddy prepares the conversion ratio assay method and rubber asphalt preparation method of rubber asphalt.Assay method is comprised the following steps：1. sampling detection solubility, weighs sample quality；2. by the filter paper with sample, add 150ml toluene to be installed in sequence with extraction tube, condenser in extraction tube, in extraction flask, be heated to reflux；3. the filter paper with insoluble matter is put into baking oven and dried, be cooled to room temperature, weighing obtains constant weight quality；4. calculate and obtain solubility, solubility is compared into calculating with theoretical dissolution degree, obtain conversion ratio.Dissolubility difference of the present invention using asphalt and rubber powder in toluene, the solubility to rubber asphalt is measured, improves accuracy of detection, simplifies detecting step；The assay method is used in the preparation of rubber asphalt simultaneously, the properties of product of rubber asphalt are improve.
Description
Technical field
The present invention relates to a kind of preparation of the asphalt material for pavement engineering, specifically a kind of shoddy prepares rubber drip
Blue or green conversion ratio assay method and rubber asphalt preparation method.
Background technology
The rubber asphalt made of shoddy no matter from comprehensive utilization, the environmental protection of useless rubber powder, or from promoting road
The development of traffic all has highly important application value.Most of domestic and international research to rubber asphalt at present is all concentrated on and added
Influence of influence and different condition of the work treatment conditions to the modified pitch rheological equationm of state to the interphase interaction of pitch and rubber, makes
Production method mainly has two kinds：Wet method and dry method, either rubber powder does not have with pitch in this process for dry method or wet method
Chemically react, the rubber asphalt of formation is heterogeneous, is made up of pitch medium and rubber particle, but pitch is light
Fragrance packet part can be penetrated into micelle, make micelle swelling, therefore viscosity improves many compared with pitch, as a result causes in mixing
The increase of viscosity at temperature and pumping temperature, can make pumping and the mixing of the mixed pitch of heat and compacting more difficult, be easily caused road
Voidage is high, and adhesive is possible to no complete wetting and gathers materials and cause road damage, and due to rubber powder be not dissolved it is swelling,
There is certain resilience, also easily cause Asphalt Concrete Pavement Compaction deficiency, voidage is larger, and road surface water resistant stability is poor, adhesive
It is easily peeled off with gathering materials, water occurs and surely destroys.
Rubber asphalt exist another problem be that system stability is very poor during storage and use, rubber powder with drip
It is blue or green easily to isolate, settle.
General polymerization thing modifying agent such as SBS, SBR, SIS and EVA can preferably dissolve and be dispersed in pitch, form sub- equal
Phase structure, therefore polymer modified asphalt is than more uniform.And rubber asphalt modified system and other polymer modified asphalt systems
Difference, because shoddy can not be dissolved in pitch, can only be filled in pitch as elastic particle, therefore, rubber asphalt is at this
It is heterogeneous in matter, is a kind of heterogeneous system, inhomogeneity is the key factor for influenceing rubber asphalt property and using.
The content of the invention
It can be that rubber asphalt prepared by raw material has to shoddy that the technical problems to be solved by the invention are to provide a kind of
Effect conversion rate carries out the assay method of Accurate Determining, and based on the assay method, it is possible to increase rubber asphalt usability
The rubber asphalt preparation method of preparation time, can be shortened.
The conversion ratio assay method that shoddy of the invention prepares rubber asphalt is comprised the following steps：
1. the rubber asphalt sampling detection solubility that will be prepared as raw material with shoddy, weighs constant weight quantitative filter paper matter
Amount m1, then it weighs sample quality m above again2。
2. the filter paper with sample is folded, is put into extraction tube, to adding 150ml toluene and extraction tube, cold in extraction flask
Condenser is installed in sequence, is heated to reflux 1.5~3h or colourless to lower dropping liquid, and backflow is finished, and removes extraction flask, extraction tube.
3. the filter paper with insoluble matter is put into baking oven, is 100 DEG C -110 DEG C, keeps more than 0.5h in temperature, taken out
Afterwards, room temperature is cooled in equipped with dryer, weighing obtains constant weight quality m3。
4. rubber asphalt solubility S1={ 1- (m3-m1)/(m2-m1) × 100%, the solubility and theoretical dissolution that will be determined
Degree compares calculating, obtains conversion ratio.
A kind of preparation method of rubber asphalt is：It is (excellent by the 5~50% of material quality by the shoddy of mesh number 10~300
Elect 15 as~50%) be added to asphalt of the temperature at 150~230 DEG C, add 0.5~5% accelerator (thiazoles M, two
Thiocarbamate class ZDMC, xanthic acid salt ZBX), between the reactor and shearing grinding or High shear device of band stirring,
It is circulated reaction and shearing grinding or high shear；In the shearing grinding of reaction or high shear process, sample is extracted according to upper
The conversion ratio assay method detection conversion ratio that shoddy prepares rubber asphalt is stated, reaction acquisition is stopped most after reaching setting conversion ratio
Finished product.
The accelerator is one of thiazoles M, dithiocarbamates ZDMC, xanthic acid salt ZBX.
Dissolubility difference of the present invention using asphalt and rubber powder in toluene, the solubility to rubber asphalt is carried out
Determine, while containing more insoluble matter in considering rubber asphalt, easily block filter paper, cannot using T0607 solubility methods
Experiment, thus using rubber asphalt solubility is determined with apparatus,Soxhlet's, so as to improve accuracy of detection, simplify detection step
Suddenly；The assay method is used in the preparation of rubber asphalt simultaneously, the properties of product of rubber asphalt are improve.
Specific embodiment
Embodiment one：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 10,70# asphalt of the temperature at 150~160 DEG C is added to by the 15% of material quality,
One-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 4h, 6h, detects its conversion ratio, and detecting step is such as
Under：
(1) sampling detection solubility, weighs constant weight quantitative filter paper quality m1, and then it weighs sample quality above again
m2。
(2) filter paper with sample is folded, is put into extraction tube, to adding 150ml toluene and extraction tube, cold in extraction flask
Condenser is installed in sequence, is heated to reflux 1.5~3h or colourless to lower dropping liquid, and backflow is finished, and removes extraction flask, extraction tube.
(3) filter paper with insoluble matter is put into baking oven, is 100 DEG C -110 DEG C, keeps more than 0.5h in temperature, taken out
Afterwards, room temperature is cooled in equipped with dryer, weighing obtains constant weight quality m3。
(4) rubber asphalt solubility S1={ 1- (m3-m1)/(m2-m1) × 100%, the solubility that will be determined is molten with theory
Xie Du compares calculating, obtains conversion ratio, and the data for obtaining are shown in Table one.
The unit of table one：%
| Theoretical value | 2h | 4h | 6h | |
| Solubility % | 95.5 | 90.2 | 93.1 | 95.4 |
| Conversion ratio % | 94.7 | 97.6 | 99.9 |
Be can be seen that by table one：Shearing grinding or the extension in high shear reaction time, more, the rubber powder turn of shoddy degraded
Rate is higher, and easier to form sub- phase structure, product storage stability and construction workability are better.
Embodiment two：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 10,70# asphalt of the temperature at 150~160 DEG C is added to by the 15% of material quality,
0.5% thiazoles M is added simultaneously, one-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 3h, 4h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table two.
The unit of table two：%
As can be seen from the first embodiment and the second embodiment：In the effect of accelerator, the speed of shoddy degraded, explanation
Rubber powder conversion ratio is shorter close to 100% time, and system is easier to form sub- phase structure, product storage stability and construction workability
Better.
Embodiment three：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 30,70# asphalt of the temperature at 150~160 DEG C is added to by the 15% of material quality,
One-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 3h, 4h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table three.
The unit of table three：%
| Theoretical value | 2h | 3h | 4h | |
| Solubility % | 95.5 | 91.9 | 93.8 | 95.4 |
| Conversion ratio % | 96.4 | 98.3 | 99.9 |
Be can be seen that by embodiment two and embodiment three：Mesh number is bigger, and the speed of shoddy degraded is faster, illustrates that rubber powder turns
Rate is shorter close to 100% time, and system is easier to form sub- phase structure, and product storage stability and construction workability are better.
Example IV：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 30,70# asphalt of the temperature at 150~160 DEG C is added to by the 20% of material quality,
One-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 4h, 7h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table four.
The unit of table four：%
| Theoretical value | 2h | 4h | 7h | |
| Solubility % | 94 | 88.9 | 92.8 | 93.8 |
| Conversion ratio % | 94.9 | 98.8 | 99.8 |
Be can be seen that by embodiment three and example IV：Addition is bigger, and the speed of shoddy degraded is slower, illustrates rubber powder
Conversion ratio is more long close to 100% time.
Embodiment five：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 30,70# asphalt of the temperature at 170~180 DEG C is added to by the 20% of material quality,
One-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 3h, 5h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table five.
The unit of table five：%
| Theoretical value | 2h | 3h | 5h | |
| Solubility % | 94 | 89.5 | 93.0 | 93.9 |
| Conversion ratio % | 95.5 | 98.0 | 99.9 |
Be can be seen that by example IV and embodiment five：Temperature is higher, and the speed of shoddy degraded is faster, illustrates that rubber powder turns
Rate is shorter close to 100% time.
Embodiment six：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 40,90# asphalt of the temperature at 180~190 DEG C is added to by the 30% of material quality,
One-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 4h, 8h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table six.
The unit of table six：%
| Theoretical value | 2h | 4h | 8h | |
| Solubility % | 91 | 84.5 | 87.5 | 90.9 |
| Conversion ratio % | 93.5 | 96.5 | 99.9 |
Be can be seen that by embodiment six：Addition increases, slowing for shoddy degraded, illustrates that rubber powder conversion ratio is approached
100% time is more long.
Embodiment seven：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 40,90# asphalt of the temperature at 180~190 DEG C is added to by the 30% of material quality,
Three-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 1h, 2h, 3h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table seven.
The unit of table seven：%
Be can be seen that by embodiment six and embodiment seven：As shearing grinding or high shear series increase, shoddy degraded
Speed accelerate, illustrate that rubber powder conversion ratio is shorter close to 100% time.
Embodiment eight：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 100,110# oil drip of the temperature at 190~200 DEG C is added to by the 40% of material quality
Green grass or young crops, while 3% dithiocarbamates ZDMC is added, three-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 4h, 6h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table eight.
The unit of table eight：%
| Theoretical value | 2h | 4h | 6h | |
| Solubility % | 88 | 75.5 | 82.7 | 87.8 |
| Conversion ratio % | 87.5 | 94.7 | 99.8 |
Be can be seen that by embodiment eight：The volume of rubber powder 40%, in the case where accelerator acts on, shears grinding or height is cut through three-level
Cut, the speed of shoddy degraded illustrates that rubber powder conversion ratio can also close to 100% also than very fast.
Embodiment nine：
It is prepared by degradable rubber asphalt
1., by the shoddy of mesh number 200,110# oil drip of the temperature at 200~230 DEG C is added to by the 50% of material quality
Green grass or young crops, while 5% xanthic acid salt ZBX is added, three-level shearing grinding or high shear between stirred autoclave.
2. continuous shear stress grinds or the high shear reaction time is respectively 2h, 4h, 6h, detects its conversion ratio.
According to the identical assay method of embodiment one on detect conversion ratio, the data for obtaining are shown in Table nine.
The unit of table nine：%
| Theoretical value | 2h | 4h | 6h | |
| Solubility % | 85 | 73.2 | 81.7 | 84.7 |
| Conversion ratio % | 88.2 | 93.7 | 99.7 |
Be can be seen that by embodiment nine：The volume of rubber powder 50%, in the case where accelerator acts on, shears grinding or height is cut through three-level
Cut, shoddy also can all degrade, also there is the conversion ratio close to 100%.
Claims (3)
1. a kind of shoddy prepares the conversion ratio assay method of rubber asphalt, it is characterized in that：Comprise the following steps,
（1）The rubber asphalt sampling detection solubility that will be prepared as raw material with shoddy, weighs constant weight quantitative filter paper quality
m1, then it weighs sample quality m above again2；
（2）The filter paper with sample is folded, is put into extraction tube, to addition 150ml toluene in extraction flask and extraction tube, condenser
Install in sequence, be heated to reflux 1.5~3h or colourless to lower dropping liquid, backflow is finished, and removes extraction flask, extraction tube；
（3）Filter paper with insoluble matter is put into baking oven, is 100 DEG C -110 DEG C, is kept more than 0.5h in temperature, after taking-up,
Room temperature is cooled in equipped with dryer, weighing obtains constant weight quality m3；
（4）Rubber asphalt solubility S1={1-（m3- m1）/（m2- m1）} × 100%, solubility and the theoretical dissolution degree that will be determined
Compare calculating, obtain conversion ratio.
2. a kind of preparation method of rubber asphalt, it is characterized in that：By the shoddy of mesh number 10~300, by material quality 5~
50% is added to asphalt of the temperature at 150~230 DEG C, adds 0.5~5% accelerator（Thiazoles M, dithiocarbamates first
Barbiturates ZDMC, xanthic acid salt ZBX）, between the reactor and shearing grinding or High shear device of band stirring, it is circulated
Reaction and shearing grinding or high shear；In the shearing grinding of reaction or high shear process, sample is extracted according to claim 1 institute
The shoddy stated prepares the conversion ratio assay method detection conversion ratio of rubber asphalt, and reaction acquisition is stopped after reaching setting conversion ratio
Final products.
3. the preparation method of rubber asphalt according to claim 2, it is characterized in that：The accelerator is thiazoles M, two sulphur
For one of Carbamates ZDMC, xanthic acid salt ZBX.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611144944.1A CN106750699A (en) | 2016-12-13 | 2016-12-13 | Shoddy prepares the conversion ratio assay method and rubber asphalt preparation method of rubber asphalt |
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| CN201611144944.1A CN106750699A (en) | 2016-12-13 | 2016-12-13 | Shoddy prepares the conversion ratio assay method and rubber asphalt preparation method of rubber asphalt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107389496A (en) * | 2017-07-26 | 2017-11-24 | 河北省交通规划设计院 | A kind of method of the quick measure effective rubber powder content of rubber powder modified asphalt |
| CN109164008A (en) * | 2018-11-02 | 2019-01-08 | 交通运输部公路科学研究所 | A kind of test method of bitumen solubility |
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| CN102417736A (en) * | 2011-11-18 | 2012-04-18 | 武汉科技大学 | Waste rubber powder modified asphalt and preparation method thereof |
| CN102977621A (en) * | 2012-12-25 | 2013-03-20 | 天津海泰环保科技发展有限公司 | SBS (styrene-butadiene-styrene)/scrap rubber powder composite modified asphalt and preparation method thereof |
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2016
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|---|---|---|---|---|
| CN107389496A (en) * | 2017-07-26 | 2017-11-24 | 河北省交通规划设计院 | A kind of method of the quick measure effective rubber powder content of rubber powder modified asphalt |
| CN107389496B (en) * | 2017-07-26 | 2020-08-14 | 河北省交通规划设计院 | Method for rapidly determining effective rubber powder content of rubber powder modified asphalt |
| CN109164008A (en) * | 2018-11-02 | 2019-01-08 | 交通运输部公路科学研究所 | A kind of test method of bitumen solubility |
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Application publication date: 20170531 |