CN102924933A - Desulfuration rubber powder modified asphalt with high storage stability and preparation method thereof - Google Patents
Desulfuration rubber powder modified asphalt with high storage stability and preparation method thereof Download PDFInfo
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Abstract
The invention relates to desulfuration rubber powder modified asphalt with high storage stability and a preparation method thereof. The method comprises the following steps of: premixing asphalt, a stabilizer and desulfuration rubber powder at the temperature of between 160 and 190 DEG C; and mixing the asphalt, the stabilizer and the desulfuration rubber powder uniformly by high-speed shearing under the action of mechanical force to obtain the desulfuration rubber powder modified asphalt. According to the method, the compatibility of the asphalt and the desulfuration rubber powder is improved by the stabilizer under the chemical action, so that the storage stability of the desulfuration rubber powder modified asphalt is improved, and three index performances of the modified asphalt are also improved greatly. Simultaneously, the aims of recycling wastes and reducing environmental pollution are fulfilled.
Description
Technical field:
The present invention relates to a kind of high storage stability asphalt modified with desulfurized rubber powder and preparation method thereof.
Background technology:
Pitch has been widely used in the construction of high-grade highway, but the plain asphalt road surface exists shortcomings such as high temperature easily softening, fragile under low temperaturely splits, poor flexibility.Polymer modified asphalt can improve these use propertieies of bituminous pavement, and simultaneously ageing-resistant and weather resistance and anti-water damage property are also largely strengthened.Studies show that polymer modified asphalt also is very significantly improved at aspects such as anti-rut, antifatigue cracking, resistance to permanent deformation.Because the existence of these premium propertiess, polymeric modification pitch more and more are applied to the construction of high-grade highway at present.The polymerization that is applied at present modifying asphalt mainly contains SBS thermoplastic elastomer, styrene-butadiene rubber(SBR), polyethylene etc., and still, the cost of these materials is higher, limits its application on highway.
Rubber powder is made through smashing to process by rubber wastes such as junked tires, and rubber powder modified asphalt not only can improve the various performances of pitch, can also recycle waste old, reduce solid waste to the pollution of environment, and cost is lower.The shortcomings such as but from domestic and international research situation, common waste rubber powder modified asphalt exists that viscosity is large, poor fluidity, compound stir difficulty and the bad dispersibility of rubber powder in pitch, causes easily compactness of pavement not enough, and porosity is large; Secondly, rubber powder is combined bad with the interface of pitch, poor stability, and in storing use procedure, the modifying asphalt poor stability produces laminated segregation easily between rubber powder and the pitch, have a strong impact on road quality.
The desulfurization rubber powder is the waste rubber powder that waste rubber powder is made through certain desulfurization means desulfurization, the desulfurization rubber powder is owing to be that the cross-link bond of three-dimensional net structure in the original shoddy is destroyed, the viscosity of asphalt modified with desulfurized rubber powder is descended rapidly, solved common rubber powder modified asphalt and had that viscosity is large, the problem of constructional difficulties.It is joined carry out the premium properties that modification not only can keep the waste rubber powder modifying asphalt in the pitch, simultaneously because it is in the process of carrying out desulfurization, under the effect of high temperature and high shear force, make the desulfurization vulcanized rubber powder produce the part active group, can well improve the consistency of itself and pitch, storage stability is had some improvement.But the desulfurization degree of the desulfurization rubber powder for preparing under present employed high temperature and the high shear force is smaller, segregation still can appear in the long-time high temperature storage process, simultaneously owing to the desulfurization rubber powder that exists of sweetening agent also can further be degraded, have influence on the use properties on modifying asphalt and road surface, need further to improve.The present invention comes modifying asphalt with the overcritical desulfurization rubber powder of high desulfurization degree, under the effect of stablizer, the storage stability of modifying asphalt is improved greatly, and high temperature and the low-temperature performance of pitch have also obtained further improvement simultaneously.
Summary of the invention:
The invention provides a kind of high storage stability asphalt modified with desulfurized rubber powder and preparation method thereof, the desulfurization rubber powder that makes with pitch, stablizer with supercritical process is premix at a certain temperature, then makes after high speed shear.Because used desulfurization rubber powder adopts supercritical process to make, its desulfurization degree is high, and the crosslinking structure of original rubber is broken, so that the viscosity of modifying asphalt reduces, ductility increases.In addition, the active group effect in the stablizer of interpolation and the desulfurization rubber powder so that the storage stability of modifying asphalt is improved, has suppressed the degraded of rubber powder in storage process simultaneously.
A kind of high storage stability asphalt modified with desulfurized rubber powder that the present invention relates to, its essentially consist and mass fraction are: 100 parts of pitches, 10～30 parts of desulfurization rubber powders, 0.1～10 part of stablizer.
Described stablizer is any in the following material or their mixture: Pyroglutaric acid, Succinic anhydried, resol, acrylate.
Described desulfurization rubber powder is the desulfurization rubber powder of waste rubber powder through making after the desulfurization, and particle diameter is 20 ~ 80 orders.
Described desulfurization rubber powder is the desulfurization rubber powder that supercritical process makes, can adopt commercial product also can adopt following method preparation: in high-temperature high-pressure reaction kettle, to add rubber powder, activator and dry ice and react, the quality of activator is 2% ~ 10% of rubber powder quality, and the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 150 ℃ ~ 190 ℃ conditions, react 120min ~ 300min; Then in the high speed Banbury mixer, shear 15min ~ 60min and obtain the desulfurization rubber powder.
Described activator is: N, N'-(dithio two-2,1-phenylene) dibenzamide, curing-2, any in 2'-dibenzoyl amido hexichol, tertiary butyl disulphide, the allyl disulfide or their mixture.
The present invention also provides a kind of preparation method of asphalt modified with desulfurized rubber powder, comprises two steps of material pre-mixing and high speed shear mixing, is specially:
(1) material pre-mixing: with pitch, desulfurization rubber powder and stablizer in proportion, under 160～190 ℃ of temperature, fully mix, obtain pre-composition;
(2) high speed shear is mixed: the pre-composition with step (1) obtains, and under 160～190 ℃ of temperature, use high-speed shearing emulsion machine to carry out continuous high shear mixing, make asphalt modified with desulfurized rubber powder.
The premixed time is 5～25min in the above-mentioned steps (1).
The rotating speed of above-mentioned steps (2) high speed emulsification pretreatment machine is 10000～16000r/min.
Above-mentioned steps (2) the high speed shear-mixed time is 30～60min.
The present invention makes pitch, stablizer and desulfurization rubber powder under 160～190 ℃ temperature through high speed shear.Used desulfurization rubber powder is the high desulfurization degree rubber powder that makes with supercritical process, in the two-phase system of this asphalt modified with desulfurized rubber powder, the rubber powder of partial desulfurization and pitch have good consistency and form homogeneous system with pitch, and the content of rubber powder phase is reduced, and assemble thereby reduce rubber powder granule.The reaction of active group in stablizer and the modifying asphalt further strengthens consistency, thereby has solved the problems such as the segregation layering that occurs in storage and the use procedure, degraded.And preparation process of the present invention is simple, and raw material is cheap, has very strong practicality.
Embodiment:
Below by Comparative Examples and embodiment the present invention is further elaborated.
Comparative Examples 1:
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, 20 mass parts, 40 purpose desulfurization rubber powders (the Jiangsu peace is strong), under 600r/min, stir 15min with common stirrer first at 180 ℃, then shear dispersion 45min at 180 ℃ of lower high-speed shearing machines that adopt, rotating speed is 10000r/min, obtain modifying asphalt, the performance index of modifying asphalt see Table 1.
Comparative Examples 2:
Add 100 mass parts, 40 order rubber powders, 3 mass parts N in high-temperature high-pressure reaction kettle, N'-(dithio two-2,1-phenylene) dibenzamide and dry ice react, and the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 170 ℃ of conditions, react 180min; Then be to shear 30min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 20 mass parts makes, under 600r/min, stir 15min with common stirrer first at 180 ℃, then shear dispersion 60min at 180 ℃ of lower high-speed shearing machines that adopt, rotating speed is 10000r/min, obtain modifying asphalt, the performance index of modifying asphalt see Table 1.
Embodiment 1:
Add 100 mass parts, 40 order rubber powders, 4.5 mass parts curing-2 in high-temperature high-pressure reaction kettle, 2'-dibenzoyl amido hexichol and dry ice react, and the add-on of dry ice makes CO in the still
2Degree is 0.466g/cm
3~ 0.6g/cm
3, under 170 ℃ of conditions, react 180min; Then be to shear 45min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 25 mass parts makes, 2 mass parts Pyroglutaric acids, under 600r/min, stir 15min with common stirrer first at 180 ℃, then shear and disperse 45min at 180 ℃ of lower high-speed shearing machines (German Fu Luke D type, lower with) that adopt, rotating speed is 12000r/min, obtain modifying asphalt, the performance index of test modifying asphalt.The results are shown in Table 2.
Embodiment 2:
Add 100 mass parts, 40 order rubber powders, 6 mass parts tertiary butyl disulphide and dry ice and react in high-temperature high-pressure reaction kettle, the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 180 ℃ of conditions, react 150min; Then be to shear 45min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 25 mass parts makes, 1.5 mass parts acrylate, under 600r/min, stir 20min with common stirrer first at 160 ℃, then shear and disperse 45min at 160 ℃ of lower high-speed shearing machines (German Fu Luke D type, lower with) that adopt, rotating speed is 14000r/min, obtain modifying asphalt, the performance index of test modifying asphalt.The results are shown in Table 2.
Embodiment 3:
In high-temperature high-pressure reaction kettle, add 100 mass parts, 40 order rubber powders, 2 mass parts N, N'-(dithio two-2, the 1-phenylene) dibenzamide, 1.5 mass parts curing-2,2'-dibenzoyl amido hexichol and dry ice react, and the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 180 ℃ of conditions, react 150min; Then be to shear 60min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 25 mass parts makes, 1 mass parts Pyroglutaric acid, 0.5 mass parts acrylate, under 600r/min, stir 20min with common stirrer first at 170 ℃, then shear and disperse 30min at 170 ℃ of lower high-speed shearing machines (German Fu Luke D type, lower with) that adopt, rotating speed is 16000r/min, obtain modifying asphalt, the performance index of test modifying asphalt.The results are shown in Table 2.
Embodiment 4:
Add 100 mass parts, 40 order rubber powders, 2 mass parts curing-2 in high-temperature high-pressure reaction kettle, 2`-dibenzoyl amido hexichol, 4 mass parts tertiary butyl disulphide and dry ice react, and the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 170 ℃ of conditions, react 180min; Then be to shear 60min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 20 mass parts makes, 1 mass parts Pyroglutaric acid, 0.5 mass parts resol, 0.5 mass parts acrylate, under 600r/min, stir 25min with common stirrer first at 170 ℃, then shear and disperse 55min at 170 ℃ of lower high-speed shearing machines (German Fu Luke D type, lower with) that adopt, rotating speed is 10000r/min, obtain modifying asphalt, the performance index of test modifying asphalt.The results are shown in Table 2.
Embodiment 5:
Add 100 mass parts, 40 order rubber powders, 3 mass parts allyl disulfides, 2 mass parts tertiary butyl disulphide and dry ice and react in high-temperature high-pressure reaction kettle, the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 190 ℃ of conditions, react 120min; Then be to shear 30min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 20 mass parts makes, 1 mass parts Succinic anhydried, 0.5 mass parts resol, 0.3 mass parts acrylate, under 600r/min, stir 15min with common stirrer first at 190 ℃, then shear and disperse 45min at 190 ℃ of lower high-speed shearing machines (German Fu Luke D type, lower with) that adopt, rotating speed is 12000r/min, obtain modifying asphalt, the performance index of test modifying asphalt.The results are shown in Table 2.
Embodiment 6:
In high-temperature high-pressure reaction kettle, add 100 mass parts, 40 order rubber powders, 1 mass parts N, N'-(dithio two-2, the 1-phenylene) dibenzamide, 1.3 mass parts curing-2,2`-dibenzoyl amido hexichol, 3 mass parts allyl disulfides and dry ice react, and the add-on of dry ice makes CO in the still
2Density is 0.466g/cm
3~ 0.6g/cm
3, under 160 ℃ of conditions, react 220min; Then be to shear 45min in the high speed Banbury mixer (model F370, U.S. Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A.) of 55r/min to obtain overcritical desulfurization rubber powder at rotating speed.
It is 100 parts matrix pitch (Qinhuangdao 70#) with mass fraction, the desulfurization rubber powder that the overcritical doctor treatment of 20 mass parts makes, 0.8 mass parts Pyroglutaric acid, 0.5 mass parts Succinic anhydried, 0.25 mass parts resol, 0.15 mass parts acrylate, under 600r/min, stir 10min with common stirrer first at 180 ℃, then at 180 ℃ of lower high-speed shearing machine (German Fu Luke D types that adopt, together lower) shear and disperse 45min, rotating speed is 13000r/min, obtain modifying asphalt, the performance index of test modifying asphalt.The results are shown in Table 2.
The data of contrast table 1, table 2 can be learnt, the desulfurization rubber powder modified asphalt of the present invention's preparation, on its penetration degree, softening temperature, low-temperature ductility, the especially stability in storage, the asphalt modified with desulfurized rubber powder performance of all not adding properties-correcting agent is significantly improved, and can reach the Ministry of Communications about the performance index requirement of rubber powder modified asphalt.
The performance data of table 1 asphalt modified with desulfurized rubber powder
| Test index | Matrix pitch | Comparative Examples 1 | Comparative Examples 2 |
| Penetration degree (0.1mm) | 67 | 35 | 34 |
| 5 ℃ of ductilities (cm) | 0 | 8 | 11 |
| Softening temperature (° C) | 46 | 65 | 63 |
| 165 ℃ of viscositys (Pa.s) | 0.15 | 1.8 | 1.2 |
| Storage stability (℃, up and down softening point difference) | - | 8.3 | 7.4 |
The performance data of the modifying asphalt of table 2 the present invention preparation
Annotate: the testing method of property indices is in table 1, the table 2:
The penetration degree test:
In the water bath with thermostatic control with 25 ℃ on sample, the draw point of load 100g weight freely falls, and the degree of depth of injection in 5 seconds sample is take 0.1mm as unit.
The ductility test:
In 5 ℃ water bath with thermostatic control, with the speed tension specimen of the 5cm/min length (cm) when rupturing.
Softening temperature test (ring and ball method):
5 ℃/min heats up in 5 ℃ of distilled water, and steel ball falls to when the lower floor backplate surface contacts on the sample loop, reads immediately temperature, be softening temperature (℃).
The stable storing property testing:
Pour the rubber powder modified asphalt sample for preparing into diameter 2.5Cm, long for vertically being positioned over 48h in 163 ℃ of baking ovens in the aluminum pipe of 14cm, put into up and down each 1/3 place of sample thief behind the refrigerator cooling 4h after the taking-up, test respectively softening temperature, and get its difference and be used for estimating storage stability.
Claims (7)
1. one kind high storage stability asphalt modified with desulfurized rubber powder, its essentially consist and mass fraction are: 100 parts of pitches, 10～30 parts of desulfurization rubber powders, 0.1～10 part of stablizer; Described stablizer is any in the following material or their mixture: Pyroglutaric acid, Succinic anhydried, resol, acrylate.
2. high storage stability asphalt modified with desulfurized rubber powder according to claim 1 is characterized in that: described desulfurization rubber powder is the desulfurization rubber powder of waste rubber powder through making after the desulfurization, and particle diameter is 20 ~ 80 orders.
3. high storage stability asphalt modified with desulfurized rubber powder according to claim 1 and 2, it is characterized in that: described desulfurization rubber powder makes under super critical condition.
4. the preparation method of a high storage stability asphalt modified with desulfurized rubber powder claimed in claim 1 comprises two steps of material pre-mixing and high speed shear mixing, is specially:
(1) material pre-mixing: with pitch, desulfurization rubber powder and stablizer in proportion, under 160～190 ℃ of temperature, fully mix, obtain pre-composition;
(2) high speed shear is mixed: the pre-composition with step (1) obtains, and under 160～190 ℃ of temperature, use high-speed shearing emulsion machine to carry out continuous high shear mixing, make asphalt modified with desulfurized rubber powder.
5. according to claim 4 preparation method, it is characterized in that: the premixed time is 5～25min in the step (1).
6. according to claim 4 preparation method, it is characterized in that: the rotating speed of step (2) high speed emulsification pretreatment machine is 10000～16000r/min.
7. according to claim 4 preparation method, it is characterized in that: step (2) the high speed shear-mixed time is 30～60min.
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| CN107325569A (en) * | 2017-08-22 | 2017-11-07 | 四川知行路桥股份有限公司 | A kind of modifying agent for high viscosity compound rubber asphalt |
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| CN110746788A (en) * | 2019-11-08 | 2020-02-04 | 同济大学 | High-solubility rubber powder modified asphalt and preparation method thereof |
| CN113061288A (en) * | 2021-03-29 | 2021-07-02 | 广西交科集团有限公司 | Desulfurized rubber powder and preparation method thereof, and rubber asphalt composite material and preparation method thereof |
| CN113214535A (en) * | 2021-03-31 | 2021-08-06 | 长安大学 | Activated rubber powder and preparation method thereof, and modified asphalt based on activated rubber powder and preparation method thereof |
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Application publication date: 20130213 |