CN115678299B - Rubber powder modified asphalt and preparation method thereof - Google Patents
Rubber powder modified asphalt and preparation method thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a rubber powder modified asphalt and a preparation method thereof, wherein the quantity of active groups of the rubber powder is increased by adopting hydrogen peroxide to carry out oxidation pretreatment on the rubber powder, meanwhile, the surface roughness of the rubber powder is increased, the subsequent reaction is convenient, then the rubber powder is modified by utilizing a silane coupling agent tridecafluorooctyl triethoxysilane, the modified rubber powder reacts with the active groups in the asphalt, and the modified rubber powder and the asphalt form two phases which are mutually crosslinked, so that the high-temperature storage stability of the asphalt is remarkably improved; and then, the alkali lignin and the carbon disulfide are reacted in an alkaline environment to obtain modified lignin, and the modified lignin is applied to asphalt, so that the vulcanization at the interface of modified rubber powder and asphalt can be promoted, and simultaneously, phenolic hydroxyl groups which do not participate in the reaction in the alkali lignin, the modified rubber powder and active groups in the asphalt form a crosslinked network structure, so that the high-temperature deformation resistance of the asphalt is further enhanced, and the stability of a modified asphalt product is improved.
Description
Technical Field
The invention relates to the technical field of asphalt material processing, in particular to rubber powder modified asphalt and a preparation method thereof.
Background
At present, with the development of the automobile industry, the yield of waste tires is greatly increased, a large amount of waste tires are difficult to degrade and contain harmful substances, the solid waste forms serious black pollution, the environmental protection pressure is also higher and higher, so that the recycling of waste rubber is increasingly focused, and with the development of development, technicians increasingly become research hotspots by recycling waste tires and preparing the waste tires into rubber powder to remove modified asphalt.
However, because the mobility of the rubber powder and the asphalt material is poor, the viscosity of the modified asphalt synthesis system is high in the process of producing the modified asphalt, the rubber powder is not easy to be highly dispersed in the asphalt, the intersolubility between the rubber powder and the asphalt is poor, the phenomenon of poor adhesion between the rubber powder and the asphalt is easy to occur, and the quality of a modified asphalt product is influenced; at present, the surface of particles is activated or polarized by adopting a physicochemical method to carry out surface modification treatment on rubber powder, so that the adsorption effect between the rubber powder and asphalt components is enhanced, the interfacial binding force between the rubber powder and asphalt is improved, and then the compatibility between the rubber powder and asphalt is improved, and Chinese patent document CN201711499037.3 discloses rubber powder modified asphalt and a preparation method thereof.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the rubber powder modified asphalt and the preparation method thereof, which solve the technical problem of unstable product performance caused by poor compatibility between rubber powder and asphalt in the traditional process.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding the rubber powder into hydrogen peroxide, heating and stirring for reaction, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing the pretreated rubber powder in deionized water, then adding tridecafluorooctyl triethoxysilane, stirring for reaction, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Dissolving alkali lignin in deionized water, regulating the pH of the solution to 10-12, adding carbon disulfide to react, centrifuging, washing, and freeze-drying to obtain modified lignin after the reaction is completed;
(4) Adding asphalt into a premixing tank, stirring and heating to 170-180 ℃, maintaining the temperature unchanged, adding modified rubber powder, stirring and mixing uniformly, adding coal tar, continuously stirring and mixing uniformly to obtain a premix, adding the premix into a preparation tank, uniformly refining for 20-30min at 180-200 ℃, adding modified lignin, firstly shearing for 10-20min at a shearing rate of 1000-1500r/min, secondly shearing for 30-60min at a shearing rate of 3000-4000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Preferably, in the step (1), the mass ratio of the rubber powder to the hydrogen peroxide is 20-30:100, wherein the mass fraction of the hydrogen peroxide is 20-30%.
Preferably, in the step (1), the temperature of the heating and stirring reaction is 60-80 ℃, and the time of the heating and stirring reaction is 2-3 hours.
Preferably, in the step (2), the mass ratio of the pretreatment rubber powder, the deionized water and the tridecafluorooctyl triethoxysilane is 10-20:100:2-4.
Preferably, in the step (2), the temperature of the stirring reaction is 40-60 ℃, and the time of the stirring reaction is 3-5h.
Preferably, in the step (3), the mass ratio of the alkali lignin to the carbon disulfide is 10-15:2-4.
Preferably, in the step (3), the reaction temperature is 30-40 ℃ and the reaction time is 3-4h.
Preferably, in the step (4), the mass ratio of the asphalt to the modified rubber powder to the coal tar to the modified lignin is 100:25-30:2-4:8-12.
The invention also provides the rubber powder modified asphalt prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, hydrogen peroxide is adopted to carry out oxidation pretreatment on the rubber powder, so that the number of active groups of the rubber powder is increased, meanwhile, the surface roughness of the rubber powder is increased, the subsequent reaction is facilitated, then the silane coupling agent tridecafluorooctyl triethoxysilane is utilized to modify the rubber powder, the modified rubber powder reacts with the active groups in asphalt, and the modified rubber powder and asphalt form two phases which are mutually crosslinked, so that the high-temperature storage stability of the asphalt is remarkably improved; meanwhile, the tridecafluorooctyl triethoxysilane has good permeability, so that the compatibility between the modified rubber powder and asphalt is better, the swelling is more sufficient, and the modified asphalt system is more stable.
(2) According to the invention, the alkali lignin and the carbon disulfide are utilized to react in an alkaline environment to obtain the modified lignin, and then the modified lignin is applied to asphalt, so that the vulcanization at the interface of the modified rubber powder and the asphalt can be promoted, the vulcanization time is shortened, the vulcanization efficiency is improved, and meanwhile, the phenolic hydroxyl group which does not participate in the reaction in the alkali lignin, the modified rubber powder and active groups in the asphalt form a crosslinked network structure, so that the high-temperature deformation resistance of the asphalt is further enhanced, and the stability of a modified asphalt product is improved.
Detailed Description
The present invention will be described in further detail with reference to the following preferred examples, but the present invention is not limited to the following examples.
Unless otherwise specified, the chemical reagents involved in the present invention are all commercially available.
The rubber powder used in the invention is purchased from Hebei Hengguang mineral products limited company, and the granularity is 20-80 meshes;
tridecafluorooctyltriethoxysilane is available from Jiangsu Pu Le Si Biotech Inc., CAS:51851-37-7;
alkali lignin was purchased from shandong Ai Limo chemical technology limited, model: ALW001;
the asphalt is medium-temperature coal asphalt, and is purchased from Miao rubber chemical Co., ltd;
coal tar is purchased from the constant water and huge rubber chemical industry limited company.
Example 1
A preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding 2kg of rubber powder into 10kg of 20wt% hydrogen peroxide, heating and stirring at 60 ℃ for reaction for 2 hours, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing 1kg of pretreatment rubber powder in 10kg of deionized water, then adding 0.2kg of tridecafluorooctyl triethoxysilane, stirring at 40 ℃ for reaction for 3 hours, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Dissolving 100g of alkali lignin in 1500g of deionized water, regulating the pH of the solution to 10, adding 20g of carbon disulfide, stirring at 30 ℃ for reaction for 3 hours, and centrifuging, washing and freeze-drying after the reaction is completed to obtain modified lignin;
(4) Adding 10kg of asphalt into a premixing tank, stirring and heating to 170 ℃, maintaining the temperature unchanged, adding 2.5kg of modified rubber powder, stirring and mixing uniformly, adding 0.2kg of coal tar, continuously stirring and mixing uniformly to obtain a premix, adding the premix into a preparation tank, uniformly refining for 20min at 180 ℃, adding 0.8kg of modified lignin, firstly shearing for 10min at a shearing rate of 1000r/min, then shearing for 30min at a shearing rate of 3000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Example 2
A preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding 2kg of rubber powder into 10kg of 30wt% hydrogen peroxide, heating and stirring at 80 ℃ for reaction for 3 hours, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing 2kg of pretreatment rubber powder in 10kg of deionized water, then adding 0.4kg of tridecafluorooctyl triethoxysilane, stirring at 60 ℃ for reaction for 5 hours, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Dissolving 150g of alkali lignin in 1500g of deionized water, regulating the pH of the solution to 12, adding 40g of carbon disulfide, stirring at 40 ℃ for reaction for 4 hours, and centrifuging, washing and freeze-drying after the reaction is completed to obtain modified lignin;
(4) Adding 10kg of asphalt into a premixing tank, stirring and heating to 180 ℃, maintaining the temperature unchanged, adding 3.0kg of modified rubber powder, stirring and mixing uniformly, adding 0.4kg of coal tar, continuously stirring and mixing uniformly to obtain premix, adding the premix into a preparation tank, uniformly refining for 30min at 200 ℃, adjusting the temperature to 175 ℃, adding 0.8kg of modified lignin, firstly shearing for 10min at a shear rate of 1500r/min, then shearing for 30min at a shear rate of 4000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Example 3
A preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding 3kg of rubber powder into 10kg of 25wt% hydrogen peroxide, heating and stirring at 70 ℃ for reaction for 2 hours, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing 2kg of pretreatment rubber powder in 10kg of deionized water, then adding 0.3kg of tridecafluorooctyl triethoxysilane, stirring at 50 ℃ for reaction for 4 hours, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Dissolving 120g of alkali lignin in 1500g of deionized water, regulating the pH of the solution to 12, adding 30g of carbon disulfide, stirring at 35 ℃ for reaction for 3 hours, and centrifuging, washing and freeze-drying after the reaction is completed to obtain modified lignin;
(4) Adding 10kg of asphalt into a premixing tank, stirring and heating to 175 ℃, maintaining the temperature unchanged, adding 2.6kg of modified rubber powder, stirring and mixing uniformly, adding 0.3kg of coal tar, continuously stirring and mixing uniformly to obtain premix, adding the premix into a preparation tank, uniformly refining for 30min at 200 ℃, adjusting the temperature to 175 ℃, adding 1.2kg of modified lignin, firstly shearing for 20min at a shear rate of 1200r/min, then shearing for 60min at a shear rate of 3000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Example 4
A preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding 2.5kg of rubber powder into 10kg of 20wt% hydrogen peroxide, heating and stirring at 80 ℃ for reaction for 2 hours, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing 1.5kg of pretreatment rubber powder in 10kg of deionized water, then adding 0.4kg of tridecafluorooctyl triethoxysilane, stirring at 60 ℃ for reaction for 3 hours, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Dissolving 120g of alkali lignin in 1500g of deionized water, regulating the pH of the solution to 12, adding 40g of carbon disulfide, stirring at 40 ℃ for reaction for 4 hours, and centrifuging, washing and freeze-drying after the reaction is completed to obtain modified lignin;
(4) Adding 10kg of asphalt into a premixing tank, stirring and heating to 175 ℃, maintaining the temperature unchanged, adding 2.8kg of modified rubber powder, stirring and mixing uniformly, adding 0.4kg of coal tar, continuously stirring and mixing uniformly to obtain premix, adding the premix into a preparation tank, uniformly refining for 30min at 200 ℃, adjusting the temperature to 175 ℃, adding 1.0kg of modified lignin, firstly shearing for 20min at a shearing rate of 1000r/min, then shearing for 60min at a shearing rate of 3000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Comparative example 1
A preparation method of rubber powder modified asphalt comprises the following steps:
adding 10kg of asphalt into a premixing tank, stirring and heating to 175 ℃, maintaining the temperature unchanged, adding 2.6kg of rubber powder, stirring and mixing uniformly, adding 0.3kg of coal tar, continuously stirring and mixing uniformly to obtain premix, adding the premix into a preparation tank, uniformly refining for 30min at 200 ℃, adjusting the temperature to 175 ℃, adding 1.2kg of alkali lignin, firstly shearing for 20min at a shear rate of 1200r/min, then shearing for 60min at a shear rate of 3000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Comparative example 2
A preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding 3kg of rubber powder into 10kg of 25wt% hydrogen peroxide, heating and stirring at 70 ℃ for reaction for 2 hours, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing 2kg of pretreatment rubber powder in 10kg of deionized water, then adding 0.3kg of tridecafluorooctyl triethoxysilane, stirring at 50 ℃ for reaction for 4 hours, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Adding 10kg of asphalt into a premixing tank, stirring and heating to 175 ℃, maintaining the temperature unchanged, adding 2.6kg of modified rubber powder, stirring and mixing uniformly, adding 0.3kg of coal tar, continuously stirring and mixing uniformly to obtain premix, adding the premix into a preparation tank, uniformly refining for 30min at 200 ℃, adjusting the temperature to 175 ℃, firstly shearing for 20min at a shear rate of 1200r/min, then shearing for 60min at a shear rate of 3000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
Comparative example 3
A preparation method of rubber powder modified asphalt comprises the following steps:
(1) Adding 3kg of rubber powder into 10kg of 25wt% hydrogen peroxide, heating and stirring at 70 ℃ for reaction for 2 hours, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dissolving 120g of alkali lignin in 1500g of deionized water, regulating the pH of the solution to 12, adding 30g of carbon disulfide, stirring at 35 ℃ for reaction for 3 hours, and centrifuging, washing and freeze-drying after the reaction is completed to obtain modified lignin;
(3) Adding 10kg of asphalt into a premixing tank, stirring and heating to 175 ℃, maintaining the temperature unchanged, adding 2.6kg of pretreated rubber powder, stirring and mixing uniformly, adding 0.3kg of coal tar, continuously stirring and mixing uniformly to obtain premix, adding the premix into a preparation tank, uniformly refining for 30min at 200 ℃, adjusting the temperature to 175 ℃, adding 1.2kg of modified lignin, firstly shearing for 20min at a shear rate of 1200r/min, then shearing for 60min at a shear rate of 3000r/min, and obtaining the rubber powder modified asphalt after shearing is finished.
The modified asphalt samples prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance test, specifically as follows:
ductility test experiment: the testing method refers to an asphalt ductility measuring method disclosed in GB/T4508-2010, the testing temperature is 5 ℃, the stretching speed is 5cm/min, the testing is carried out for 3 times, and the result is averaged;
softening point test: asphalt softening point test (ring ball method) is carried out according to standard T0606-2011, the test is carried out for 3 times, and the result is averaged;
isolation softening point difference test experiment: the test method refers to the polymer modified asphalt segregation test method disclosed in SH/T0740-2003, the test is carried out for 48 hours at 163 ℃, the softening point is measured, the softening point difference is calculated, the test is carried out for 3 times, and the result is averaged;
the test results are shown in the following table:
| ductility at 5 deg.C (cm) | Softening point temperature (. Degree. C.) | Isolation softening Point difference (. Degree. C.) | |
| Example 1 | 30.2 | 84.8 | 0.64 |
| Example 2 | 30.6 | 85.5 | 0.59 |
| Example 3 | 30.4 | 85.1 | 0.63 |
| Example 4 | 30.3 | 84.9 | 0.62 |
| Comparative example 1 | 19.1 | 72.4 | 4.85 |
| Comparative example 2 | 22.7 | 73.6 | 2.68 |
| Comparative example 3 | 24.5 | 78.3 | 1.37 |
Finally, it should be noted that: the above examples are not intended to limit the present invention in any way. Modifications and improvements will readily occur to those skilled in the art upon the basis of the present invention. Accordingly, any modification or improvement made without departing from the spirit of the invention is within the scope of the invention as claimed.
Claims (8)
1. The preparation method of the rubber powder modified asphalt is characterized by comprising the following steps:
(1) Adding the rubber powder into hydrogen peroxide, heating and stirring for reaction, and filtering, washing and drying a reaction product after the reaction is completed to obtain pretreated rubber powder;
(2) Dispersing the pretreated rubber powder in deionized water, then adding tridecafluorooctyl triethoxysilane, stirring for reaction, and after the reaction is completed, filtering, washing and drying the reaction product to obtain modified rubber powder;
(3) Dissolving alkali lignin in deionized water, regulating the pH of the solution to 10-12, adding carbon disulfide to react, centrifuging, washing, and freeze-drying to obtain modified lignin after the reaction is completed;
(4) Adding asphalt into a premixing tank, stirring and heating to 170-180 ℃, maintaining the temperature unchanged, adding modified rubber powder, stirring and mixing uniformly, adding coal tar, continuously stirring and mixing uniformly to obtain a premix, adding the premix into a preparation tank, uniformly refining for 20-30min at 180-200 ℃, adding modified lignin, firstly shearing for 10-20min at a shearing rate of 1000-1500r/min, then shearing for 30-60min at a shearing rate of 3000-4000r/min, and obtaining rubber powder modified asphalt after shearing is finished;
in the step (4), the mass ratio of the asphalt to the modified rubber powder to the coal tar to the modified lignin is 100:25-30:2-4:8-12.
2. The preparation method according to claim 1, wherein in the step (1), the mass ratio of the rubber powder to the hydrogen peroxide is 20-30:100, and the mass fraction of the hydrogen peroxide is 20-30%.
3. The process according to claim 1, wherein in the step (1), the temperature of the heating and stirring reaction is 60 to 80℃and the time of the heating and stirring reaction is 2 to 3 hours.
4. The method according to claim 1, wherein in the step (2), the mass ratio of the pretreated rubber powder, deionized water and tridecafluorooctyltriethoxysilane is 10-20:100:2-4.
5. The process according to claim 1, wherein in the step (2), the temperature of the stirring reaction is 40 to 60℃and the time of the stirring reaction is 3 to 5 hours.
6. The method according to claim 1, wherein in the step (3), the mass ratio of the alkali lignin to the carbon disulfide is 10-15:2-4.
7. The process according to claim 1, wherein in step (3), the reaction temperature is 30 to 40℃and the reaction time is 3 to 4 hours.
8. The rubber powder modified asphalt prepared by the preparation method according to any one of claims 1 to 7.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5704971A (en) * | 1997-03-04 | 1998-01-06 | Memon; Mohammed | Homogeneous crumb rubber modified asphalt |
| CN101580639B (en) * | 2008-05-14 | 2011-04-06 | 中国石油化工股份有限公司抚顺石油化工研究院 | Lignin modified asphalt composition and preparation method thereof |
| CN103205131B (en) * | 2013-04-24 | 2015-01-14 | 广西交通科学研究院 | Chemical modified rubber asphalt with stable performance and preparation method thereof |
| CN106189299A (en) * | 2016-08-25 | 2016-12-07 | 仇颖超 | A kind of preparation method of appts of modified asphalt by utilizing waste tyre rubber powder |
| CN106861645A (en) * | 2017-03-14 | 2017-06-20 | 南京林业大学 | A kind of preparation method of the thio strong oil absorption material of aminated lignin base |
| CN107201047A (en) * | 2017-06-06 | 2017-09-26 | 安徽圣源橡塑科技有限公司 | A kind of activated waste rubber powder modified asphalt material |
| CN112724692A (en) * | 2020-12-17 | 2021-04-30 | 华运通达(广东)道路科技有限公司 | Modified asphalt using lignin and preparation method thereof |
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