CN111909529A - Desulfurized waste tire rubber powder crosslinked modified asphalt and preparation method thereof - Google Patents
Desulfurized waste tire rubber powder crosslinked modified asphalt and preparation method thereof Download PDFInfo
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- CN111909529A CN111909529A CN202010520712.1A CN202010520712A CN111909529A CN 111909529 A CN111909529 A CN 111909529A CN 202010520712 A CN202010520712 A CN 202010520712A CN 111909529 A CN111909529 A CN 111909529A
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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
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2319/00—Characterised by the use of rubbers not provided for in groups C08J2307/00 - C08J2317/00
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a desulfurized waste tire rubber powder cross-linked modified asphalt and a preparation method thereof, wherein a swelling agent is used for swelling rubber powder, a three-dimensional cross-linked network of rubber macromolecules is expanded, and the swelling stress is favorable for promoting the fracture of cross-linked bonds in the rubber powder; the surface and the inside of the rubber powder have rich pore structures, the contact area of ammonia and the rubber powder is increased, the microwave treatment is combined to activate S-S bonds and S-C bonds in the waste tires, the consistency of the desulfurization degree of the inside and the outside of rubber powder particles is ensured, a macromolecular chain segment structure is formed, the rubber powder particles and the activated rubber powder are promoted to form a cross-linked network, and a chemical cross-linked reticular structure is formed between the active group of the desulfurization rubber powder chain segment and an asphalt base material, so that the stability of the rubber powder modified asphalt is improved, and the problem of the stripping property of a rubber powder-asphalt mixture is solved.
Description
Technical Field
The invention relates to the technical field of tire rubber powder recycling, in particular to desulfurized waste tire rubber powder crosslinked modified asphalt and a preparation method thereof.
Background
Along with the improvement of the living standard of substances of people, the using amount of automobiles is increased year by year, meanwhile, the scrappage of the automobiles is increased year by year, corresponding waste tires are also generated in large quantity, a large number of researchers recycle the waste tires to produce rubber powder or recycle the waste tires to produce fuel oil or carbon black, but because a large amount of sulfur components are remained in the waste tires, the sulfur components in the waste tires need to be removed in the preparation process of the rubber powder or the carbon black, so that the performance of the product and the quality of the product can meet the requirements, and the reuse and the expanded application of the prepared rubber powder or carbon black product in the chemical field can be promoted.
The prior art for producing the waste tire rubber powder modified asphalt at home and abroad comprises the following steps: directly putting the waste tire rubber powder with the fineness of more than 30 meshes into hot asphalt with the temperature of 160-180 ℃ according to the proportion of 10-20% of the weight of the asphalt, premixing and stirring, dynamically shearing and grinding the asphalt rubber powder mixture, and then mixing, reacting and developing the sheared and ground asphalt rubber powder mixture to form a product.
The rubber powder is a material containing a cross-linking structure and composed of rubber, carbon black and the like. The rubber powder has low surface activity, and when the rubber powder is added into a matrix material, the interaction force between the rubber powder and the matrix material is weak, so that the performance of the material is reduced. The interface binding capacity between the rubber powder and the asphalt is poor, the rubber powder and the asphalt have the phenomenon of uneven distribution in stirring dispersion and high-temperature movement, and the rubber powder does not react with the asphalt basically or only reacts weakly, so-called reaction is just the combination between the rubber powder of the waste tire and the asphalt by hydrogen bonds and intermolecular acting force, the acting force is weak and is a metastable mixture, and therefore, the rubber powder and the asphalt tend to separate, converge and reduce the surface energy.
Disclosure of Invention
The invention aims to provide a method for modifying asphalt by crosslinking desulfurized waste tire rubber powder, which changes the performance of tire rubber powder, improves the crosslinking performance between the rubber powder and an asphalt base material, forms a crosslinking network and improves the performance of the modified asphalt.
The invention is realized by adopting the following technical scheme:
a method for desulfurizing waste tire rubber powder cross-linking modified asphalt specifically comprises the following steps:
(1) crushing waste tire rubber into rubber powder particles of 100-200 meshes, removing impurities, placing the rubber powder particles in a desulfurization tank, adding a rubber swelling agent into the desulfurization tank, starting a motor of the desulfurization tank, stirring at a rotating speed of 50-200r/min, stirring for 15-30min, standing for 2-8h, continuing stirring for 15-30min, standing again, and repeatedly performing stirring-standing operation for 3-5 times;
(2) after the swelling agent of the swelled rubber powder is drained, the rubber powder is directly subjected to freeze drying treatment to obtain dried low-temperature frozen rubber powder;
(3) grinding in a grinder, sieving with a 50-80 mesh sieve, placing the powder in a circulating fluidized bed processor, introducing ammonia gas from the bottom of the circulating fluidized bed processor, and recovering the rubber powder particles which do not meet the conditions after sieving;
(4) starting a microwave generator arranged on the circulating fluidized bed processor, wherein the microwave frequency is 2450Hz, adjusting the radiation power of the microwave generator to 800-;
(5) carrying out ultrasonic activation treatment on the unqualified rubber powder sieved in the step (3);
(6) placing the desulfurized rubber powder and the rubber powder activated in the step (5) into a screw extruder, adding a modifier, and performing multi-stage extrusion blending to obtain composite rubber powder;
(7) adding the composite rubber powder into the molten asphalt, mixing, shearing for 30-90min at the temperature of 160-200 ℃ by using a shearing emulsifying machine, standing and developing for 0.5-3h at the temperature of 150-180 ℃, and cooling to obtain the composite rubber powder modified asphalt.
Further, the rubber swelling agent is an organic solvent, and n-heptane, n-octane, cyclohexane, toluene, xylene, ethyl acetate, dibutyl phthalate or dimethyl sulfoxide is selected.
Furthermore, the mass ratio of the rubber particles to the rubber swelling agent in the step (1) is (0.8-1.5): 1, and mixing.
Further, the ammonia gas introducing speed in the step (3) is 0.7-1.3cm3Min-kg, the time of introducing is 30-50 min.
Further, in the step (5), ultrasonic activation treatment is carried out at 40-60 ℃, the ultrasonic power is 200-500W, and the treatment time is 2-5 h.
Further, in the step (6), the modifier is one or more of sulfur powder, an accelerator MBT, an accelerator TMTD and a metal oxide.
Further, the mass ratio of the rubber powder after desulfurization to the rubber powder after activation in the step (6) is (1.2-2.5): 1.
Further, the mass ratio of the composite rubber powder to the asphalt in the step (7) is (0.1-0.2): 1.
the invention also aims to provide a rubber powder modified asphalt composite material prepared by the method for crosslinking and modifying asphalt by using the desulfurized waste tire rubber powder.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the swelling agent is used for swelling the coarse-grained rubber powder, so that the waste tire rubber particles are expanded, the three-dimensional crosslinked network of rubber macromolecules is expanded, and the stress effect generated by swelling is favorable for promoting the fracture of the crosslinked bonds in the rubber powder; and then the rubber powder with rich pore structures on the surface and inside is obtained through low-temperature cooling treatment, so that ammonia gas can be uniformly diffused in the rubber powder, the contact area of the ammonia gas and the rubber powder is increased, S-S bonds and S-C bonds in the waste tire are activated by combining microwave treatment, the consistent desulfurization degree of the inside and the outside of rubber powder particles is ensured, sulfur cross-linking bonds in the rubber powder are broken, a macromolecular chain segment structure containing a large number of active group sites is formed, and the cross-linking activity of the rubber powder is improved.
2. The large-particle rubber powder after freezing and crushing and the fine rubber powder after desulfurization are subjected to multi-stage extrusion blending, active sites on the surface of the rubber powder are improved through ultrasonic activation treatment, the active sites and desulfurization rubber powder chain segments with more active group sites are promoted to form a cross-linking network, active groups of the desulfurization rubber powder chain segments are taken as cross-linking sites, a chemical cross-linking net structure is formed between the active groups and an asphalt base material, the stability of rubber powder modified asphalt is improved, and the problem of the stripping performance of a rubber powder-asphalt mixture is solved.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
Example 1
A method for desulfurizing waste tire rubber powder cross-linking modified asphalt specifically comprises the following steps:
(1) crushing the waste tire rubber into rubber powder particles of 100-200 meshes, removing impurities, placing the rubber powder particles into a desulfurization tank, adding dimethylbenzene into the desulfurization tank, starting a motor of the desulfurization tank, stirring at the rotating speed of 800r/min, stirring for 30min, standing for 4h, continuing stirring for 30min, standing again, and repeatedly performing stirring-standing operation for 3-5 times;
wherein the mass ratio of the rubber particles to the dimethylbenzene is 1.2: 1, and mixing.
(2) After the swelling agent of the swelled rubber powder is drained, the rubber powder is directly subjected to freeze drying treatment to obtain dried low-temperature frozen rubber powder;
(3) grinding in a grinder, sieving with a 50-80 mesh sieve, placing the powder in a circulating fluidized bed processor, introducing ammonia gas from the bottom of the circulating fluidized bed processor, and recovering the rubber powder particles which do not meet the conditions after sieving;
wherein the ammonia gas is introduced at a speed of 1.0cm3Min-kg, the aeration time is 30 min.
(4) Starting a microwave generator arranged on the circulating fluidized bed processor, wherein the microwave frequency is 2450Hz, adjusting the radiation power of the microwave generator to 800W, and continuously radiating for 30min under the power to obtain the rubber powder after desulfurization treatment;
(5) carrying out ultrasonic activation treatment on the unqualified rubber powder sieved in the step (3), wherein the temperature is 60 ℃, the ultrasonic power is 500W, and the treatment time is 3 h;
(6) mixing the desulfurized rubber powder and the rubber powder activated in the step (5) according to the ratio of 2: 1, placing the mixture in a screw extruder, adding an accelerator MBT, and performing multi-stage extrusion blending to obtain composite rubber powder;
(7) adding the composite rubber powder accounting for 15 percent of the mass of the asphalt into the molten asphalt, mixing, shearing for 60min at the temperature of 180 ℃ by using a shearing emulsifying machine, standing and developing for 2h at the temperature of 160 ℃, and cooling to obtain the composite rubber powder modified asphalt.
Example 2
A method for desulfurizing waste tire rubber powder cross-linking modified asphalt specifically comprises the following steps:
(1) crushing the waste tire rubber into rubber powder particles of 100-200 meshes, removing impurities, placing the rubber powder particles into a desulfurization tank, adding dimethyl sulfoxide into the tank, starting a motor of the desulfurization tank, stirring at the rotating speed of 800r/min, stirring for 30min, standing for 4h, continuing stirring for 30min, standing again, and repeatedly performing stirring-standing operation for 3-5 times;
wherein the mass ratio of the rubber particles to the dimethyl sulfoxide is 1.5: 1, and mixing.
(2) After the dimethyl sulfoxide of the swollen rubber powder is leached, the rubber powder is directly subjected to freeze drying treatment to obtain dried low-temperature frozen rubber powder;
(3) grinding in a grinder, sieving with a 50-80 mesh sieve, placing the powder in a circulating fluidized bed processor, introducing ammonia gas from the bottom of the circulating fluidized bed processor, and recovering the rubber powder particles which do not meet the conditions after sieving;
wherein the ammonia gas is introduced at a rate of 1.0cm 3/min-kg for 30 min.
(4) Starting a microwave generator arranged on the circulating fluidized bed processor, wherein the microwave frequency is 2450Hz, adjusting the radiation power of the microwave generator to 800W, and continuously radiating for 30min under the power to obtain the rubber powder after desulfurization treatment;
(5) carrying out ultrasonic activation treatment on the unqualified rubber powder sieved in the step (3), wherein the temperature is 60 ℃, the ultrasonic power is 500W, and the treatment time is 3 h;
(6) mixing the desulfurized rubber powder and the rubber powder activated in the step (5) according to the weight ratio of 1.5: 1, placing the mixture in a screw extruder, adding an accelerator MBT, and performing multi-stage extrusion blending to obtain composite rubber powder;
(7) adding the composite rubber powder accounting for 10 percent of the mass of the asphalt into the molten asphalt, mixing, shearing for 60min at the temperature of 180 ℃ by using a shearing emulsifying machine, standing and developing for 2h at the temperature of 160 ℃, and cooling to obtain the composite rubber powder modified asphalt.
Example 3 Performance testing
Control group: crushing rubber powder of a waste tire to 50-80 meshes, desulfurizing, and mixing the rubber powder and asphalt according to the weight ratio of 0.15: the mass ratio of 1 is directly mixed with asphalt in a shearing way, and the mixture is subjected to standing development treatment, and the treatment process is the same as that of the example 1, so that the rubber powder modified asphalt material is obtained.
The performance tests of the crumb rubber modified asphalt prepared in examples 1 and 2 and the control group were carried out according to the standard of road engineering asphalt and asphalt mixture test protocol (JTG E20-2001) of the Ministry of transportation, and the test results are as follows:
| soft dead Point (. degree. C.) | Segregation softening point Difference (. degree. C.) | |
| Example 1 | 68.4 | 0.9 |
| Example 2 | 67.8 | 1.1 |
| Control group | 53.4 | 4.6 |
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications, which have the same properties or uses, should be considered as falling within the scope of the present invention without departing from the spirit of the invention.
Claims (9)
1. The method for modifying the asphalt by crosslinking the desulfurized waste tire rubber powder is characterized by comprising the following steps:
(1) crushing waste tire rubber into rubber powder particles of 100-200 meshes, removing impurities, placing the rubber powder particles in a desulfurization tank, adding a rubber swelling agent into the desulfurization tank, starting a motor of the desulfurization tank, stirring at a rotating speed of 50-200r/min, stirring for 15-30min, standing for 2-8h, continuing stirring for 15-30min, standing again, and repeatedly performing stirring-standing operation for 3-5 times;
(2) after the swelling agent of the swelled rubber powder is drained, the rubber powder is directly subjected to freeze drying treatment to obtain dried low-temperature frozen rubber powder;
(3) grinding in a grinder, sieving with a 50-80 mesh sieve, placing the powder in a circulating fluidized bed processor, introducing ammonia gas from the bottom of the circulating fluidized bed processor, and recovering rubber powder particles which do not meet the conditions after sieving;
(4) starting a microwave generator arranged on the circulating fluidized bed processor, wherein the microwave frequency is 2450Hz, adjusting the radiation power of the microwave generator to 800-900W, and continuously radiating for 15-30min under the power to obtain the rubber powder after desulfurization treatment;
(5) carrying out ultrasonic activation treatment on the unqualified rubber powder sieved in the step (3);
(6) placing the desulfurized rubber powder and the rubber powder activated in the step (5) into a screw extruder, adding a modifier, and performing multi-stage extrusion blending to obtain composite rubber powder;
(7) adding the composite rubber powder into the molten asphalt, mixing, shearing for 30-90min at the temperature of 160-200 ℃ by using a shearing emulsifying machine, standing and developing for 0.5-3h at the temperature of 150-180 ℃, and cooling to obtain the composite rubber powder modified asphalt.
2. The method for cross-linking and modifying asphalt by using desulfurized waste tire rubber powder according to claim 1, wherein the rubber swelling agent is an organic solvent, and n-heptane, n-octane, cyclohexane, toluene, xylene, ethyl acetate, dibutyl phthalate or dimethyl sulfoxide is selected.
3. The method for cross-linking and modifying asphalt by using desulfurized waste tire rubber powder as claimed in claim 1 or 2, wherein the mass ratio of the rubber particles to the rubber swelling agent in step (1) is (0.8-1.5): 1, and mixing.
4. The method for desulfurizing asphalt crosslinked with junked tire rubber powder according to claim 1, wherein the ammonia gas is introduced at a speed of 0.7-1.3cm in step (3)3Min-kg, the time of introducing is 30-50 min.
5. The method for cross-linking modified asphalt by desulfurized waste tire rubber powder as recited in claim 1, wherein the ultrasonic activation treatment in step (5) is carried out at 40-60 ℃, the ultrasonic power is 200-500W, and the treatment time is 2-5 h.
6. The method for cross-linking and modifying asphalt by using desulfurized waste tire rubber powder according to claim 1, wherein the modifier in the step (6) is one or more of sulfur powder, accelerator MBT, accelerator TMTD and metal oxide.
7. The method for cross-linking and modifying asphalt by using desulfurized waste tire rubber powder according to claim 1, wherein the mass ratio of the desulfurized rubber powder to the activated rubber powder in the step (6) is (1.2-2.5): 1.
8. the method for cross-linking and modifying asphalt by using desulfurized waste tire rubber powder as claimed in claim 1, wherein the mass ratio of the composite rubber powder to the asphalt in the step (7) is (0.1-0.2): 1.
9. a composite material prepared by using the method for cross-linking the modified asphalt by the desulfurized waste tire rubber powder according to any one of claims 1 to 8.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121873A (en) * | 2021-05-06 | 2021-07-16 | 益路恒丰衡水沥青科技有限公司 | Rubber asphalt production equipment based on activated rubber powder |
| CN113211691A (en) * | 2021-05-08 | 2021-08-06 | 益路恒丰衡水沥青科技有限公司 | Rubber asphalt production method based on microwave heating |
| CN113232212A (en) * | 2021-05-08 | 2021-08-10 | 益路恒丰衡水沥青科技有限公司 | Rubber asphalt production equipment based on microwave heating |
| CN113736137A (en) * | 2021-09-27 | 2021-12-03 | 益路恒丰衡水沥青科技有限公司 | Rubber powder desulfurization equipment for rubber asphalt production |
| CN117720321A (en) * | 2023-11-30 | 2024-03-19 | 山东高速工程建设集团有限公司 | Modified rubber reclaimed asphalt mixture and preparation method thereof |
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| CN105504840A (en) * | 2016-01-04 | 2016-04-20 | 北京东方雨虹防水技术股份有限公司 | Preparing method for low-temperature modified asphalt for roads |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121873A (en) * | 2021-05-06 | 2021-07-16 | 益路恒丰衡水沥青科技有限公司 | Rubber asphalt production equipment based on activated rubber powder |
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| CN113736137A (en) * | 2021-09-27 | 2021-12-03 | 益路恒丰衡水沥青科技有限公司 | Rubber powder desulfurization equipment for rubber asphalt production |
| CN113736137B (en) * | 2021-09-27 | 2023-07-25 | 益路恒丰衡水沥青科技有限公司 | Rubber powder desulfurization equipment for rubber asphalt production |
| CN117720321A (en) * | 2023-11-30 | 2024-03-19 | 山东高速工程建设集团有限公司 | Modified rubber reclaimed asphalt mixture and preparation method thereof |
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Application publication date: 20201110 |