CN118063798A - Pretreatment rubber powder based on supercritical fluid induced swelling, rubber powder modified asphalt and preparation method thereof - Google Patents
Pretreatment rubber powder based on supercritical fluid induced swelling, rubber powder modified asphalt and preparation method thereof Download PDFInfo
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- CN118063798A CN118063798A CN202410269029.3A CN202410269029A CN118063798A CN 118063798 A CN118063798 A CN 118063798A CN 202410269029 A CN202410269029 A CN 202410269029A CN 118063798 A CN118063798 A CN 118063798A
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- 239000000843 powder Substances 0.000 title claims abstract description 106
- 229920001971 elastomer Polymers 0.000 title claims abstract description 101
- 239000010426 asphalt Substances 0.000 title claims abstract description 80
- 230000008961 swelling Effects 0.000 title claims abstract description 52
- 239000012530 fluid Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 20
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 11
- 235000011089 carbon dioxide Nutrition 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000010920 waste tyre Substances 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 8
- 238000010276 construction Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000010907 mechanical stirring Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 9
- 239000003607 modifier Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000002522 swelling effect Effects 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Dispersion Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a pretreatment rubber powder based on supercritical fluid induced swelling, rubber powder modified asphalt and a preparation method thereof. The preparation method of the rubber powder comprises the following steps: sequentially placing rubber powder and solid carbon dioxide in a sealed high-pressure reaction kettle; heating and pressurizing the carbon dioxide in the high-pressure reaction kettle to reach a supercritical state; and (3) carrying out a swelling reaction to obtain the supercritical swelling pretreatment rubber powder. The supercritical swelling pretreatment rubber powder is mixed into the matrix asphalt preheated to flow state, so that the supercritical swelling pretreatment rubber powder and the matrix asphalt are fully and interactively mixed under the action of high-speed mechanical stirring, and the supercritical swelling pretreatment rubber powder modified asphalt is prepared. The invention obviously improves the efficiency and uniformity of the rubber powder swelling pretreatment process, and enhances the compatibility between the waste tire rubber powder and the matrix asphalt, thereby improving the storage stability, construction workability and environmental friendliness of the rubber powder modified asphalt.
Description
Technical Field
The invention belongs to road rubber powder, asphalt and a preparation method thereof, and particularly relates to a supercritical fluid induced swelling-based pretreated rubber powder, rubber powder modified asphalt and a preparation method thereof.
Background
Reasonable recycling is carried out on the waste tire rubber, so that the problem of environmental pollution caused by the waste tire rubber can be effectively solved, the defect of insufficient natural rubber resources can be overcome, and the sustainable development of the rubber industry is promoted. At present, rubber powder modified asphalt (also called rubber asphalt) prepared by using waste tire rubber particles (namely waste tire rubber powder) as a modifier is widely applied to high-grade asphalt pavement construction. However, the rubber powder modified asphalt prepared by the conventional wet method has the following problems in practical engineering: (1) The compatibility of the rubber powder modifier and the matrix asphalt is poor, and the rubber powder modifier and the matrix asphalt are easy to separate, so that the storage stability of the rubber powder modified asphalt is poor; (2) The viscosity of the rubber powder modified asphalt is high, so that the construction workability is poor, and the high mixing amount of the rubber powder modifier cannot be realized; (3) The high viscosity characteristic of the rubber powder modified asphalt further leads to higher construction temperature, and a large amount of smoke is released in the stirring, paving and rolling processes of asphalt pavement construction, so that the environment friendliness is poor.
An effective way to solve this problem is to pretreat the powder to purposefully alter the chemical and/or physical properties of the powder and thereby enhance its chemical reactivity with the asphalt matrix. To date, the mainstream gum pretreatment technology can be divided into two major categories, surface activation and internal decrosslinking (desulfurization): (1) surface activation: the surface activity of vulcanized rubber powder is improved or restored by means of pre-reaction (pre-swelling or pre-degradation by using asphalt light component analogues), oxidation, grafting, polymer coating, solution soaking, plasma treatment, gamma ray treatment and the like; (2) internal decrosslinking: the crosslinking bond inside the vulcanized rubber powder is selectively broken under the condition of not affecting the main chain of the rubber powder polymer by using physical radiation means, mechanical means, biological means and chemical means.
In the above-mentioned various rubber powder pretreatment methods, the pre-swelling technology has a great development prospect. However, the existing means cannot well achieve the purpose of carrying out high-efficiency pre-swelling pretreatment on the waste tire rubber powder, and particularly, most of the situations need to rely on the use of additional asphalt light component analogues, so that the pretreated rubber powder still has a plurality of inherent defects when being used as an asphalt modifier for preparing the modified asphalt for roads.
Considering that the existing pretreatment means cannot well achieve the limitation of swelling effect on the waste tire rubber powder (used as a road asphalt modifier), new means are needed to be considered.
Disclosure of Invention
The invention aims to: the invention aims to provide high-efficiency pretreatment rubber powder and rubber powder modified asphalt based on supercritical fluid induced swelling and a preparation method thereof, so as to obtain rubber powder and asphalt with better performance.
The invention introduces supercritical fluid technology as a new means for pretreatment of the rubber powder modifier. Supercritical fluids have both gas permeability and liquid solubility. Therefore, the supercritical fluid is an ideal swelling reaction medium for the rubber powder, and can induce and realize the efficient swelling pretreatment of the rubber powder.
The technical scheme is as follows: the first aspect of the invention provides a preparation method of pretreatment rubber powder based on supercritical fluid induced swelling, comprising the following steps:
(1) Sequentially placing rubber powder and solid carbon dioxide in a sealed high-pressure reaction kettle;
(2) Heating and pressurizing the carbon dioxide in the high-pressure reaction kettle to reach a supercritical state;
(3) And (3) carrying out a swelling reaction to obtain the supercritical swelling pretreatment rubber powder.
Further, the mass ratio of the rubber powder to the solid carbon dioxide in the step (1) is 15:10-15:20.
Further, in the step (2), the density of the supercritical carbon dioxide is more than or equal to 0.16g/cm 3, the temperature is more than or equal to 200 ℃, and the pressure is more than or equal to 8MPa.
Further, in the step (2), the density of the supercritical carbon dioxide is 0.166g/cm 3, the temperature is 205 ℃, and the pressure is 10MPa.
Further, in the step (2), the temperature rising rate of the carbon dioxide in the high-pressure reaction kettle is more than or equal to 5 ℃/min.
Further, in the step (1), the solid carbon dioxide is dry ice. The purity grade of the dry ice is up to food grade, and the purity is higher than 99.99%.
The invention also provides the rubber powder prepared by the method.
The third aspect of the invention provides a preparation method of the rubber powder modified asphalt, wherein the rubber powder after treatment is mixed with the matrix asphalt after the preheating treatment, and the mixture is mixed and dissolved to obtain the supercritical swelling pretreatment rubber powder modified asphalt.
Further, the temperature of the matrix asphalt after the preheating treatment is 160-165 ℃, and the preheating time is more than or equal to 2 hours; alternatively, the mass ratio of the treated gum powder to the pre-heat treated base asphalt is 15:85 to 40:60, e.g., 1:3. Or the rubber powder is rubber particles prepared by crushing junked tires at normal temperature or low temperature, and the particle size range is 30 meshes to 80 meshes.
The fourth aspect of the invention provides asphalt prepared by the method.
Compared with the prior art, the invention has the following characteristics:
1. compared with the common rubber powder, the supercritical swelling pretreatment rubber powder prepared by the invention has the advantages that the surface is rougher, and the internal crosslinking structure is also fluffy. When the modified asphalt is used as an asphalt modifier, the compatibility between the waste tire rubber powder and the matrix asphalt can be effectively enhanced by the characteristics, the ultra-high mixing amount application (up to 40% of the inside mixing amount) of the rubber powder in the modified asphalt for road use is realized, and the recycling rate of the waste tires in the field of road engineering is further improved.
2. Compared with the common rubber powder modified asphalt, the supercritical swelling pretreatment rubber powder modified asphalt prepared by the invention has obviously improved storage stability, low-temperature flexibility, ageing resistance and fatigue resistance, and reduced viscosity, and is beneficial to reducing the emission of high-temperature asphalt smoke. The characteristics can relieve the problem that the application of the rubber powder modified asphalt in actual engineering is limited.
3. The invention obviously improves the efficiency and uniformity of the rubber powder swelling pretreatment process, thereby improving the storage stability, construction workability and environmental friendliness of the rubber powder modified asphalt.
4. The preparation method of the supercritical swelling pretreatment rubber powder and the rubber powder modified asphalt has the characteristics of simple process, obvious effect and controllable process, and all required equipment is industrial equipment with mature technology, so that the preparation method has the prospect of mass production.
Drawings
FIG. 1 is a comparison of the microscopic morphology of a gum surface, wherein a) untreated gum, b) supercritical swelling pre-treated gum.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be further described below.
Example 1:
150g of waste truck tire rubber powder (30 mesh) was put into a high-pressure reaction kettle. 160g of food-grade dry ice was poured into the kettle and the kettle lid was quickly closed to tighten the screws. And sublimating the dry ice in the kettle into carbon dioxide by adopting external electric heating, and gradually heating and pressurizing to reach a supercritical carbon dioxide fluid state, wherein the heating rate is 5 ℃/min. The supercritical carbon dioxide is prepared in a supercritical carbon dioxide environment at 205 ℃, under the pressure of 10MPa, with the density of 0.166g/cm 3, the stirring speed of a magnetic sealing stirring paddle of 300rpm and the duration of the swelling reaction of 2 hours. The sol amount of the prepared supercritical swelling pretreatment rubber powder is 7.1%, the gel crosslinking density is 8.1 x 10 -5mol/cm3, and meanwhile, the volume of rubber powder particles is enlarged due to the swelling effect, and the surface is rough and fluffy.
Example 2
100G of the supercritical swelling pretreatment rubber powder (30 meshes) prepared by the method of reference example 1 was mixed into 300g of Beijing bo 70 # petroleum base asphalt preheated to 165 ℃ and stirred continuously for 45min under the conditions of a stirring temperature of 175 ℃ and a stirring speed of 1000rpm, to prepare a conventional mixing amount (internal mixing 25%) of the supercritical swelling pretreatment rubber powder modified asphalt. The performance test results of the conventional mixing amount supercritical swelling pretreatment rubber powder modified asphalt are shown in table 1, and each performance of the conventional mixing amount supercritical swelling pretreatment rubber powder modified asphalt can meet the requirements of the modified asphalt for road use.
TABLE 1 Performance test results of conventional blend supercritical swelling pretreatment rubber powder modified asphalt
Example 3:
160g of the supercritical swelling pretreatment rubber powder (30 meshes) prepared by the method of reference example 1 was mixed into 240g of petroleum base asphalt of Beijing bo 70 # which had been preheated to 165 ℃ and stirred continuously for 45min under the conditions of a stirring temperature of 175 ℃ and a stirring rate of 1000rpm, to prepare a high-mixing amount (internal mixing 40%) of supercritical swelling pretreatment rubber powder modified asphalt. The performance test results of the prepared high-mixing-amount supercritical swelling pretreatment rubber powder modified asphalt are shown in table 2, and each performance of the prepared high-mixing-amount supercritical swelling pretreatment rubber powder modified asphalt can meet the requirements of the modified asphalt for road use.
TABLE 2 Performance test results of high blend supercritical swelling pretreatment rubber powder modified asphalt
Comparative example 1:
The difference from example 1 is that: the observation of the surface microtopography was carried out using only untreated ordinary scrap truck tire powder (30 mesh) and compared with example 1, the results are shown in fig. 1.
Comparative example 2:
The difference from example 2 is that: 100g of common rubber powder (30 meshes) is mixed into 300g of Beijing bo 70 # petroleum base asphalt preheated to 165 ℃, and the mixture is continuously stirred for 45min under the conditions of the stirring temperature of 175 ℃ and the stirring speed of 1000rpm, so that the common rubber powder modified asphalt with 25% of the mixed mixture is prepared. According to the test specification of highway engineering asphalt and asphalt mixture (JTG E20-2011), a polymer modified asphalt segregation test method is adopted, and the storage stability of the supercritical swelling pretreatment rubber powder modified asphalt and the storage stability of the common rubber powder modified asphalt are respectively compared by taking the difference of softening points and segregation rate as evaluation indexes. As shown in Table 3, the segregation degree of the common rubber powder modified asphalt is remarkably higher, and compared with the supercritical swelling pretreatment rubber powder modified asphalt, the common rubber powder modified asphalt has more excellent storage stability. And secondly, the rotational viscosity of the supercritical swelling pretreatment rubber powder modified asphalt at 135 ℃ measured at the same temperature is far smaller than that of the common rubber powder modified asphalt, so that the supercritical swelling pretreatment rubber powder modified asphalt is easier to pump and spread, and compared with the common rubber powder modified asphalt, the supercritical swelling pretreatment rubber powder modified asphalt has more excellent construction workability.
TABLE 3 results of comparison of storage stability of supercritical swelling pretreatment rubber powder modified asphalt and ordinary rubber powder modified asphalt
The foregoing is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any person skilled in the art will make any equivalent substitution or modification to the technical solution and technical content disclosed in the invention without departing from the scope of the technical solution of the invention, and the technical solution of the invention is not departing from the scope of the invention.
Claims (10)
1. A preparation method of pretreatment rubber powder based on supercritical fluid induced swelling is characterized by comprising the following steps: the method comprises the following steps:
(1) Sequentially placing rubber powder and solid carbon dioxide in a sealed high-pressure reaction kettle;
(2) Heating and pressurizing the carbon dioxide in the high-pressure reaction kettle to reach a supercritical state;
(3) And (3) carrying out a swelling reaction to obtain the supercritical swelling pretreatment rubber powder.
2. The method for preparing the pretreatment rubber powder based on supercritical fluid induced swelling according to claim 1, wherein the method comprises the following steps: the mass ratio of the rubber powder to the solid carbon dioxide in the step (1) is 15:10-15:20.
3. The method for preparing the pretreatment rubber powder based on supercritical fluid induced swelling according to claim 1, wherein the method comprises the following steps: in the step (2), the density of the supercritical carbon dioxide is more than or equal to 0.16g/cm 3, the temperature is more than or equal to 200 ℃, and the pressure is more than or equal to 8MPa.
4. A method for preparing a pre-treated gum powder based on supercritical fluid induced swelling according to claim 3, wherein: in the step (2), the density of the supercritical carbon dioxide is 0.166g/em 3, the temperature is 205 ℃, and the pressure is 10MPa.
5. A method for preparing a pre-treated gum powder based on supercritical fluid induced swelling according to claim 3, wherein: in the step (2), the temperature rising rate of the carbon dioxide in the high-pressure reaction kettle is more than or equal to 5 ℃/min.
6. A method for preparing a pre-treated gum powder based on supercritical fluid induced swelling according to claim 3, wherein: in the step (1), the solid carbon dioxide is dry ice.
7. A gum powder prepared by the method of any one of claims 1-6.
8. A preparation method of rubber powder modified asphalt is characterized by comprising the following steps: blending the rubber powder treated by any one of claims 1-6 into the preheated matrix asphalt, and mixing to obtain the supercritical swelling pretreatment rubber powder modified asphalt.
9. The method for preparing the rubber powder modified asphalt according to claim 8, wherein the method comprises the following steps: the temperature of the matrix asphalt after the preheating treatment is 160-165 ℃, and the preheating time is more than or equal to 2 hours; alternatively, the mass ratio of the treated gum powder to the pre-heat treated base asphalt is 15:85 to 40:60, e.g., 1:3.
10. Asphalt prepared by the method of any one of claims 8-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410269029.3A CN118063798A (en) | 2024-03-08 | 2024-03-08 | Pretreatment rubber powder based on supercritical fluid induced swelling, rubber powder modified asphalt and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410269029.3A CN118063798A (en) | 2024-03-08 | 2024-03-08 | Pretreatment rubber powder based on supercritical fluid induced swelling, rubber powder modified asphalt and preparation method thereof |
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| Publication Number | Publication Date |
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| CN118063798A true CN118063798A (en) | 2024-05-24 |
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| CN202410269029.3A Pending CN118063798A (en) | 2024-03-08 | 2024-03-08 | Pretreatment rubber powder based on supercritical fluid induced swelling, rubber powder modified asphalt and preparation method thereof |
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| CN (1) | CN118063798A (en) |
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- 2024-03-08 CN CN202410269029.3A patent/CN118063798A/en active Pending
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