NL2026510A - Method for preparing capsules with attapulgite/calcium alginate composite wall for asphalt self-healing - Google Patents
Method for preparing capsules with attapulgite/calcium alginate composite wall for asphalt self-healing Download PDFInfo
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- NL2026510A NL2026510A NL2026510A NL2026510A NL2026510A NL 2026510 A NL2026510 A NL 2026510A NL 2026510 A NL2026510 A NL 2026510A NL 2026510 A NL2026510 A NL 2026510A NL 2026510 A NL2026510 A NL 2026510A
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- asphalt
- attapulgite
- capsules
- healing
- composite wall
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- 239000002775 capsule Substances 0.000 title claims abstract description 69
- 229960000892 attapulgite Drugs 0.000 title claims abstract description 48
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 48
- 239000010426 asphalt Substances 0.000 title claims abstract description 41
- 235000010410 calcium alginate Nutrition 0.000 title claims abstract description 26
- 239000000648 calcium alginate Substances 0.000 title claims abstract description 26
- 229960002681 calcium alginate Drugs 0.000 title claims abstract description 26
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 25
- 239000000661 sodium alginate Substances 0.000 claims abstract description 25
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 7
- 229920000053 polysorbate 80 Polymers 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 4
- 239000007970 homogeneous dispersion Substances 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000004064 recycling Methods 0.000 abstract description 29
- 238000010008 shearing Methods 0.000 abstract description 22
- 230000035876 healing Effects 0.000 abstract description 10
- 238000011068 loading method Methods 0.000 description 7
- 239000011384 asphalt concrete Substances 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 6
- 230000008719 thickening Effects 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 235000019486 Sunflower oil Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000012779 reinforcing material Substances 0.000 description 2
- 239000002600 sunflower oil Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention discloses a method for preparing capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing, including the following steps: preparing an industrial-grade sodium alginate solution; adding attapulgite, and subjecting the resulting mixture to high-speed shearing for even dispersion to give a mixture of sodium alginate and attapulgite; adding an asphaltrecycling agent and a surfactant to the obtained mixture of sodium alginate and attapulgite, and subjecting the resulting mixture to high-speed shearing for even dispersion to give a blend; adding the obtained blend dropwise to a calcium chloride solution, and stirring the resulting mixture to form wet capsules; and filtering out, washing and drying the wet capsules to give capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing. The rod-like channel structure of attapulgite itself provides storage space for the asphaltrecycling agent, which allows the capsules with a composite wall for asphalt self- healing to release a significantly-lower amount of asphalt-recycling agent during drying shrinkage than the capsules with a calcium alginate wall for asphalt selfhealing, and have higher content of asphalt-recycling agent inside, resulting in longer functioning period during service.
Description
TECHNICAL FIELD The present invention belongs to the technical field of materials, and specifically, designs a method for preparing capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing.
BACKGROUND Adding capsules to asphalt concrete to improve the healing performance of the pavement and extend the service life of the pavement has been widely recognized by researchers. The capsule for asphalt self-healing prepared by encapsulating asphalt-recycling agent with calcium alginate can gradually release the asphalt-recycling agent in the chamber due to elastic contraction under the cyclic loading without being broken, which is expected to solve the aging and cracking problem of asphalt pavement. However, the capsule with a calcium alginate wall for asphalt self-healing has disadvantages, such as low strength, early release of the asphalt-recycling agent during the drying shrinkage process, and low encapsulation efficiency of the asphalt-recycling agent, making the capsule hardly meet the requirements of application.
SUMMARY The present invention is intended to provide capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing and a preparation method thereof. The capsule has a controllable strength, releases a very small amount of asphalt-recycling agent during the drying shrinkage process, and can significantly improve the self-healing performance of asphalt concrete under traffic loading.
In order to achieve the above objectives, the following technical solutions are adopted.
The present invention provides a method for preparing capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing, including the following steps: (1) preparing an industrial-grade sodium alginate solution with a concentration of 1 wi% to 8 wt®%; adding attapulgite at an amount 0.5% to 3.5% of the mass of the sodium alginate solution; and subjecting the resulting mixture to high-speed shearing for even dispersion to give a mixture of sodium alginate and attapulgite; {2) adding an asphalt-recycling agent and a surfactant to the obtained mixture of sodium alginate and attapulgite, and subjecting the resulting mixture to high-speed shearing for even dispersion to give a blend, where, the asphalt- recycling agent has a volume accounting for 5% to 30% of the volume of the sodium alginate solution, and the surfactant has a volume accounting for 2% to 8% of the volume of the asphalt-recycling agent; {3) adding the obtained blend dropwise to a 1 wt®% to 3 wt®% calcium chloride solution, and stirring the resulting mixture at 50°C to 55°C for 6 h to 12 h to form wet capsules; and (4) filtering out the wet capsules, then washing the capsules with deionized water, and removing water in the capsules by drying to give capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing.
According to the above solution, the asphalt-recycling agent is a common commercially-available asphalt-recycling agent.
According to the above solution, the surfactant is Tween 80.
According to the above solution, the high-speed shearing for dispersion described in step 2 and step 3 is conducted for 8 min to 15 min at a shearing rate of 2,000 rpm to 5,000 rpm.
According to the above solution, the drying in step (4) is conducted as follows: forced-air drying in an oven at 40°C to 60°C for 4 h to 8 h, or air drying at room temperature for 48 h to 72 h.
Attapulgite is a kind of clay with large reserves in China, low price and availability, which has excellent colloidal properties and can be evenly dispersed in a solution. Attapulgite is a prominent thickening and reinforcing material, and has a microstructure of rod-like channels, which provides space for storing substances.
The capsules with an attapulgite/calcium alginate composite wall for asphalt self- healing prepared in the present invention can avoid the problem of early release of the asphalt-recycling agent, and the strength of the capsules can be independently adjusted by controlling the content of attapulgite. In addition, the present invention can also provide a new way for high-value utilization of attapulgite.
Beneficial effects of the present invention are as follows:
1. Attapulgite, as a thickening material, can increase the viscosity of an industrial-grade sodium alginate solution, and as a reinforcing material, can be used at varying amounts to adjust the strength of capsules, thereby effectively solving the problem that capsules for asphalt self-healing prepared from industrial- grade sodium alginate have low strength and cannot meet the requirements of application.
2. The rod-like channel structure of attapulgite itself provides storage space for the asphalt-recycling agent, which allows the capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing to release a significantly-lower amount of asphalt-recycling agent during drying shrinkage than the capsules with a calcium alginate wall for asphalt self-healing, and have higher content of asphalt-recycling agent inside, resulting in longer functioning period during service.
3. The capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing prepared by the method can enhance the healing performance of asphalt concrete, prolong the service life of a pavement, and save the maintenance cost.
4. Attapulgite, with large output in China, is cheap and easily available, resulting in the reduction of the preparation cost of capsules for asphalt self- healing.
5. The utilization of attapulgite is greatly restricted in China, and the present invention develops a new way for high-value utilization of this mineral.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a schematic diagram for the step of adding the blend dropwise to the calcium chloride solution according to a specific embodiment of the present invention; and FIG. 2 shows the appearance and size (with a diameter of 1 mm to 2 mm) of the capsules prepared in Example 3 of the present invention.
DETAILED DESCRIPTION The technical solution of the present invention is further explained below through examples, but the claimed scope of the present invention is not limited thereto.
Example 1 Four types of capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing were prepared. Four 1.875 wt% industrial-grade sodium alginate solutions were prepared, each of 400 mi; then 0g, 4 g, 8 g and 12 g of attapulgite were added to the above solutions separately, where the attapulgite had a fineness of 325 mesh; and the resulting mixtures were separately subjected to high-speed shearing for 10 min in a shear, with a shearing rate of 4,000 rpm. 40 ml of asphalt-recycling agent and 2 mi of Tween 80 (surfactant) were added to each of the mixtures, and the resulting mixtures were separately subjected to high-speed shearing for 10 min in a shear, with a shearing rate of 4,000 rpm. The obtained mixtures were numbered as A1, A2, A3 and A4 in sequence. Then the viscosity was tested for the four different mixtures using a dynamic shear rheometer. The test was conducted at 25°C and a shearing rate of 0.1 s to 1,000 st. The test result for viscosity was as follows: A1 < A2 < A3 < A4. lt indicates that attapulgite has a thickening effect on the sodium alginate solution. Calcium chloride solutions with a concentration of 2.5 wt% were prepared; then the sheared blends were separately added dropwise to the calcium chloride solutions; and the resulting mixtures reacted for 8 h to form four different types of wet capsules. The wet capsules were air-dried for 72 h at room temperature to give four different types of capsules. The schematic diagram for the step of adding the blend dropwise to the calcium chloride solution is shown in FIG. 1.
As measured, the four types of capsules have compressive strengths of 9.6 N, 11.8 N, 14.3 N and 16.6 N, respectively. It can be seen that the compressive strength of the capsule increases as the content of attapulgite increases.
Thermogravimetric analysis (TGA) test was conducted with reference to the method for measuring the capsule-core content of the self-healing capsule (CN201811140923.1). The results show that the four types of capsules have asphalt-recycling agent contents of 56.3%, 60.1%, 67.3% and 75.1%, respectively.
Asphalt was extracted from a mixed and compacted asphalt mixture for Fourier-transform infrared spectroscopy (FTIR) test. The area was calculated for the absorption peak of C-O at 1,745 cm’ (the characteristic peak for asphalt- recycling agent, where there was no absorption peak for asphalt), and referring to a standard spectrum, the release amount and the release rate were determined for the asphalt-recycling agent in the compacted capsules (see Construction and Building Materials, 2019, 211: 298-307 for specific methods). The results show that the four types of capsules, in the mixed and compacted asphalt mixture, exhibit release rates of 9.1%, 4.2%, 2.3% and 0.4%, respectively.
It is proved that the addition of attapulgite increases the strength of the capsule and the content of asphalt-recycling agent, and reduces the early release of asphalt-recycling agent. 5 Example 2 Two types of capsules with an attapulgite/calcium alginate composite wall for asphalt self-healing were prepared. 400 g of 2.5 wt% sodium alginate solution was prepared, then 16 g (accounting for 4% of the mass of the sodium alginate solution) of attapulgite was added, and the resulting mixture was labelled as A1. 400 g of 1.25 wt% sodium alginate solution was prepared, then 1.5 g (accounting for 0.375% of the mass of the sodium alginate solution) of attapulgite was added, and the resulting mixture was labelled as B1. The resulting mixtures were separately subjected to high-speed shearing for 10 min in a shear, with a shearing rate of 4,000 rpm. 40 mi of sunflower oil (asphalt-recycling agent) and 2 ml of Tween 80 (surfactant) were added to each of the mixtures, and the resulting mixtures were separately subjected to high-speed shearing for 10 min in a shear, with a shearing rate of 4,000 rpm.
The emulsions, made from At and B1 respectively, were separately added dropwise to a calcium chloride solution with a concentration of 2 wt%, and it was found that the emulsion made from B1 was unable to form capsules due to its too-low viscosity.
The capsules formed by the emulsion made from A1 have a strength of 28 N after dried, which is so high that it is difficult to release the asphalt-recycling agent during fatigue loading.
The capsules were added to asphalt concrete, and it was found that the capsules exhibited no significant reinforcement on the healing performance of the asphalt concrete.
Example 3 Calcium alginate capsules were prepared. 200 g of 1 wt% industrial-grade sodium alginate solution was prepared, then 20 mi of asphalt-recycling agent and 1 ml of Tween 80 were added, and the resulting mixture was subjected to shearing.
The resulting emulsion was dropped, and it was found that droplets flowed out linearly and were unable to form capsules due to low viscosity.
Using attapulgite to increase the viscosity of the emulsion can effectively solve this problem. 200 g of 1 wi% industrial-grade sodium alginate solution was prepared, then 6 g (accounting for 3% of the mass of the sodium alginate solution) of attapulgite was added, and the resulting mixture was subjected to shearing; and then the same volumes of asphalt-recycling agent and Tween 80 were added, and the resulting mixture was subjected to shearing. It was found that the emulsion exhibited an increased viscosity and was able to form capsules. The prepared capsules have a strength of 12 N, which meets the technical requirements of asphalt concrete construction. The capsules prepared in this example have appearance shown in FIG. 2. Example 4 Two types of calcium alginate capsules were prepared. Two 1.875 wt% sodium alginate solutions were prepared, each of 400 mi; then 0 g and 12 g of attapulgite were added to the above solutions separately; and the resulting mixtures were separately subjected to high-speed shearing for 10 min in a shear, with a shearing rate of 3,500 rpm. 40 mi of sunflower oil (asphalt-recycling agent) and 2 ml of Tween 80 (surfactant) were added to each of the mixtures, and the resulting mixtures were separately subjected to high-speed shearing for 10 min in a shear, with a shearing rate of 4,000 rpm. The obtained capsules were dried in an oven at 45°C for 6 h. Then the dried capsules were added to an asphalt mixture (at an amount of 0.5 wt%), and an asphalt mixture without capsules was prepared as a control group. Then three point bending test, fatigue loading test (inducing the release of the asphalt-recycling agent), and three point bending test were conducted in sequence on a trabecular specimen prepared from the asphalt mixture to test the strength recovery rate for the healed trabecular specimen. The fatigue loading test was conducted under the following conditions: temperature: 20°C; loading intensity: 0.7 MPa; and the number of loading: 30,000. The healing rates (strength recovery rates) of the trabeculae with capsules were determined as
60.3% and 71.3%, respectively, and the healing rate of the trabecula without capsules was determined as 45%. It shows that the asphalt-recycling agent released from the capsule improves the healing performance of the asphalt mixture, and the attapulgite enhances the effect of the calcium alginate capsule on the healing performance of asphalt.
Claims (5)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910934048.2A CN110511435B (en) | 2019-09-29 | 2019-09-29 | Preparation method of attapulgite/calcium alginate composite wall material asphalt self-healing capsule |
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| Publication Number | Publication Date |
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| NL2026510A true NL2026510A (en) | 2021-04-19 |
| NL2026510B1 NL2026510B1 (en) | 2023-01-19 |
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| NL2026510A NL2026510B1 (en) | 2019-09-29 | 2020-09-21 | Method for preparing capsules with attapulgite/calcium alginate composite wall for asphalt self-healing |
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| CN (1) | CN110511435B (en) |
| NL (1) | NL2026510B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486580A (en) * | 2021-12-27 | 2022-05-13 | 哈尔滨工业大学 | Graphene microcapsule asphalt self-healing test evaluation method |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102199842B1 (en) * | 2020-08-27 | 2021-01-08 | 창원대학교 산학협력단 | Micro Core-Shell Capsule for Self-Healing and Self-Healable Composite Including the Same |
| CN112205399B (en) * | 2020-10-22 | 2022-03-04 | 中国科学院合肥物质科学研究院 | Construction method of electrically-driven controlled-release and migrating gel-based pesticide system, constructed pesticide system and application thereof |
| CN112341830B (en) * | 2020-11-09 | 2022-07-08 | 武汉理工大学 | Preparation method of self-packaging calcium alginate asphalt self-healing capsule |
| CN112321898A (en) * | 2020-11-09 | 2021-02-05 | 武汉理工大学 | Preparation method of dual-response type asphalt self-healing capsule |
| CN112408846A (en) * | 2020-11-19 | 2021-02-26 | 武汉理工大学 | Preparation method of shrinkage compensation type asphalt self-healing capsule |
| CN113603395A (en) * | 2020-12-28 | 2021-11-05 | 武汉理工大学 | Flame-retardant warm-mixing self-healing asphalt concrete and preparation method and application thereof |
| CN113603394B (en) * | 2020-12-28 | 2022-08-05 | 武汉理工大学 | Flame-retardant warm-mixing self-healing asphalt concrete and preparation method and application thereof |
| CN113999434B (en) * | 2021-11-10 | 2022-07-05 | 招商局重庆交通科研设计院有限公司 | Preparation method of calcium alginate asphalt self-healing capsule with excellent thermal stability |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7147708B2 (en) * | 2002-09-23 | 2006-12-12 | Solomon Colors, Inc. | Fiber gel mixture for use in cementicious products |
| CN104911171A (en) * | 2015-05-25 | 2015-09-16 | 淮阴工学院 | Method for preparing probiotics microcapsule by compounding sodium alginate, gelatin and attapulgite |
| CN106117497A (en) * | 2016-07-19 | 2016-11-16 | 黄伟 | A kind of attapulgite modified compound polyurethane material and preparation method thereof |
| CN107201656B (en) * | 2017-07-11 | 2020-01-24 | 盐城工业职业技术学院 | Application of attapulgite/sodium alginate organic-inorganic hybrid material in modification of cotton fabric and cotton fabric finishing method |
| CN108997793A (en) * | 2018-04-24 | 2018-12-14 | 曹俊峰 | A kind of processing method of the inorganic filler for pervious asphalt production |
| CN109437674B (en) * | 2018-12-07 | 2021-06-08 | 武汉理工大学 | Long-acting self-repairing asphalt concrete based on stress response type multi-cavity capsule |
| CN110305492B (en) * | 2019-07-16 | 2021-04-30 | 长沙理工大学 | Emulsified asphalt with improved strength after curing |
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2019
- 2019-09-29 CN CN201910934048.2A patent/CN110511435B/en active Active
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486580A (en) * | 2021-12-27 | 2022-05-13 | 哈尔滨工业大学 | Graphene microcapsule asphalt self-healing test evaluation method |
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| NL2026510B1 (en) | 2023-01-19 |
| CN110511435A (en) | 2019-11-29 |
| CN110511435B (en) | 2021-01-05 |
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