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CN112250830B - Environment-friendly road microcapsule, preparation method thereof and application of illegal cooking oil - Google Patents

Environment-friendly road microcapsule, preparation method thereof and application of illegal cooking oil Download PDF

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CN112250830B
CN112250830B CN202011015509.5A CN202011015509A CN112250830B CN 112250830 B CN112250830 B CN 112250830B CN 202011015509 A CN202011015509 A CN 202011015509A CN 112250830 B CN112250830 B CN 112250830B
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microcapsule
environment
friendly road
solution
oil
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CN112250830A (en
Inventor
纪小平
陈云
华文龙
司柏通
张阳
姚秉辰
胡永林
李加
汤振农
曹正道
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Highway Management Section Of Jindong District Jinhua City
Jinhua Highway And Transportation Management Center
Changan University
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Highway Management Section Of Jindong District Jinhua City
Jinhua Highway And Transportation Management Center
Changan University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/16Catalysts
    • C08G18/22Catalysts containing metal compounds
    • C08G18/24Catalysts containing metal compounds of tin
    • C08G18/244Catalysts containing metal compounds of tin tin salts of carboxylic acids
    • C08G18/246Catalysts containing metal compounds of tin tin salts of carboxylic acids containing also tin-carbon bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/36Hydroxylated esters of higher fatty acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/62Polymers of compounds having carbon-to-carbon double bonds
    • C08G18/6212Polymers of alkenylalcohols; Acetals thereof; Oxyalkylation products thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/6547Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B15/00Solidifying fatty oils, fats, or waxes by physical processes
    • EFIXED CONSTRUCTIONS
    • E01CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
    • E01CCONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
    • E01C7/00Coherent pavings made in situ

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Architecture (AREA)
  • Dispersion Chemistry (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Road Paving Structures (AREA)

Abstract

The invention belongs to the technical field of asphalt pavements, and discloses an environment-friendly road microcapsule, a preparation method thereof and application of illegal cooking oil, wherein the environment-friendly road microcapsule comprises the following raw materials: polyvinyl alcohol, illegal cooking oil, isophorone diisocyanate, dibutyltin dilaurate and deionized water. The preparation method comprises the following steps: preparing an emulsifier solution; mixing the illegal cooking oil with isophorone diisocyanate to obtain an activated capsule core solution; shearing and mixing the emulsifier solution and the activated capsule core solution, and dropwise adding dibutyltin dilaurate into the mixture for catalytic emulsification reaction to obtain a permeable microcapsule turbid solution; centrifuging and drying the mixture. The invention utilizes the illegal cooking oil to prepare the environment-friendly road self-healing microcapsule with the grain diameter range of 15-30 mu m and the capsule core coating rate of 75 percent, and realizes the self-healing of cracks when the cracks appear.

Description

Environment-friendly road microcapsule, preparation method thereof and application of illegal cooking oil
Technical Field
The invention relates to the technical field of asphalt pavements, in particular to an environment-friendly road microcapsule, a preparation method thereof and application of illegal cooking oil.
Background
The illegal cooking oil generally refers to various inferior oils existing in life, such as recycled edible oil, repeatedly used frying oil, etc. The largest source of the swill-cooked dirty oil is an oil separation tank of a sewer of a large-scale urban restaurant, namely the oil obtained by simply processing and extracting greasy floaters in the sewer or leftovers and leftovers (generally called swill) of hotels and restaurants is non-edible oil which is extremely poor in quality and extremely insanitary, belongs to domestic garbage, has great harm to human bodies when flowing into dining tables, and has great significance on healthy life and green life of human beings.
The cracks are one of the most common diseases of the asphalt pavement, are gradually formed by micro cracks under the coupling action of temperature and load, and are further developed into macro cracks under the action of concentrated stress. If measures are not taken in time, the area of the crack is gradually increased, extends deeply and downwards, and the diseases such as pit pits, looseness and the like are formed under the action of moisture and traffic load. The microcapsule technology is one of the methods for realizing the self-healing of the asphalt pavement, when the microcracks extend to the microcapsules, the capsule wall is broken, the capsule core material is released, the cracks heal at the initial stage, and the service life of the asphalt pavement is prolonged.
The microcapsule used for the road at present has larger grain diameter and thick capsule wall, so that the microcapsule has larger influence on the performance of the asphalt pavement and lower coating rate. The preparation method of the microcapsules for the road at present mainly comprises a physical adsorption method and an in-situ polymerization method, wherein the particle size of the microcapsules prepared by the physical adsorption method is 1-2mm, the thickness of the capsule wall depends on external adsorption rocks, and the coating rate of the capsule core is determined by the pores of the external capsule wall and cannot be stabilized. The capsule prepared by the in-situ polymerization method has the size of 50-100 mu m, the capsule wall thickness of 5-10 mu m and the capsule core coating rate of 60-65 percent. The smaller the particle size of the microcapsule is, the smaller the influence on road performance such as high-temperature stability, low-temperature crack resistance and the like of the asphalt pavement is; the smaller the thickness of the capsule wall is, the more easily the capsule wall is cracked under the stimulation of the same crack stress; the higher the coating rate is, the higher the utilization rate of raw materials in the preparation process is, and the higher the healing rate of the microcapsule with the high coating rate is than the lower coating rate.
Disclosure of Invention
Aiming at the problems, the invention aims to provide an environment-friendly road microcapsule, a preparation method thereof and application of illegal cooking oil, and provides a brand-new application way of the illegal cooking oil, the particle size range of the prepared environment-friendly road self-healing microcapsule is 15-30 mu m, the capsule core coating rate is 75%, when cracks appear, the self-healing of the cracks can be well realized, and the road performance of an asphalt mixture is improved.
The invention is realized by adopting the following technical scheme:
the environment-friendly road microcapsule comprises the following raw materials: polyvinyl alcohol, illegal cooking oil, isophorone diisocyanate, dibutyltin dilaurate and deionized water.
Furthermore, the using ratio of the polyvinyl alcohol, the gutter oil, the isophorone diisocyanate, the dibutyltin dilaurate and the deionized water is 300: 150-200: 75: 450.
Still further, the mass of said dibutyltin dilaurate is 10% of the mass of said isophorone diisocyanate.
Further, the polyvinyl alcohol is a polyvinyl alcohol 1788 type, and is a liquid.
(II) a preparation method of environment-friendly road microcapsules, which comprises the following steps:
step 1, preparing an emulsifier solution; mixing the illegal cooking oil with isophorone diisocyanate to obtain an activated capsule core solution;
step 2, shearing and mixing the emulsifier solution and the activated capsule core solution to obtain an oil-in-water type emulsion;
step 3, dropwise adding dibutyltin dilaurate into the oil-in-water type emulsion for catalytic emulsification reaction to obtain an environment-friendly road microcapsule turbid liquid; and (4) carrying out centrifugal treatment and drying on the turbid solution of the environment-friendly road microcapsule to obtain the environment-friendly road microcapsule.
Further, the process for preparing the emulsifier solution is as follows: and (3) dripping polyvinyl alcohol into deionized water to obtain the polyvinyl alcohol.
Further, the shearing speed of the shearing and mixing is 4000-5000 r/min, and the shearing time is 5-10 min.
Further, the conditions of the catalytic emulsification reaction are as follows: reacting for 4-5 h at 80-90 ℃.
Further, the specific process of the centrifugal treatment is as follows: centrifuging the environment-friendly road at 10000r/min of microcapsule turbid liquid for 3min, washing the floating substances on the upper part of a centrifugal tube with water, and then continuously centrifuging; centrifugation was repeated at least 3 times.
Further, the drying temperature is 60-70 ℃, and the drying time is 1-2 hours.
And (III) application of the illegal cooking oil in microcapsule capsule cores for asphalt mixture roads.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention opens up a brand-new application field of the illegal cooking oil, actively utilizes the domestic garbage, changes waste into valuable, and is green and environment-friendly.
(2) The invention utilizes emulsification reaction to prepare the microcapsule core-shell structure, so that the grain diameter of the road microcapsule reaches 15-30 mu m, compared with the grain diameter of the existing road microcapsule of 50-2 mm, the grain diameter of the microcapsule is greatly reduced, and the influence of the road microcapsule on the road performances of asphalt pavement such as high-temperature stability, low-temperature crack resistance and the like is reduced.
(3) The invention firstly prepares the oil-in-water emulsion, and then carries out curing reaction on the water phase to form a capsule wall with a very thin coating on the oil phase, thereby greatly improving the capsule core coating rate of the road microcapsule, compared with the existing coating rate of 60-65%, the capsule core coating rate of the environment-friendly road microcapsule prepared by the invention can reach 75%, and further improving the capability of repairing the micro-cracks of the asphalt pavement.
Drawings
FIG. 1 is a flow chart of a process for preparing environmentally friendly microcapsules for road use according to an embodiment of the present invention;
FIG. 2 is a diagram of a finished product of the environmentally friendly road microcapsule prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the environmentally friendly road microcapsule prepared in example 1 of the present invention;
FIG. 4 is a particle size distribution diagram of an environmentally friendly road microcapsule prepared in example 1 of the present invention;
FIG. 5 is an optical microscopic image of the environmentally friendly road microcapsule prepared in example 1 of the present invention.
Detailed Description
In order to further understand the present invention, the technical solution of the present invention will be further described with reference to examples and experiments, but the present invention is not limited to the following embodiments.
An environment-friendly road microcapsule comprises the following raw materials: polyvinyl alcohol (PVA), illegal cooking oil, isophorone diisocyanate (IPDI), dibutyltin dilaurate (DBTDL) and deionized water, wherein the raw materials are in proportion:
polyvinyl alcohol: waste oil: isophorone diisocyanate: 300 percent of deionized water to 150-200 percent of deionized water to 75-450 percent of deionized water, wherein the adding amount of dibutyltin dilaurate is 10 percent of the mass of the isophorone diisocyanate. Wherein, dibutyltin dilaurate is used as a catalyst, and PVA is used as an emulsifier.
As shown in fig. 1, the preparation method of the microcapsule for environment-friendly road of the present invention comprises the following steps:
step 1, preparing an emulsifier solution; mixing the illegal cooking oil with isophorone diisocyanate to obtain an activated capsule core solution;
step 2, shearing and mixing the emulsifier solution and the activated capsule core solution to obtain an oil-in-water type emulsion;
step 3, dropwise adding dibutyltin dilaurate into the oil-in-water emulsion for catalytic emulsification reaction to obtain an environment-friendly road microcapsule turbid liquid; and (4) carrying out centrifugal treatment and drying on the turbid solution of the environment-friendly road microcapsule to obtain the environment-friendly road microcapsule.
Example 1
An environment-friendly road microcapsule comprises the following substances in percentage by weight: waste oil: IPDI: deionized water 300: 175: 75: 450, and DBTDL 10% of the mass of IPDI. Referring to fig. 1, the preparation method thereof includes the steps of:
33.3g of 1788 type liquid PVA is taken and dripped into 50g of deionized water to prepare an emulsifier solution; mixing 19.4g of illegal cooking oil with 8.3g of isophorone diisocyanate to prepare an activated capsule core solution; mixing the emulsifier solution with the activated capsule core solution, and shearing at a high speed of 5000r/min for 5min to obtain oil-in-water emulsion; dropwise adding 0.83g of dibutyltin dilaurate into the oil-in-water emulsion, and reacting for 4 hours at 80 ℃ to obtain an environment-friendly road microcapsule turbid liquid; centrifuging the turbid solution of microcapsule at 10000r/min for 3min, collecting the upper floating matter, washing with deionized water, centrifuging, repeating for 3 times, and drying in a drying oven at 60 deg.C for 1 hr to obtain powdery environment-friendly road microcapsule, as shown in FIG. 2.
Example 2
An environment-friendly road microcapsule comprises the following substances in percentage by weight: waste oil: IPDI: deionized water 300: 150: 75: 450, and DBTDL is added in an amount of 10% of the mass of IPDI. Referring to fig. 1, the preparation method thereof includes the steps of:
33.3g of 1788 type liquid PVA is taken and dripped into 50g of deionized water to prepare an emulsifier solution; mixing 16.7g of illegal cooking oil with 8.3g of isophorone diisocyanate to prepare an activated capsule core solution; mixing the emulsifier solution with the activated capsule core solution, and shearing at a high speed of 4000r/min for 8min to obtain oil-in-water emulsion; dropwise adding 0.83g of dibutyltin dilaurate into the oil-in-water emulsion, and reacting for 4 hours at 80 ℃ to obtain an environment-friendly road microcapsule turbid liquid; centrifuging the turbid solution of the microcapsule at 10000r/min for 3min, taking the upper floating object, washing with deionized water, continuing centrifuging, repeating for 3 times, and drying in a drying oven at 70 ℃ for 1h to obtain the powdery environment-friendly road microcapsule.
Example 3
An environment-friendly road microcapsule comprises the following substances in percentage by weight: waste oil: IPDI: deionized water is 300: 200: 75: 450, and the addition amount of DBTDL is 10% of the mass of IPDI. Referring to fig. 1, the preparation method thereof includes the following steps:
33.3g of 1788 type PVA is taken and dripped into 50g of deionized water to prepare an emulsifier solution; mixing 22.2g of illegal cooking oil with 8.3g of isophorone diisocyanate to prepare an activated capsule core solution; mixing the emulsifier solution with the activated capsule core solution, and shearing at a high speed of 4000r/min for 6min to obtain oil-in-water emulsion; dropwise adding 0.83g of dibutyltin dilaurate into the oil-in-water emulsion, and reacting at 85 ℃ for 4 hours to obtain an environment-friendly road microcapsule turbid liquid; centrifuging the turbid solution of the microcapsule for 3min at 10000RPM, taking the upper floating object, washing with deionized water, continuing centrifuging, repeating for 3 times, and drying in a drying oven at 60 ℃ for 1h to obtain the powdery environment-friendly road microcapsule.
The environmental-friendly road microcapsule product prepared in example 1 was subjected to microscopic morphology and particle size tests using a scanning electron microscope, a laser particle size analyzer and an optical microscope, and the results are shown in fig. 3 to 5. From the microscopic morphology of fig. 3, it can be seen that the environment-friendly road microcapsule prepared by the invention has a smooth and complete surface. As can be seen from FIG. 4, the microcapsules have a particle size distribution of 15-30 μm and an average particle size of 21 μm. As can be seen from the results of the optical microscope of FIG. 5, the wall thickness of the microcapsule was 2 to 3 μm and the core coating rate was 75%.
The coating rate test process in the embodiment of the invention is as follows:
accurately weighing the dry microcapsule product prepared at one time, fully grinding the dry microcapsule product, and soaking the dry microcapsule product in acetone for 72 hours; wherein, the solvent is replaced once in 24 hours, the capsule core is dissolved out, the capsule wall is filtered, dried and weighed, the difference between the two is obtained to obtain the capsule core mass, and the coating rate is calculated to be (capsule core mass/raw material capsule core mass) × 100%.
The particle size and wall thickness measurements were made on the samples prepared in example 2 and example 3, respectively, and the results were: the microcapsule for the environment-friendly road prepared in the embodiment 2 has a capsule core coating rate of 63%, a particle size of 15-25 μm and an average particle size of 18 μm; the microcapsule for an environmentally friendly road prepared in example 3 had a capsule core coating rate of 75%, a particle diameter of 17 to 35 μm and an average particle diameter of 28 μm. The results show that the microcapsules prepared by the method have smaller particle size and higher coating rate.
Road performance testing
The microcapsules prepared in the embodiments of the invention are added into the asphalt mixture according to the mass ratio of 0.6%, the asphalt mixture is respectively selected from AC-13, SMA-13 and AC-20 type asphalt mixtures, the practical manufacturing is carried out by specifically referring to JTG E10-2011 road engineering asphalt and a compaction method in the asphalt mixture test procedure-T0702-2011 asphalt mixture test piece manufacturing method, the corresponding road microcapsule asphalt mixture test piece is manufactured, then the healing performance of the test piece is tested, and the results are shown in tables 1 and 2.
The test method and the evaluation index of the road microcapsule asphalt mixture test piece corresponding to each embodiment of the invention are as follows:
(1) healing index: the test adopts an electronic universal material testing machine (UTM) to carry out a three-point loading test, and the test conditions are controlled as follows: the test temperature is 0 ℃ and the loading rate is 5 mm/min. The ratio of the critical load after healing and before healing of the test piece is defined as the healing index HI of the microcapsule asphalt mixture 2 And the self-healing performance of the asphalt mixture is used as an evaluation index of the self-healing performance of the asphalt mixture.
Figure BDA0002698922680000071
In the formula: HI (high-intensity) 2 Expressing the healing index of the microcapsule asphalt mixture; p 0 Indicating healing of the test pieceA forward critical load; p 1 The critical load after healing of the test piece is shown.
(2) Fatigue life: the test is carried out by adopting an MTS Landmark (MTS 810) universal tester, and the test conditions are controlled as follows: the stress level is 0.4N, the test temperature is 15 ℃, the loading frequency is 10Hz, the loading wave mode is sine wave, and the intermittent time is 48 h. The number of intermittent fatigue lives of the test was used as an index for evaluating the fatigue life. The method is specifically carried out by referring to JTG E10-2011 road engineering asphalt and asphalt mixture test procedure-T0739-2011 asphalt mixture four-point bending fatigue life test.
TABLE 1 healing index of microencapsulated asphalt mixtures for different roads
Figure BDA0002698922680000081
The results in table 1 show that the healing indexes of various asphalt mixtures after the environment-friendly road microcapsule of the invention is added show a rising trend, that is, the self-healing performance of the asphalt mixture after the microcapsule is added is improved to a certain extent. From the table 1, it can be seen that, for different types of asphalt mixtures, the influence of the environment-friendly road microcapsules prepared by the invention on the healing index is different, the microcapsules of the invention have a very significant improvement effect on the healing performance of the AC-13 asphalt mixture, and the self-healing performance of the AC-13 asphalt mixture is greatly improved.
TABLE 2 intermittent fatigue life (times) of microcapsule asphalt mixture for different roads
Figure BDA0002698922680000082
The results in table 2 show that the microcapsules of the embodiments of the present invention significantly improve the intermittent fatigue life of various asphalt mixtures, which increases the fatigue life by more than 50%, and the fatigue life is an important index of the pavement performance of the asphalt mixtures, and directly reveals the actual service life of the asphalt mixtures, which indicates that the addition of the microcapsules of the present invention significantly improves the service life of various common asphalt mixtures.
The waste oil is obtained from the upper floating oil of leftovers in restaurants; the basic performance indexes and the regeneration effect are shown in the following tables 3 and 4: the basic performance test was carried out using the petroleum asphalt thin film oven test method (GB/T5304-2001).
TABLE 3 basic Performance index of the illegal cooking oil used in each example
Figure BDA0002698922680000091
TABLE 4 regeneration Effect of illegal cooking oil used in examples
Figure BDA0002698922680000092
The PVA adopted by the invention is PVA1788 type and liquid reagent. The IPDI selected by the invention reacts with water to obtain a polymer with higher molecular weight, long molecular chain and high crosslinking density; the catalyst is added to form a shell structure at an oil-water interface, and the shell structure wraps an oil phase to form a microcapsule.
The reaction process of IPDI and water is as follows:
Figure BDA0002698922680000101
the DBTDL adopted by the invention can catalyze the curing reaction of isocyanate, and the catalytic principle of the DBTDL is as follows:
(H 9 C 4 )Sn(OCOC 11 H 23 ) 2 +2NCO-R-OCN→(H 9 C 4 ) 2 Sn(NCO-R-OCN) 2 +C 11 H 23 OCOC 11 H 23 +CO 2 isocyanate monomer can react with DBTDL to generate an organotin compound, one molecular structure of the organotin compound is a compound with a binary ring structure, and the chemical formula of the compound is
Figure BDA0002698922680000102
Is an active component of the catalyst, and has strong catalytic activity on the curing reaction of the cyanate monomer.
The function of the emulsifier is as follows: the oily caplet is dispersed in the aqueous phase in the form of tiny droplets and remains stable.
The invention adopts the illegal cooking oil as the capsule core material of the road microcapsule through the chemical reaction design, prepares the road microcapsule with small grain diameter and thin capsule wall, and has obvious improvement effect on the self-healing performance and the fatigue life of the asphalt mixture road.
Although the present invention has been described in detail in this specification with reference to specific embodiments and illustrative embodiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the present invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (6)

1. An environment-friendly road microcapsule is characterized by being prepared from the following raw materials: polyvinyl alcohol, illegal cooking oil, isophorone diisocyanate, dibutyltin dilaurate and deionized water;
the using amount ratio of the polyvinyl alcohol to the gutter oil to the isophorone diisocyanate to the deionized water is 300: 150-200: 75: 450;
the mass of the dibutyltin dilaurate accounts for 10% of that of the isophorone diisocyanate;
the preparation method of the environment-friendly road microcapsule comprises the following steps:
step 1, dripping polyvinyl alcohol into deionized water to prepare an emulsifier solution; mixing the illegal cooking oil with isophorone diisocyanate to obtain an activated capsule core solution;
step 2, shearing and mixing the emulsifier solution and the activated capsule core solution to obtain an oil-in-water type emulsion;
step 3, dropwise adding dibutyltin dilaurate into the oil-in-water type emulsion for catalytic emulsification reaction to obtain an environment-friendly road microcapsule turbid liquid; and (4) carrying out centrifugal treatment and drying on the turbid solution of the environment-friendly road microcapsule to obtain the environment-friendly road microcapsule.
2. The environmentally friendly road microcapsule according to claim 1, wherein the polyvinyl alcohol is of polyvinyl alcohol 1788 type and is a liquid.
3. The process for preparing environment-friendly road microcapsules according to claim 1, which comprises the following steps:
step 1, dripping polyvinyl alcohol into deionized water to prepare an emulsifier solution; mixing the illegal cooking oil with isophorone diisocyanate to obtain an activated capsule core solution;
step 2, shearing and mixing the emulsifier solution and the activated capsule core solution to obtain an oil-in-water type emulsion;
step 3, dropwise adding dibutyltin dilaurate into the oil-in-water type emulsion for catalytic emulsification reaction to obtain an environment-friendly road microcapsule turbid liquid; and (4) carrying out centrifugal treatment and drying on the turbid solution of the environment-friendly road microcapsule to obtain the environment-friendly road microcapsule.
4. The method of claim 3, wherein the shear mixing is carried out at a shear rate of 4000 to 5000r/min for a shear time of 5 to 10 min.
5. The preparation method according to claim 3, characterized in that the conditions of the catalytic emulsification reaction are: reacting for 4-5 h at 80-90 ℃.
6. The preparation method according to claim 3, wherein the centrifugation treatment comprises the following specific steps: centrifuging the microcapsule turbid solution at 10000r/min for 3min, washing the floating substances on the upper part of a centrifugal tube with water, and then centrifuging continuously; centrifugation was repeated at least 3 times.
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