CN114874459A - Emulsified rubber asphalt material and preparation method thereof - Google Patents
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/04—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers
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- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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Abstract
The invention relates to an emulsified rubber asphalt material and a preparation method thereof, wherein the emulsified rubber asphalt material comprises composite colloidal particle modified asphalt and emulsified soap liquid, and the composite colloidal particle modified asphalt accounts for 40-60% of the emulsified rubber asphalt material by weight; the preparation method of the composite colloidal particle modified asphalt comprises the following steps: firstly, preparing low-Mooney reclaimed rubber, then carrying out banburying, melting and blending on the low-Mooney reclaimed rubber and SBS and maleic anhydride, carrying out screw extrusion granulation to prepare composite colloidal particles, adding the composite colloidal particles into matrix asphalt, and then adding rubber oil to prepare the rubber; the emulsified soap liquid consists of a compound cationic emulsifier, self-emulsifying waterborne epoxy resin, a stabilizer, a pH regulator and deionized water. The emulsified rubber asphalt material prepared by the invention has the advantages of high emulsification stability, obvious high-temperature deformation resistance, low-temperature crack resistance and durability.
Description
Technical Field
The invention relates to an emulsified rubber asphalt material and a preparation method thereof, belonging to the technical field of preparation of road materials.
Background
The existing emulsified asphalt is an emulsion which is prepared by uniformly dispersing asphalt into an aqueous phase in a micro-droplet state under the action of an emulsifier and mechanical force. Compared with hot asphalt and diluted asphalt, the emulsified asphalt has the advantages of obvious technology, cost and environmental protection. The emulsified asphalt can be directly sprayed as a sticky layer oil, a permeable layer oil, a fog sealing layer and the like, and can also be used as a binding material of a gravel sealing layer and a penetration type pavement. In addition, the emulsified asphalt can be mixed at normal temperature to prepare a cold-mixed cold-paved mixture, and the cold-mixed cold-paved mixture is used in the field of preventive maintenance of roads.
With the rapid development of social economy in China, the traffic flow and load pressure are increased rapidly. The conventional emulsified asphalt can not meet the use requirements of asphalt pavements gradually. In particular, emulsified asphalt has not been able to function as a road functional structural layer. Various modifiers have been tried to modify emulsified asphalt. At present, more materials comprise SBS and SBR latex, the SBS has a good modification effect on hot asphalt, but when the SBS is used for modified asphalt emulsification, the process is complex, the requirement on equipment is high, the cost is high, and the SBS is not resistant to aging. When SBR latex is used for modification, the requirements on the production process of raw materials are high. The low-temperature polymerized SBR latex can obviously improve the high-temperature and low-temperature performances of the emulsified asphalt, and the high-temperature polymerized SBR latex has a common modification effect and poor high-temperature performance. And according to different charge properties, the SBR latex modified asphalt needs to be matched with an emulsifier with the same charge type for emulsification.
The waste tire rubber is composed of various rubber molecules, such as styrene butadiene rubber, isoprene rubber and the like. The rubber asphalt prepared by modifying the asphalt with the waste rubber can effectively improve the low-temperature crack resistance, the high-temperature stability and the adhesion with aggregate of the asphalt, reduce black pollution and reduce production cost, and is widely applied. However, the odor problem always restricts the development of the rubber asphalt, and the construction at normal temperature can be realized and the odor problem is eliminated through emulsification. However, the stable preparation of high performance emulsified rubber asphalt is always an industry problem, which is bound by the crosslinked network of rubber.
Patent CN101173106A discloses a method for preparing rubber powder-asphalt emulsion, the rubber powder used in the method has larger particle size, and the rubber powder is not subjected to desulphurization pretreatment, which results in poor rubber dispersibility and poor emulsion stability. Patent CN102660125A discloses a method for preparing waste rubber modified emulsified asphalt, which comprises pretreating rubber, mixing it with activating agent in supercritical CO2, preparing rubber with high sol content by high temperature and high pressure method, and modifying and emulsifying asphalt with the rubber. The method has the advantages of complex process and higher cost, the supercritical CO2 activated rubber is not industrialized all the time, the actual application is difficult to be realized, and the stability of the emulsified rubber asphalt is not reported. Patent CN103881401A discloses a crumb rubber modified emulsified asphalt and a preparation method thereof, which realizes the successful preparation of rubber modified emulsified asphalt, but the long-term stability of the emulsified asphalt still has a problem, and the specific implementation effect of the emulsified asphalt applied to a mixture is not seen. CN105176115B discloses SBS rubber powder composite modified asphalt, which comprises the following components in parts by mass: 15-21 parts of waste rubber powder, 2-3 parts of SBS modifier, 0.2-0.4 part of stabilizer, 0.03-0.04 part of activator and 75-82 parts of asphalt. The preparation method comprises the steps of preheating the matrix asphalt to 180 ℃, adding the SBS modifier into the hot asphalt, shearing and dispersing for 20min at a high speed, then adding the activating agent, the rubber powder and the stabilizing agent, and shearing and dispersing for 2h at a high speed at 185 ℃, but the stability of the formed emulsion is unreliable.
Disclosure of Invention
The invention aims to solve the problems in the background and provides an emulsified rubber asphalt material and a preparation method thereof, and the prepared emulsified rubber asphalt material has the advantages of high emulsification stability, obvious high-temperature deformation resistance, low-temperature crack resistance and durability, can be directly used on a construction site, and does not need on-site compounding.
The purpose of the invention is realized as follows:
an emulsified rubber asphalt material comprises composite colloidal particle modified asphalt and emulsified soap liquid, wherein the composite colloidal particle modified asphalt accounts for 40-60% of the emulsified rubber asphalt material by weight; the preparation method of the composite colloidal particle modified asphalt comprises the following steps: firstly, preparing low-Mooney reclaimed rubber, then carrying out banburying, melting and blending on the low-Mooney reclaimed rubber and SBS and maleic anhydride, carrying out screw extrusion granulation to prepare composite colloidal particles, adding the composite colloidal particles into matrix asphalt, and then adding rubber oil to prepare the rubber; the emulsified soap liquid consists of a compound cationic emulsifier, self-emulsifying waterborne epoxy resin, a stabilizer, a pH regulator and deionized water.
Further, the raw materials of the composite colloidal particle modified asphalt comprise composite colloidal particles, rubber oil and matrix asphalt; the emulsified rubber asphalt material comprises 10-30 wt% of composite colloidal particles and 1-10 wt% of rubber oil.
Further, the base asphalt is 70 # Or 90 # Petroleum asphalt for road.
Further, the raw materials of the composite colloidal particle consist of low-Mooney reclaimed rubber, SBS and maleic anhydride; the mass ratio of the three components is (80-90): (5-20): 1-10).
Further, the preparation process of the low-Mooney reclaimed rubber comprises the steps of carrying out desulfurization treatment on rubber powder or waste rubber powder, wherein the Mooney viscosity is less than 30; the SBS has a star-shaped or linear structure; the particle size of the composite colloidal particle is below 6 mm.
Further, the proportion of the compound cationic emulsifier in the emulsified soap liquid is 1-8 wt%, the proportion of the self-emulsifying water-based epoxy resin is 5-10 wt%, and the proportion of the stabilizer is 1-10 wt%.
Further, the compound cationic emulsifier is one or more of quaternary ammonium salts, alkyl amines, lignin amines, imidazolines and amidoamines.
Further, the stabilizer is one or more of calcium chloride, magnesium chloride, sodium chloride and ammonium chloride.
Further, the pH regulator is one or more of hydrochloric acid, sulfuric acid, oxalic acid and formic acid.
A preparation method of an emulsified rubber asphalt material is characterized by comprising the following steps:
(1) at the temperature of 150-;
(2) heating the matrix asphalt at 140 ℃ to a flowing state, adding the composite colloidal particles, stirring and swelling at 160-180 ℃ for 1h, adding rubber oil, shearing at 5000rpm at 170-190 ℃ for 1h, stirring and developing at 500rpm for 3h to prepare the composite colloidal particle modified asphalt;
(3) taking a compound cationic emulsifier, adding deionized water at 50-60 ℃ into self-emulsifying water-based epoxy resin, adding a stabilizer, quickly and uniformly stirring, adding a pH regulator to adjust the pH value of the emulsion to 1-3, and preparing an emulsified soap solution;
(4) and (3) synchronously adding the composite colloidal particle modified asphalt and the emulsified soap liquid into a high-speed shearing machine or a colloid mill, and circulating for 10-20min until the emulsion is changed into grey brown to prepare the emulsified rubber asphalt.
The composite rubber modified asphalt has the advantages of obvious high-temperature deformation resistance, low-temperature crack resistance and durability. However, the rubber powder for preparing the composite rubber asphalt has a complex structure and poor compatibility with asphalt, so that the rubber asphalt is extremely difficult to emulsify. The invention provides a formula and a process of emulsified rubber asphalt. Firstly, rubber powder is activated to prepare low-Mooney reclaimed rubber, and then the low-Mooney reclaimed rubber and SBS are added with maleic anhydride to carry out melt blending for mechanochemical grafting granulation to prepare the composite rubber particles. The composite colloidal particles are added into asphalt to prepare composite rubber modified asphalt, and then the composite rubber asphalt is successfully emulsified by compounding a cationic emulsifier. The content of evaporation residue of the emulsified rubber asphalt can reach 59.8% when the oil-water ratio is 6: 4. The material has the characteristics of simple preparation process, excellent mechanical property, high softening point, high storage stability and the like. The softening point of the residual sulfur can reach 89 ℃, and the storage stability of the products 1d and 5d is 0.1 percent and 0.8 percent respectively. The emulsified rubber asphalt can be used in adhesive layer oil, stress absorbing layer and cold mixing mixture, and has good construction and road performance.
The waste rubber powder is a sulfide mainly having sulfur bonds such as s-s, c-s bonds, and the low-Mooney reclaimed rubber becomes softer by opening the s-s bonds and the c-s bonds through desulfurization. When the low-Mooney reclaimed rubber and the asphalt are dissolved together, the reclaimed rubber is easily dissolved with the asphalt and forms a stable colloid structure, so that the material is more exquisite; maleic anhydride also has the function of promoting emulsification, and can well form emulsion; the conventional rubber powder or waste rubber powder cannot be used for emulsification; if the emulsion is prepared by force, the emulsion will separate into layers in about 3 hours and cannot be used.
In addition, the low-Mooney reclaimed rubber also contains amino which can be emulsified together with epoxy resin in the emulsified soap liquid, and after the product is sprayed, constructed and dried, the structure is compact and uniform, and the adhesion is good.
Compared with the prior art, the invention has the following advantages:
(1) the synergistic effect of the reclaimed rubber and the SBS composite polymer on the molecular level is fully exerted, and the performance shortness of the single modified asphalt is compensated.
(2) Maleic anhydride is introduced for mechanochemical grafting, and the compatibility among rubber, SBS and asphalt is improved through the combination of polar functional groups, so that stable emulsion is easier to form.
(3) Specific low-Mooney reclaimed rubber, SBS and maleic anhydride are granulated to form composite colloidal particles with a certain size, so that the composite colloidal particles can be better compatible with asphalt, the material is finer, the stability is greatly improved, the drawing strength of emulsified asphalt is improved, and the adhesion of the asphalt and aggregate is improved.
(4) The emulsification and stable storage of the reclaimed rubber/SBS modified asphalt are realized through the reasonable compounding of the emulsified soap liquid, and the reclaimed rubber/SBS modified asphalt is applied to high-performance viscous layer oil, cold-mixed cold-laid mixtures and the like.
Detailed Description
The present invention will be further described with reference to the following examples.
The self-emulsifying waterborne epoxy resin is purchased from Tianjin Henry Cheng-Tai road building materials science and technology Co., Ltd, model HY-R. The rest are purchased from conventional models in the market. The low-Mooney reclaimed rubber is obtained by desulfurizing waste rubber powder and enabling the Mooney viscosity of the waste rubber powder to be less than 30; SBS is linear structure; the compound cationic emulsifier is a conventional quaternary ammonium salt emulsifier, an alkylamine emulsifier 1: 1 weight ratio of the compound product. The stabilizer is calcium chloride. The pH regulator is hydrochloric acid.
Example 1
At the temperature of 200 ℃, the low-Mooney reclaimed rubber and SBS and maleic anhydride are subjected to banburying melt blending in a screw extrusion or banburying melt blending mode, and the composite colloidal particles are prepared by screw extrusion granulation. Wherein, 8 parts of low Mooney reclaimed rubber, 1.7 parts of SBS and 0.3 part of maleic anhydride. The size of the composite colloidal particles is below 6 mm.
Taking 5040g of matrix asphalt, heating to a flowing state at 140 ℃, adding 600g of composite colloidal particles, stirring and swelling for 1h at 160 ℃, adding 360g of rubber oil, shearing for 1h at 180 ℃ at 5000rpm, stirring and developing for 3h at 500rpm, and obtaining 6000g of composite colloidal particle modified asphalt.
Taking 80g of compound cationic emulsifier, adding 300g of self-emulsifying water-based epoxy resin, adding a certain amount of deionized water at 50-60 ℃, adding 20g of stabilizer, quickly and uniformly stirring, adding a pH regulator to adjust the pH value of the emulsion to 1-3, and preparing 4000g of emulsified soap solution.
And (3) synchronously adding the composite colloidal particle modified asphalt and the emulsified soap liquid into a high-speed shearing machine or a colloid mill according to the weight ratio of 6:4, and circulating for 10min until the emulsion is changed into grey brown to prepare the emulsified rubber asphalt material.
Example 2
At the temperature of 200 ℃, the low-Mooney reclaimed rubber and SBS and maleic anhydride are subjected to banburying melt blending in a screw extrusion or banburying melt blending mode, and the composite colloidal particles are prepared by screw extrusion granulation. Wherein, 8 parts of low Mooney reclaimed rubber, 1.7 parts of SBS and 0.3 part of maleic anhydride. The size of the composite colloidal particles is below 6 mm.
Taking 5040g of matrix asphalt, heating to a flowing state at 140 ℃, adding 600g of composite colloidal particles, stirring and swelling for 1h at 160 ℃, adding 360g of rubber oil, shearing for 1h at 180 ℃ at 5000rpm, stirring and developing for 3h at 500rpm, and obtaining 6000g of composite colloidal particle modified asphalt.
Taking 120g of compound cationic emulsifier, adding 200g of self-emulsifying waterborne epoxy resin, adding a certain amount of deionized water at 50-60 ℃, adding 20g of stabilizer, rapidly and uniformly stirring, adding pH regulator to adjust the pH value of the emulsion to 1-3, and preparing 4000g of emulsified soap solution.
And (3) synchronously adding the composite colloidal particle modified asphalt and the emulsified soap liquid into a high-speed shearing machine or a colloid mill according to the weight ratio of 6:4, and circulating for 10min until the emulsion is changed into grey brown to prepare the emulsified rubber asphalt material.
Comparative example 1
Essentially the same as example 1 except that no maleic anhydride was added.
Comparative example 2
Essentially the same as example 1 except that the low mooney reclaimed rubber was replaced with ordinary waste rubber crumb.
Comparative example 3
Essentially the same as example 1 except that no self-emulsifying aqueous epoxy resin was added.
Comparative example 4
8 parts of low-Mooney reclaimed rubber, 1.7 parts of SBS and 0.3 part of maleic anhydride, and the three materials are directly mixed and uniformly stirred to prepare the compound material.
5040g of matrix asphalt is heated to a flowing state at 140 ℃, 600g of compound material is added, the mixture is stirred and swelled at 160 ℃ for 1h, 360g of rubber oil is added, the mixture is sheared at 180 ℃ at 5000rpm for 1h, and stirred at 500rpm for 3h, and 6000g of compound colloidal particle modified asphalt is prepared.
Taking 80g of compound cationic emulsifier, adding 300g of emulsified waterborne epoxy resin, adding a certain amount of deionized water at 50-60 ℃, adding 20g of stabilizer, rapidly and uniformly stirring, adding a pH regulator to adjust the pH value of the emulsion to 1-3, and preparing 4000g of emulsified soap solution.
And (3) synchronously adding the composite colloidal particle modified asphalt and the emulsified soap liquid into a high-speed shearing machine or a colloid mill according to the weight ratio of 6:4, and circulating for 10min until the emulsion is changed into grey brown to prepare the emulsified rubber asphalt material.
The materials of the examples and comparative examples were tested according to the standard and the results are given in the following table:
TABLE 1 Evaporation residue Performance of emulsified rubber asphaltTest results
| Technical index | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Test specification |
| Speed of emulsion breaking | Slow crack | Slow crack | Slow crack | Can not emulsify | Slow crack | Slow crack | T0658-1993 |
| Content of evaporation residue/%) | 58.9 | 59.5 | 59.4 | - | 58.2 | 59.0 | T0651-1993 |
| Penetration/0.1 mm | 38.6 | 37 | 62 | - | 44 | 40 | T0604-2011 |
| Softening point/. degree.C | 87 | 89 | 72 | - | 78 | 85 | T0606-2011 |
| Ductility (5 ℃)/cm | 22 | 23 | 24 | - | 25 | 23 | T0605-2011 |
| Dynamic viscosity (60 ℃) Pa.s | 510200 | 509080 | 8900 | - | 207600 | 486800 | T0620-2000 |
| Brookfield viscosity (135 ℃) Pa.s | 25.5 | 26.4 | 9.6 | - | 15.3 | 24.6 | T0625-2011 |
| Storage stability (1d)/% | 0.2 | 0.3 | 0.7 | Layering | 0.5 | Instability of the film | T0655-1993 |
| Storage stability (5d)/% | 0.8 | 0.6 | 2.1 | Layering | 0.9 | Layering | T0655-1993 |
The results show that the emulsified rubber asphalt material prepared by the method for preparing the cationic emulsified composite colloidal particle modified asphalt can greatly improve the high-low temperature performance and the storage stability of the modified emulsified rubber asphalt, so that the capacity of resisting various cracks and deformations under the alternate action of vehicle load and environmental change when a bonding layer, a cold-mixed cold-paved mixture and the like are used as a road structure layer is enhanced, the service life is prolonged, and the method has high application and popularization values.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (10)
1. The emulsified rubber asphalt material is characterized by comprising composite colloidal particle modified asphalt and emulsified soap liquid, wherein the composite colloidal particle modified asphalt accounts for 40-60% of the emulsified rubber asphalt material by weight; the preparation method of the composite colloidal particle modified asphalt comprises the following steps: firstly, preparing low-Mooney reclaimed rubber, then carrying out banburying, melting and blending on the low-Mooney reclaimed rubber and SBS and maleic anhydride, carrying out screw extrusion granulation to prepare composite colloidal particles, adding the composite colloidal particles into matrix asphalt, and then adding rubber oil to prepare the rubber; the emulsified soap liquid consists of a compound cationic emulsifier, self-emulsifying waterborne epoxy resin, a stabilizer, a pH regulator and deionized water.
2. The emulsified rubber asphalt material as claimed in claim 1, wherein the raw material of said composite crumb modified asphalt is composed of composite crumb, rubber oil, base asphalt; the emulsified rubber asphalt material comprises 10-30 wt% of composite colloidal particles and 1-10 wt% of rubber oil.
3. The emulsified rubber asphalt material as defined in claim 1, wherein said base asphalt is 70% # Or 90 # Petroleum asphalt for road.
4. The emulsified rubber asphalt material as set forth in claim 1, wherein the raw material of said composite crumb rubber is composed of a low-mooney reclaimed rubber, SBS and maleic anhydride; the mass ratio of the three components is (80-90): (5-20): 1-10).
5. The emulsified rubber asphalt material as claimed in claim 1, wherein said low-mooney reclaimed rubber is prepared by subjecting rubber powder or waste rubber powder to desulfurization treatment, and has a mooney viscosity of less than 30; the SBS has a star-shaped or linear structure; the particle size of the composite colloidal particle is below 6 mm.
6. The emulsified rubber asphalt material as claimed in claim 1, wherein the proportion of the compound cationic emulsifier in the emulsified soap solution is 1-8 wt%, the proportion of the self-emulsifying water-based epoxy resin is 5-10 wt%, and the proportion of the stabilizer is 1-10 wt%.
7. The emulsified rubberized asphalt material of claim 1, wherein the built cationic emulsifier is one or more of quaternary ammonium salts, alkyl amines, lignin amines, imidazolines, and amidoamines.
8. The emulsified rubber asphalt material as defined in claim 1, wherein said stabilizer is one or more of calcium chloride, magnesium chloride, sodium chloride and ammonium chloride.
9. The emulsified rubber asphalt material as defined in claim 1, wherein the pH regulator is one or more of hydrochloric acid, sulfuric acid, oxalic acid and formic acid.
10. The method for preparing an emulsified rubber asphalt material according to any one of claims 1 to 9, which comprises the steps of:
(1) at the temperature of 150 plus 300 ℃, the low Mooney regenerated rubber and SBS and maleic anhydride are mixed and melted and blended, and then are extruded by a screw rod for granulation to prepare composite rubber particles;
(2) heating the matrix asphalt at 140 ℃ to a flowing state, adding the composite colloidal particles, stirring and swelling at 160-180 ℃ for 1h, adding rubber oil, shearing at 5000rpm at 170-190 ℃ for 1h, and stirring and developing at 500rpm for 3h to prepare the composite colloidal particle modified asphalt;
(3) taking a compound cationic emulsifier, adding deionized water at 50-60 ℃ into self-emulsifying water-based epoxy resin, adding a stabilizer, quickly and uniformly stirring, adding a pH regulator to adjust the pH value of the emulsion to 1-3, and preparing an emulsified soap solution;
(4) and (3) synchronously adding the composite colloidal particle modified asphalt and the emulsified soap liquid into a high-speed shearing machine or a colloid mill, and circulating for 10-20min until the emulsion is changed into grey brown to prepare the emulsified rubber asphalt.
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| CN115746774A (en) * | 2022-11-19 | 2023-03-07 | 东南大学 | Normal-temperature fast-curing crack repairing agent, preparation method and application thereof |
| CN116178974A (en) * | 2023-03-02 | 2023-05-30 | 浙江数智交院科技股份有限公司 | Non-sticky emulsified asphalt as well as preparation method and application thereof |
| CN116463060A (en) * | 2023-03-21 | 2023-07-21 | 东南大学 | Composite modified asphalt for odor-removal weather-resistant high-speed railway asphalt concrete waterproof sealing layer and preparation method thereof |
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|---|---|---|---|---|
| CN115746774A (en) * | 2022-11-19 | 2023-03-07 | 东南大学 | Normal-temperature fast-curing crack repairing agent, preparation method and application thereof |
| CN116178974A (en) * | 2023-03-02 | 2023-05-30 | 浙江数智交院科技股份有限公司 | Non-sticky emulsified asphalt as well as preparation method and application thereof |
| CN116463060A (en) * | 2023-03-21 | 2023-07-21 | 东南大学 | Composite modified asphalt for odor-removal weather-resistant high-speed railway asphalt concrete waterproof sealing layer and preparation method thereof |
| CN116463060B (en) * | 2023-03-21 | 2024-03-12 | 东南大学 | Composite modified asphalt for odor-removal weather-resistant high-speed railway asphalt concrete waterproof sealing layer and preparation method thereof |
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