CN116814087A - Rare earth synergistic flame-retardant asphalt composition and preparation method thereof - Google Patents

Rare earth synergistic flame-retardant asphalt composition and preparation method thereof Download PDF

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Publication number
CN116814087A
CN116814087A CN202310820733.9A CN202310820733A CN116814087A CN 116814087 A CN116814087 A CN 116814087A CN 202310820733 A CN202310820733 A CN 202310820733A CN 116814087 A CN116814087 A CN 116814087A
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China
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flame retardant
asphalt
rare earth
parts
retardant
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唐乃膨
任宝
薛晨阳
李睿
杨博
朱洪洲
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Chongqing Jiaotong University
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Chongqing Jiaotong University
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Abstract

The application discloses a rare earth synergistic flame-retardant asphalt composition and a preparation method thereof, wherein the composition comprises the following raw materials in parts by weight: 10 parts of composite flame retardant and 100 parts of asphalt; wherein the composite flame retardant consists of magnesium hydroxide, a rare earth synergist, a silane coupling agent KH550 and absolute ethyl alcohol; the preparation method comprises the following steps: s100: preparing a composite flame retardant intermediate; s200: preparing a composite flame retardant; s300: preparing the flame-retardant asphalt. The beneficial effects are that: compared with the existing flame retardant, the asphalt has the advantages that the asphalt has high-efficiency flame retardance and smoke suppression performance, the emission of pollutants can be eliminated in the pavement process, the emission of toxic substances in the flame retardance process is reduced, the pavement construction working environment in a tunnel is improved, the physical health burden of constructors is reduced, meanwhile, the fire loss and casualties of a highway tunnel can be greatly reduced, the driving safety is improved, and the service life of the pavement of the highway tunnel is prolonged.

Description

Rare earth synergistic flame-retardant asphalt composition and preparation method thereof
Technical Field
The application relates to the technical field of pavement materials, in particular to a rare earth synergistic flame-retardant asphalt composition and a preparation method thereof.
Background
With the development of land traffic infrastructure, the total mileage of mountain tunnels is continuously increased, and China enters the high-speed development period of tunnel construction. Asphalt concrete pavement has excellent travelling comfort and is currently the main stream form of tunnel pavement. But the main component of the asphalt material is hydrocarbon, and has combustibility. The asphalt pavement of the tunnel is in a semi-closed space, and once a fire disaster occurs, asphalt in the asphalt mixture burns to generate a large amount of toxic and harmful gas, so that the asphalt is not easy to disperse, and the life and the health of personnel in the tunnel are endangered. The flame-retardant asphalt technology is applied to the tunnel asphalt pavement, so that the possibility of tunnel fire accidents can be reduced to a certain extent, and personnel injury and property loss caused by the fire can be reduced.
The flame-retardant asphalt product at the present mainly improves the flame-retardant and smoke-suppressing performance of asphalt, but has the problems of poor compatibility of flame retardant and asphalt, poor flame-retardant and smoke-suppressing effects, high preparation cost, environmental pollution and the like, so that the application of the flame-retardant asphalt is limited. Chinese patent No. CN 116218028A discloses a pitch fire retardant, wherein the pitch fire retardant comprises the following raw materials in parts by weight: metal hydroxide: 30-60 parts of montmorillonite: 5-10 parts of hydrotalcite: 5-10 parts of nitrogen-phosphorus flame retardant: 10-50 parts of silicon flame retardant: 10-20 parts of surface modifier: 1-10 parts. The preparation method comprises the following steps: mixing and grinding the raw materials to 1000-2000 meshes, carrying out wet modification on the ground raw materials, filtering, washing and drying to obtain the finished product. The wet modification method comprises the following steps: preparing the ground raw materials into slurry by deionized water, heating to 60-110 ℃ under stirring in a reaction kettle, adding a surface modifier, and stirring and reacting at the temperature for 30-60 min. The patent can play a role in flame retardance and smoke suppression, and simultaneously controls the blending amount of the flame retardant, but the patent does not prove the influence of the flame retardant on the basic performance of asphalt, and materials such as montmorillonite and hydrotalcite can cause the asphalt material to harden. Patent CN 116218039A proposes a new asphalt composite flame retardant and a preparation method thereof, wherein the new asphalt composite flame retardant comprises 10-30 parts of organic phosphate metal salt, 20-60 parts of magnesium hydroxide, 2-5 parts of titanate coupling agent and 10-30 parts of expandable graphite; the preparation method comprises the following steps: dissolving phenol in an organic solvent, adding phosphorus oxychloride and triethylamine, reacting for a period of time to generate organic phosphorus oxychloride, and then carrying out hydrolysis reaction to obtain organic phosphate; sequentially adding the organic phosphate and the alkaline substance containing metal ions into an organic solvent to obtain organic phosphate metal salt; the titanate coupling agent and the organic solvent are mixed to prepare an organic solution, the organic metal phosphate, the expandable graphite and the magnesium hydroxide are sequentially added into the organic solution, the organic solution is filtered after being soaked for a period of time, and the obtained filter body is dried and cooled to obtain the novel flame retardant. However, the preparation process of the patent is complex, solution soaking is needed, the production is not environment-friendly, the industrial production is difficult to realize, and the flame retardant effect is general (the oxygen index value of the F-doped flame retardant in the embodiment 5 is 25.7%).
The preparation process of the flame retardant is complex, the production cost is high, and the problems of difficult application and popularization and the like exist. Based on the above, the application provides a preparation method of rare earth synergistic flame retardant modified asphalt, so as to solve the problems.
Disclosure of Invention
The application aims to solve the problems and provide a rare earth synergistic flame-retardant asphalt composition and a preparation method thereof, and the preferable technical scheme in the technical schemes provided by the application is as follows: the preparation process is simple, has little influence on the performance of the asphalt material, and has good technical effects such as flame retardance and smoke suppression effect, and the like, and is explained in detail below.
In order to achieve the above purpose, the present application provides the following technical solutions:
the application provides a rare earth synergistic flame-retardant asphalt composition, which comprises the following raw materials in parts by weight: 10 parts of composite flame retardant and 100 parts of asphalt;
wherein the composite flame retardant consists of magnesium hydroxide, a rare earth synergist, a silane coupling agent KH550 and absolute ethyl alcohol.
Preferably, the rare earth synergist is one of lanthanum oxide and cerium oxide.
Preferably, the composite flame retardant comprises the following components in percentage by mass: 9 parts of magnesium hydroxide, 1 part of rare earth synergist, 5500.09 parts of silane coupling agent KH and 0.81 part of absolute ethyl alcohol.
The preparation method of the rare earth synergistic flame retardant asphalt composition is characterized by comprising the following steps of:
s100,: preparing a composite flame retardant intermediate, namely uniformly stirring 9 parts of magnesium hydroxide and 1 part of lanthanum oxide/cerium oxide at normal temperature, and then drying the mixture in an oven to prepare the composite flame retardant intermediate;
s200, namely: preparing a composite flame retardant, mixing 0.009 parts of a silane coupling agent KH500 with 0.81 parts of absolute ethyl alcohol to prepare 0.9 parts of treatment liquid, uniformly spraying the treatment liquid onto the surface of a composite flame retardant intermediate, and mixing the treatment liquid and the intermediate uniformly while stirring to obtain the composite flame retardant;
s300: preparing flame-retardant asphalt, adding the composite flame retardant into 100 parts of heated asphalt, shearing and dispersing by a high-speed shearing machine, and preserving heat and developing for 20min to obtain the flame-retardant asphalt.
Preferably, in step S100, the stirring time of magnesium hydroxide and lanthanum oxide/cerium oxide is 5mi n.
Preferably, in step S100, the oven temperature is 160℃and the drying time is 30min.
Preferably, in step S200, the treatment solution and the composite flame retardant intermediate are uniformly mixed and then dried at 65 ℃ for 1,5 hours.
Preferably, in step S300, the asphalt is a matrix asphalt or a modified asphalt, wherein the heating temperature and the heat preservation temperature of the matrix asphalt are 160 ℃ and the heating temperature and the heat preservation temperature of the modified asphalt are 180 ℃.
Preferably, in step S300, the high-speed shearing machine may be replaced by a colloid mill, and the rotation speed of the colloid mill is 4000r/min.
In summary, the application has the following beneficial effects: by adopting the magnesium hydroxide, the nanometer lanthanum oxide/cerium oxide synergistic flame retardant and the asphalt to be fused, the asphalt not only can have high-efficiency flame retardance and smoke suppression performance, but also can eliminate the emission of pollutants in the pavement process, reduce the emission of toxic substances in the flame retardance process, improve the pavement construction working environment of the pavement in a tunnel, reduce the physical health burden of constructors, but also can greatly reduce the fire loss and casualties of a highway tunnel, improve the driving safety and prolong the service life of the pavement of the highway tunnel.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a photograph of a composite flame retardant of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, based on the examples herein, which are within the scope of the application as defined by the claims, will be within the scope of the application as defined by the claims.
The application provides a rare earth synergistic flame-retardant asphalt composition, which comprises the following raw materials in parts by weight: 10 parts of composite flame retardant and 100 parts of asphalt;
the composite flame retardant consists of magnesium hydroxide, a rare earth synergist, a silane coupling agent KH550 and absolute ethyl alcohol, wherein the rare earth synergist is one of lanthanum oxide and cerium oxide. The magnesium hydroxide is industrial magnesium hydroxide, mg (OH) 2 The effective content of the magnesium hydroxide is not less than 90 percent, the mesh number of the magnesium hydroxide is 3000-5000 meshes,the mesh number of lanthanum oxide and cerium oxide is 18000 mesh, the concentration of the silane coupling agent KH550 is 97.7wt%, and the analytically pure concentration of absolute ethyl alcohol is 95wt%;
the composite flame retardant comprises the following components in percentage by mass: 9 parts of magnesium hydroxide, 1 part of rare earth synergist, 5500.09 parts of silane coupling agent KH and 0.81 part of absolute ethyl alcohol.
The preparation method of the rare earth synergistic flame retardant asphalt composition is characterized by comprising the following steps of:
s100,: preparing a composite flame retardant intermediate, namely stirring 9 parts of magnesium hydroxide and 1 part of lanthanum oxide/cerium oxide at normal temperature for 5min until the mixture is uniformly mixed, and then drying the mixture in an oven to obtain the composite flame retardant intermediate, wherein the temperature of the oven is 160 ℃, and the drying time is 30 min;
s200, namely: preparing a composite flame retardant, mixing 0.009 parts of a silane coupling agent KH500 with 0.81 parts of absolute ethyl alcohol to prepare 0.9 parts of treatment liquid, uniformly spraying the treatment liquid onto the surface of an intermediate of the composite flame retardant, and stirring the treatment liquid and the intermediate of the composite flame retardant while spraying to uniformly mix the treatment liquid and the intermediate of the composite flame retardant, and drying the mixture at 65 ℃ for 1 and 5 hours to obtain the composite flame retardant;
s300: preparing flame-retardant asphalt, adding the composite flame retardant into 100 parts of asphalt in a heating state, shearing and dispersing (4000 r/min) by a high-speed shearing machine (or a colloid mill), and preserving heat and developing for 20min to obtain the flame-retardant asphalt; the asphalt is matrix asphalt or modified asphalt, wherein the heating temperature and the heat preservation temperature of the matrix asphalt are 160 ℃ and 180 ℃ respectively.
Specific examples are as follows:
example 1:
comprises 9 parts of magnesium hydroxide, 1 part of lanthanum oxide, 5500.09 parts of silane coupling agent KH, 0.81 part of absolute ethyl alcohol and 100 parts of matrix asphalt;
example 2
Comprises 9 parts of magnesium hydroxide, 1 part of cerium oxide, 5500.09 parts of silane coupling agent KH, 0.81 part of absolute ethyl alcohol and 100 parts of matrix asphalt;
example 3
Comprises 9 parts of magnesium hydroxide, 1 part of cerium oxide, 5500.09 parts of silane coupling agent KH, 0.81 part of absolute ethyl alcohol and 100 parts of modified asphalt;
after setting matrix asphalt, 10% magnesium hydroxide+90% matrix asphalt and SBS modified asphalt as three sets of comparative examples, limiting oxygen index test, penetration and softening point test were performed for each of the comparative examples and examples, and the formulation table of examples is shown in Table 1:
numbering device Formulation of (Code)
Comparative example 1 Matrix asphalt SDJZ
Comparative example 2 10% magnesium hydroxide+90% matrix asphalt 10%M-SDJZ
Example 1 10% composite flame retardant (lanthanum oxide synergistic flame retardant) +90% matrix asphalt 10%ML-SDJZ
Example 2 10% composite flame retardant (cerium oxide synergistic flame retardant) +90% matrix asphalt 10%MS-SDJZ
Comparative example 3 SBS modified asphalt SBS
Example 3 10% composite flame retardant (lanthanum oxide synergistic flame retardant) +90% matrix asphalt 10%ML-SBS
TABLE 1
The experimental results are shown in table 2:
TABLE 2
As can be seen from table 2, the limiting oxygen index value of example 1 (10% ml-SDJZ, rare earth synergistic flame retardant asphalt with lanthanum oxide added) is 26.5%, the limiting oxygen index value of example 2 (10% ms-SDJZ, rare earth synergistic flame retardant asphalt with cerium oxide added) is 27.8%, which is much higher than that of comparative example 1 (SDJZ, base asphalt), and higher than that of comparative example 2 (only magnesium hydroxide as flame retardant), and the addition of synergistic flame retardant has a significant effect on the improvement of flame retardant properties of asphalt.
On the other hand, as can be seen from table 2, after the matrix asphalt is modified by the flame retardant, the softening point is slightly improved, which indicates that the two flame retardants have a certain improvement effect on the high temperature stability of the asphalt, and the penetration is slightly reduced, which indicates that the addition of the flame retardant can improve the modulus of the asphalt to a certain extent and improve the deformation resistance of the asphalt.
Meanwhile, it can be seen from Table 2 that the limiting oxygen index of example 3 (10% ML-SBS, lanthanum oxide-added rare earth synergistic flame retardant SBS modified asphalt) is as high as 27.1%, which is far higher than that of comparative example 3 (SBS modified asphalt), and the flame retardant effect of the composite flame retardant is excellent. And the addition of the composite flame retardant has little influence on the basic performance of the SBS modified asphalt.
In conclusion, the flame-retardant asphalt prepared by adopting the scheme of the application has excellent flame-retardant effect, has no negative influence on the performance of asphalt, and even has certain positive promotion on the performance of matrix asphalt.
The foregoing is merely illustrative of the present application, and the present application is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.

Claims (9)

1. The rare earth synergistic flame-retardant asphalt composition is characterized by comprising the following raw materials in parts by weight: 10 parts of composite flame retardant and 100 parts of asphalt;
wherein the composite flame retardant consists of magnesium hydroxide, a rare earth synergist, a silane coupling agent KH550 and absolute ethyl alcohol.
2. The rare earth synergistic flame retardant asphalt composition of claim 1, wherein the rare earth synergistic agent is one of lanthanum oxide and cerium oxide.
3. The rare earth synergistic flame retardant asphalt composition according to claim 2, wherein the composite flame retardant comprises the following components in percentage by mass: 9 parts of magnesium hydroxide, 1 part of rare earth synergist, 5500.09 parts of silane coupling agent KH and 0.81 part of absolute ethyl alcohol.
4. A method of preparing a rare earth synergistic flame retardant asphalt composition using the method of claim 3, comprising the steps of:
s100,: preparing a composite flame retardant intermediate, namely uniformly stirring 9 parts of magnesium hydroxide and 1 part of lanthanum oxide/cerium oxide at normal temperature, and then drying the mixture in an oven to prepare the composite flame retardant intermediate;
s200, namely: preparing a composite flame retardant, mixing 0.009 parts of a silane coupling agent KH500 with 0.81 parts of absolute ethyl alcohol to prepare 0.9 parts of treatment liquid, uniformly spraying the treatment liquid onto the surface of a composite flame retardant intermediate, and mixing the treatment liquid and the intermediate uniformly while stirring to obtain the composite flame retardant;
s300: preparing flame-retardant asphalt, adding the composite flame retardant into 100 parts of heated asphalt, shearing and dispersing by a high-speed shearing machine, and preserving heat and developing for 20 minutes to obtain the flame-retardant asphalt.
5. The rare earth synergistic flame retardant asphalt composition and its preparation method as claimed in claim 4, wherein in step S100, the stirring time of magnesium hydroxide and lanthanum oxide/cerium oxide is 5min.
6. The rare earth synergistic flame retardant asphalt composition and its preparation method as claimed in claim 4, wherein in step S100, the oven temperature is 160℃and the drying time is 30min.
7. The rare earth synergistic flame retardant asphalt composition and the preparation method thereof according to claim 4, wherein in step S200, the treatment liquid and the composite flame retardant intermediate are uniformly mixed and then dried at 65 ℃ for 1,5 hours.
8. The rare earth synergistic flame retardant asphalt composition and its preparation method as claimed in claim 4, wherein in step S300, the asphalt is matrix asphalt or modified asphalt, wherein the heating temperature and the heat preservation temperature of the matrix asphalt are 160 ℃ and the heating temperature and the heat preservation temperature of the modified asphalt are 180 ℃.
9. The rare earth synergistic flame retardant asphalt composition and its preparation method as claimed in claim 4, wherein in step S300, the high speed shearing machine may be replaced by a colloid mill, and the rotation speed of the colloid mill is 4000r/min.
CN202310820733.9A 2023-07-06 2023-07-06 Rare earth synergistic flame-retardant asphalt composition and preparation method thereof Pending CN116814087A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59227935A (en) * 1983-06-10 1984-12-21 Furukawa Electric Co Ltd:The Flame-retarding polyolefin resin composition
CN101709123A (en) * 2009-12-27 2010-05-19 长沙理工大学 Nano asphalt flame-retardant smoke inhibition modifying agent and preparation thereof
CN104629256A (en) * 2015-03-03 2015-05-20 北京奥格森新材料科技有限公司 Flame-retardant smoke inhibitor for sprayed polyurethane foam as well as preparation method and application of flame-retardant smoke inhibitor
CN110204784A (en) * 2019-05-23 2019-09-06 长沙理工大学 A kind of asphalt flame-retardant agent and preparation method and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59227935A (en) * 1983-06-10 1984-12-21 Furukawa Electric Co Ltd:The Flame-retarding polyolefin resin composition
CN101709123A (en) * 2009-12-27 2010-05-19 长沙理工大学 Nano asphalt flame-retardant smoke inhibition modifying agent and preparation thereof
CN104629256A (en) * 2015-03-03 2015-05-20 北京奥格森新材料科技有限公司 Flame-retardant smoke inhibitor for sprayed polyurethane foam as well as preparation method and application of flame-retardant smoke inhibitor
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Title
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