CN112831190B - Asphalt with anti-freezing function prepared from salt-storage sludge particles - Google Patents
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Abstract
The invention discloses asphalt with an anti-freezing function, which is prepared from salt-storage sludge particles, and comprises the following components in parts by weight: 3-5 parts of salt-storage sludge particles, 94-96.5 parts of commercially available SBS modified asphalt and 0.5-1 part of coupling agent. The invention also discloses salt-storage sludge particles for preparing asphalt with an anti-freezing function, which are obtained by neutralizing and adjusting acidic and alkaline waste water generated in the preparation of rare earth chloride by an alkaline process, pressing, filtering, drying and grinding solid waste. The preparation method of the asphalt with the anti-freezing function is simple, the usage amount of sodium chloride in the traditional salt spreading and deicing process can be greatly reduced, the recycling, high-value and reduction treatment of sludge is realized, and the sustainable development and the circular economy development of the industry are promoted. Further experiments prove that the anti-freezing asphalt has an anti-freezing effect on surface supercooled water drops in a temperature range of 0 ℃ to-10 ℃ and has a long-term anti-freezing effect.
Description
Technical Field
The invention relates to asphalt with an anti-freezing function, in particular to asphalt with an anti-freezing function prepared by salt-storage sludge particles, belonging to the technical field of pavement engineering materials.
Background
In winter and under special severe cold weather conditions, snow and ice can be accumulated on the road surface, so that the anti-skid capability of the road surface is reduced, the friction coefficient between the vehicle tire and the road surface is reduced, and the adhesion capability is reduced. On the other hand, traffic accidents cause road congestion and even traffic interruption, which brings great inconvenience to traffic transportation.
The anti-freezing asphalt material is reported at home and abroad currently, for example, the Chinese patent with the application number of 201510060163.3 discloses a preparation method of anti-freezing asphalt, which is prepared by adding self-made anti-freezing ice filler and quartz powder into molten asphalt, uniformly stirring, pouring into a preheated aluminum mold while the mixture is hot for natural leveling, cooling to room temperature, and then polishing the surface of a sample by using metallographic abrasive paper with a certain mesh number. For example, chinese patent application No. 201010100931.0 discloses an anti-freezing road surface salt-storage seal and a construction method thereof, wherein a crushed stone aggregate layer composed of crushed stone aggregates is arranged on an asphalt upper layer, gaps of the crushed stone aggregate layer are filled with modified asphalt binder, and a sodium chloride particle layer which is formed by sodium chloride particles which are firstly subjected to hydrophobic treatment and is subjected to hydrophobic treatment is laid on the crushed stone aggregate layer and the modified asphalt binder. The pretreated sodium chloride particles have hydrophobic property, can effectively prevent the loss of the salt storage components, and have controllability on release. However, the research and development of the existing anti-freezing agent for the asphalt material mainly consider surface coating of chloride salt and controlled release treatment of a porous medium, and relate to complex physical and chemical processes, which are not beneficial to large-scale production and application. Through the research of literature, no report is found about pitch with the function of anti-freezing, which is prepared by using solid waste, namely salt-storage sludge particles, generated in the rare earth industry to greatly reduce the using amount of sodium chloride in the traditional salting deicing.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the asphalt with the function of resisting ice coagulation, which is prepared by utilizing the salt storage sludge particles.
The invention relates to asphalt with an anti-freezing function prepared by utilizing salt-storage sludge particles, which is characterized by comprising the following components in parts by weight: the asphalt comprises the following components in parts by weight: 3-5 parts of salt-storage sludge particles, 94-96.5 parts of commercially available SBS modified asphalt and 0.5-1 part of coupling agent.
The preferred embodiment of the asphalt with the function of anti-freezing prepared by using the salt-storage sludge particles is as follows: the asphalt comprises the following components in parts by weight: 4 parts of salt-storage sludge particles, 95.2 parts of SBS modified asphalt and 0.8 part of coupling agent.
In the above asphalt with an anti-freezing function prepared by using the salt-storing sludge particles: the salt-storage sludge particles are obtained by neutralizing and adjusting acidic and alkaline waste water generated in the preparation of rare earth chloride by an alkaline process, filtering by pressing cakes, drying and grinding; the content of sodium chloride in the salt-storage sludge particles is 24% +/-2% in percentage by weight; the particle size of the salt-storage sludge particles is less than 0.075 mm.
In the above asphalt with an anti-freezing function prepared by using the salt-storing sludge particles: the content of each element in the salt-storage sludge particles is, by weight, 19.92% of Si, 1.25% of Al, 17.00% of Fe, 37.52% of Ca, 0.76% of Mg, 3.90% of S, 0.05% of K, 6.43% of Na, 0.10% of Mn, 8.75% of P and 4.139% of Cl.
In the above asphalt with an anti-freezing function prepared by using the salt-storing sludge particles: the coupling agent is a silane coupling agent KH550, a silane coupling agent KH560, a silane coupling agent KH570, a silane coupling agent A151, a silane coupling agent A171 or a silane coupling agent A172.
More preferably, the coupling agent is a silane coupling agent KH560 or a silane coupling agent a 171.
The preparation method of the asphalt with the function of anti-freezing, which is prepared by utilizing the salt-storage sludge particles, comprises the following steps:
weighing salt-storage sludge particles, SBS modified asphalt and a coupling agent according to the weight parts required by the formula;
secondly, the SBS modified asphalt is heated to a molten state in a temperature control furnace, and then the salt-storage sludge particles and the coupling agent are sequentially added into the molten asphalt and uniformly stirred to obtain the asphalt with the ice coagulation preventing function.
The invention also provides salt-storage sludge particles for preparing the asphalt with the function of resisting ice coagulation, which are characterized in that: the salt-storage sludge particles are obtained by neutralizing and adjusting acidic and alkaline waste water generated in the preparation of rare earth chloride by an alkaline process, filtering by pressing cakes, drying and grinding; the content of sodium chloride in the salt-storage sludge particles is 24% +/-2% in percentage by weight; the particle size of the salt-storage sludge particles is less than 0.075 mm; the content of each element in the salt-storage sludge particles is, by weight, 19.92% of Si, 1.25% of Al, 17.00% of Fe, 37.52% of Ca, 0.76% of Mg, 3.90% of S, 0.05% of K, 6.43% of Na, 0.10% of Mn, 8.75% of P and 4.139% of Cl.
The invention relates to application of salt-storage sludge particles for preparing asphalt with an anti-freezing function in preparation of asphalt with the anti-freezing function by doping the salt-storage sludge particles into asphalt mucilage or asphalt mixture.
The research of the applicant proves that the sludge generated in the process of extracting the rare earth ore by the alkaline method contains a large amount of sodium chloride, and the sludge can become salt storage filler and asphalt anti-freezing agent after drying and granulation. Meanwhile, the salt-storage sludge particles used in the invention are used as anti-freezing agent filler, so that the use value of solid waste is improved, and the sustainable development of industrial production is promoted.
Compared with the prior art, the invention has the outstanding advantages that: (1) the salt-storage sludge particles are derived from solid wastes generated in the rare earth industry, so that high-valued and large-scale application of the solid wastes is realized; (2) the preparation method of the asphalt with the function of anti-freezing, which is prepared by utilizing the salt storage sludge particles, is simple, and can greatly reduce the sodium chloride dosage in the traditional salt spreading deicing; (3) the asphalt provided by the invention has an anti-freezing effect on surface supercooled water drops at the temperature range of 0-10 ℃, and experiments prove that the asphalt also has a long-term anti-freezing effect, and has a wide application prospect.
Drawings
FIG. 1 is a field emission scanning electron microscope image of salt-accumulating sludge particles.
FIG. 2 is an EDS spectrum analysis of a saline sludge particle field emission scanning electron microscope.
FIG. 3 shows the result of XRD (X-ray diffraction) analysis of the salt-accumulating sludge particles.
Detailed Description
The present invention will be described in detail with reference to the following detailed drawings and examples. The following examples are only preferred embodiments of the present invention, and it should be noted that the following descriptions are only for explaining the present invention and not for limiting the present invention in any form, and any simple modifications, equivalent changes and modifications made to the embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
In the following examples, the SBS modified asphalt, the coupling agent, were all commercially available.
The alkaline process for preparing rare earth chloride and salt-storage sludge particles comprises the following steps:
and (3) putting the rare earth concentrate into a reactor, and removing impurities from the rare earth concentrate by controlling the temperature and hydrochloric acid according to a conventional method. And (3) putting the rare earth concentrate and flake caustic soda after impurity removal into a reactor for an alkalization reaction, and discharging the materials after controlling the qualified alkali conversion rate. Then the material is put into a water washing tank, clean water is added for washing, and the material is put into an intermediate water washing tank for storage after being washed to be neutral. And (3) putting the qualified washed material into an enamel reaction kettle, adding hydrochloric acid according to a conventional amount, and carrying out a dissolution reaction at a high temperature to convert the rare earth hydroxide into a rare earth chloride solution. And then controlling and adjusting the pH value of the feed liquid by adding soda ash, and adjusting the pH value of the feed liquid back to be qualified to obtain the rare earth chloride. The sediment and sludge generated by slag washing in the preparation of rare earth chloride, namely solid waste, are filtered, dried and ground by pressing cakes to prepare particles, namely salt-storage sludge particles.
Example 1:
taking 3 parts (unit: kilogram) of salt-storage sludge particles, 96.5 parts (unit: kilogram) of SBS modified asphalt and 1710.5 parts (unit: kilogram) of silane coupling agent KH560 or silane coupling agent A.
The SBS modified asphalt is heated to a molten state in a temperature control furnace, and then the salt-storage sludge particles and the coupling agent are sequentially added into the molten asphalt and uniformly stirred to obtain the asphalt with the ice coagulation preventing function.
Example 2:
taking 4 parts (unit: kilogram) of salt-storage sludge particles, 95.2 parts (unit: kilogram) of SBS modified asphalt and 1710.8 parts (unit: kilogram) of silane coupling agent KH560 or silane coupling agent A.
The SBS modified asphalt is heated to a molten state in a temperature control furnace, and then the salt-storage sludge particles and the coupling agent are sequentially added into the molten asphalt and uniformly stirred to obtain the asphalt with the ice coagulation preventing function.
Example 3:
5 parts (unit: kilogram) of salt-storage sludge particles, 94 parts (unit: kilogram) of SBS modified asphalt and 1711 parts (unit: kilogram) of silane coupling agent KH560 or silane coupling agent A are taken.
The SBS modified asphalt is heated to a molten state in a temperature control furnace, and then the salt-storage sludge particles and the coupling agent are sequentially added into the molten asphalt and uniformly stirred to obtain the asphalt with the ice coagulation preventing function.
Example 4:
4.2 parts (unit: kilogram) of salt-storage sludge particles, 95.1 parts (unit: kilogram) of SBS modified asphalt and KH550 parts or KH 5700.7 parts (unit: kilogram) of silane coupling agent are taken.
The SBS modified asphalt is heated to a molten state in a temperature control furnace, and then the salt-storage sludge particles and the coupling agent are sequentially added into the molten asphalt and uniformly stirred to obtain the asphalt with the ice coagulation preventing function.
Example 5:
taking 4.5 parts (unit: kilogram) of salt-storage sludge particles, 94.5 parts (unit: kilogram) of SBS modified asphalt and 1721 parts (unit: kilogram) of silane coupling agent A151 or silane coupling agent A.
The SBS modified asphalt is heated to a molten state in a temperature control furnace, and then the salt-storage sludge particles and the coupling agent are sequentially added into the molten asphalt and uniformly stirred to obtain the asphalt with the ice coagulation preventing function.
Example 6:
the ice-freezing results of the test pieces of examples 1, 2 and 3 were observed under 3 different temperatures (-10 deg.C, -5 deg.C and-2 deg.C), and the ice-freezing conditions were observed every 60min, and the results are shown in Table 1.
Table 1: observation of the freezing result of the anti-freezing asphalt prepared in examples 1 to 3 of the present invention
Note: a-is not frozen; b-a small amount of thin ice on the surface; the C-surface is all frozen into thin ice; d-the surface is formed into thick ice but the bottom is not frozen; e-icing on the surface but not icing a small amount of water on the bottom; f-all frozen.
Further experiments also prove that the anti-freezing asphalt has long-term anti-freezing effect.
Example 7:
preparation of rare earth chloride for salt storage sludge particles by combining alkaline process
1. Chemical selection: rare earth concentrate is put into a reactor, the temperature is controlled to be 85-90 ℃, the acidity, namely the concentration of HCl solution, is 2.0 +/-0.2 mol/L, and the concentrate is subjected to impurity removal. And discharging the waste liquid into a sludge tank. The reaction formula is as follows:
CaCO3+2HCl→CaCl2+H2O+CO2
RE2(CO3).REF3+6HCl→2RECl3+REF3+3H2O+3CO2
2. alkaline hydrolysis: and (3) putting the rare earth concentrate and flake caustic soda after impurity removal into a reactor (tank) for an alkalization reaction, and discharging after controlling the qualified alkali conversion rate. Wherein the alkali decomposition reaction formula is:
decomposition of bastnasite: REFCO3+3NaOH→RE(OH)3+NaF+Na2CO3
Decomposition of monazite: REPO4+3NaOH→RE(OH)3+Na3PO4
3. Washing with water: and adding clear water into the alkali conversion material after the alkali conversion is qualified in a washing tank for washing until the pH value is 7, then putting the alkali conversion material into an intermediate washing tank for storage, and discharging the waste water into a sludge pond.
4. And (3) preferential dissolution: and (3) putting the qualified washed material into an enamel reaction kettle, adding hydrochloric acid to control the reaction end point to be pH2.0-2.5, and carrying out a dissolution reaction at 85-95 ℃ to convert the rare earth hydroxide into a rare earth chloride solution.
RE(OH)3+3HCl→RECl3+3H2O
5. And (3) callback: siphoning the supernatant after the preferential dissolution into a reduction tank, and adding sulfuric acid or barium chloride to adjust SO in the feed liquid4 2-And Ba2+Adjusting the pH value of the feed liquid to 4.0-4.5 by adding soda ash to control and adjust the Fe in the feed liquid when the content is qualified3+The content is qualified. The residue is washed with water and the waste liquid is discharged into a sludge tank.
6. Concentration: and the supernatant in the callback process is boiled by steam so as to enable the concentration of the rare earth chloride feed liquid to reach the standard.
7. Adding sodium carbonate into the supernatant generated in the slag washing process for carbon precipitation, and returning the rare earth carbonate generated by carbon precipitation to the callback process for reuse. The reaction formula is as follows:
2RECl3+3Na2CO3＝RE2(CO3)3+6NaCl
8. the sediment and the sludge generated by the washing slag discharged into the sludge tank in the process of preparing the rare earth chloride are solid wastes, and the solid wastes are filtered by pressing cakes, dried and ground to prepare particles, namely the salt-storage sludge particles.
The content of sodium chloride in the salt-storage sludge particles is 24% +/-2% in percentage by weight; the particle size of the salt-storage sludge particles is less than 0.075 mm; the image of the saline sludge particle field emission scanning electron microscope is shown in figure 1. The EDS energy spectrum analysis chart of the salt-storage sludge particle field emission scanning electron microscope is shown in figure 2. The XRD (X-ray diffraction) analysis of the salt-accumulating sludge particles is shown in FIG. 3. The results of XRF (X-ray fluorescence spectroscopy) analysis of the saline sludge particles are shown in Table 2.
Table 2: XRF analysis result of salt-storing sludge particles
| Element(s) | Si | Al | Fe | Ca | Mg | S |
| Content (wt.%) | 19.92 | 1.25 | 17.00 | 37.52 | 0.76 | 3.90 |
| Element(s) | K | Na | Mn | P | Cl | |
| Content (wt.%) | 0.05 | 6.43 | 0.10 | 8.75 | 4.139 |
Claims (7)
1. The utility model provides an utilize pitch that holds salt sludge granule preparation and have anti-freezing function which characterized in that: the asphalt comprises the following components in parts by weight: 3-5 parts of salt-storage sludge particles, 94-96.5 parts of commercially available SBS modified asphalt and 0.5-1 part of coupling agent; wherein the salt-storage sludge particles are obtained by neutralizing and adjusting acidic and alkaline waste water generated in the preparation of rare earth chloride by an alkaline process, filtering by pressing cakes, drying and grinding; the content of each element in the salt-storage sludge particles is 19.92 percent of Si, 1.25 percent of Al, 17.00 percent of Fe, 37.52 percent of Ca, 0.76 percent of Mg, 3.90 percent of S, 0.05 percent of K, 6.43 percent of Na, 0.10 percent of Mn, 8.75 percent of P and 4.139 percent of Cl; the particle size of the salt-storage sludge particles is less than 0.075 mm.
2. The asphalt with the function of resisting ice coagulation prepared by utilizing the salt-accumulating sludge granules according to claim 1, which is characterized in that: the asphalt comprises the following components in parts by weight: 4 parts of salt-storage sludge particles, 95.2 parts of commercially available SBS modified asphalt and 0.8 part of coupling agent.
3. The asphalt with an anti-freezing function prepared by using the salt-accumulating sludge granules according to claim 1 or 2, which is characterized in that: the coupling agent is a silane coupling agent KH550, a silane coupling agent KH560, a silane coupling agent KH570, a silane coupling agent A151, a silane coupling agent A171 or a silane coupling agent A172.
4. The asphalt with the function of resisting ice coagulation prepared by utilizing the salt-accumulating sludge granules according to claim 3, characterized in that: the coupling agent is a silane coupling agent KH560 or a silane coupling agent A171.
5. The method for preparing asphalt with anti-freezing function by using the salt-accumulating sludge granules as claimed in claim 1, comprises the following steps:
6. A salt-storage sludge particle for preparing asphalt with an anti-freezing function is characterized in that: the salt-storage sludge particles are obtained by neutralizing and adjusting acidic and alkaline waste water generated in the preparation of rare earth chloride by an alkaline process, filtering by pressing cakes, drying and grinding; the content of each element in the salt-storage sludge particles is 19.92 percent of Si, 1.25 percent of Al, 17.00 percent of Fe, 37.52 percent of Ca, 0.76 percent of Mg, 3.90 percent of S, 0.05 percent of K, 6.43 percent of Na, 0.10 percent of Mn, 8.75 percent of P and 4.139 percent of Cl; the particle size of the salt-storage sludge particles is less than 0.075 mm.
7. The use of the salt-accumulating sludge granules of claim 6 for preparing asphalt with anti-freezing function in asphalt cement or asphalt mixture for preparing asphalt with anti-freezing function.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935658A (en) * | 2006-09-25 | 2007-03-28 | 包头市图南稀土有限责任公司 | Method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride |
| CN101092295A (en) * | 2007-05-22 | 2007-12-26 | 当阳市公路管理段 | Rare earth modified cold repaired maintenance material for asphalt pavement, and preparation method |
| WO2012107022A2 (en) * | 2011-02-08 | 2012-08-16 | Universität Rostock | Method for purifying biogas, flue gas or liquids, adsorbent therefor, filters, and use of the adsorbent |
| CN111470798A (en) * | 2019-01-24 | 2020-07-31 | 交通运输部科学研究院 | Long-acting slow-release black anti-freezing ice modifier for asphalt pavement and preparation method thereof |
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- 2021-01-11 CN CN202110033169.7A patent/CN112831190B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935658A (en) * | 2006-09-25 | 2007-03-28 | 包头市图南稀土有限责任公司 | Method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride |
| CN101092295A (en) * | 2007-05-22 | 2007-12-26 | 当阳市公路管理段 | Rare earth modified cold repaired maintenance material for asphalt pavement, and preparation method |
| WO2012107022A2 (en) * | 2011-02-08 | 2012-08-16 | Universität Rostock | Method for purifying biogas, flue gas or liquids, adsorbent therefor, filters, and use of the adsorbent |
| CN111470798A (en) * | 2019-01-24 | 2020-07-31 | 交通运输部科学研究院 | Long-acting slow-release black anti-freezing ice modifier for asphalt pavement and preparation method thereof |
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