CN112266769B - Degradable anti-freezing material for cement concrete pavement and preparation method thereof - Google Patents
Degradable anti-freezing material for cement concrete pavement and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of road pavement anti-freezing and deicing materials, and particularly relates to a degradable anti-freezing material for a cement concrete pavement and a preparation method thereof. The preparation method comprises the following steps: crushing an antifreeze material core material to a granularity of about 200 meshes, mixing the antifreeze material core material with a silane coupling agent, heating, stirring and cooling, mixing the antifreeze material with epoxy resin, a degradable component and isocyanate under a heating condition, forming under the pressure of not less than 3KN per square centimeter, and crushing after cooling to obtain the degradable antifreeze material of about 1 mm.
Description
Technical Field
The invention belongs to the field of road pavement anti-freezing and deicing materials, and particularly relates to a degradable anti-freezing material for a cement concrete pavement and a preparation method thereof.
Background
In the period of rapid increase of traffic transportation in China, in order to ensure the smoothness of roads and driving safety and avoid traffic accidents, the research on measures for preventing snow and removing snow on the roads to ensure the smoothness and safety of the roads in snowing weather in winter is the most important in traffic transportation work, and the effective measures for preventing snow and removing snow are adopted, so that the method has very important economic benefit and social significance. The active ice suppression technology is characterized in that related technologies are adopted in advance or special materials are added into a mixture in road construction or overhaul to enable a road surface to have special functions so as to achieve the purpose of snow melting and deicing, and a salinized substance self-snow melting road surface is one of the road surfaces. The addition of the salinization anti-freezing material in the asphalt or concrete mixture enables the pavement to have the snow and ice melting capability. The construction process is simple and the effect is good, so the method is applied.
At present, the antifreeze material is added into asphalt concrete generally, and the research on adding the antifreeze material into cement concrete is less, because a large amount of water is introduced in the mixing process of the cement concrete. And the ice inhibiting component is easy to disperse in the cement concrete by continuous stirring, so that the pavement is difficult to melt ice and snow for a long time.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a degradable antifreezing material for a cement concrete pavement and a preparation method thereof.
The degradable antifreezing material for the cement concrete pavement is prepared from an anti-icing core material and a degradable membrane material, wherein the core material is mainly one or more of calcium chloride, sodium chloride, magnesium chloride, calcium acetate, magnesium acetate or potassium acetate, and the degradable membrane material is composed of a silane coupling agent, epoxy resin, tung oil, a degradable component and an isocyanate curing agent.
Wherein the silane coupling agent is one or a mixture of two of gamma-aminopropyltriethoxysilane (KH-550 for short) and gamma- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560 for short).
The epoxy resin is one or two of bisphenol A epoxy resin, bisphenol F epoxy resin and bisphenol F/A copolymerization epoxy resin.
The degradable component is one of polylactic acid or polycaprolactone, wherein the molecular weight of the polylactic acid is 40000-70000.
The isocyanate is one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI) and Hexamethylene Diisocyanate (HDI).
The granularity of the anti-freezing ice core material is not more than 200 meshes (75 micrometers), and the large-particle core material needs to be crushed.
The mass ratio of the anti-icing core material to the degradable film material is as follows: 1:0.06-0.08; the mass ratio of the anti-icing core material to the silane coupling agent is 1:0.01-0.02, wherein the mass ratio of the epoxy resin to the degradable components is 1:0.3-0.45, wherein the mass ratio of the epoxy resin to the tung oil is 1:0.05-0.1, and the mass ratio of the epoxy resin to the isocyanate is 1.
The invention also provides a preparation method of the anti-freezing material with the degradable characteristic for the cement concrete pavement, which comprises the following steps:
(1) Heating the anti-freezing ice core material to a reaction temperature, adding a silane coupling agent, stirring at a constant temperature, naturally cooling after stirring for a period of time, and standing for a period of time to obtain the blend 1.
The reaction temperature is 70-80 deg.C, stirring time is 5-15min, and standing time is 30-40min.
(2) Heating the degradable component and the epoxy resin to a reaction temperature, adding the blend 1 prepared in the step (1) after the degradable component is completely melted, continuously stirring for the first time, adding isocyanate after stirring for a period of time, continuously stirring for the second time at the reaction temperature for a period of time, and finally adding tung oil, continuously stirring for the third time for a period of time to prepare a blend 2.
The reaction temperature is 130-155 ℃, the first stirring time is 3-5min, the second stirring time is 5-10min, and the third stirring time is 10-15min.
(3) And (3) pouring the blend prepared in the step (2) into a tablet machine die for tabletting to prepare the flaky anti-freezing material, and naturally cooling the flaky anti-freezing material.
And (4) performing tabletting operation in the step (3), wherein the unit square centimeter pressure is not less than 3KN, and the tabletting time is not less than 180 seconds.
(4) And (4) crushing the flaky anti-freezing material prepared in the step (3), and taking particles with the particle size of 0.5mm-2 mm. The final product is used as the degradable antifreezing material of the cement concrete pavement.
The working principle of the invention is as follows:
the siloxy groups in the silane coupling agent are reactive with inorganic substances, and the organic functional groups are reactive or compatible with organic substances. Thus, when a silane coupling agent is interposed between the inorganic and organic interfaces, a bonding layer of organic matrix-silane coupling agent-inorganic matrix may be formed. Therefore, the silane coupling agent is added to increase the adhesive force between the epoxy resin and the inorganic salt compound and improve the adhesive property. Because the epoxy resin with strong hydrophobicity is introduced, and the degradable components and the epoxy resin completely fill the gaps between the salinization products under the high-pressure condition, the antifreeze material can not be released in the mixing process of the antifreeze material and the cement concrete, and meanwhile, the toughness after the salinization products are bonded is greatly enhanced while the hydrophobicity is increased by adding the tung oil, so that the antifreeze material can bear the extrusion abrasion in the concrete mixing process. When the antifreeze material is paved into concrete, degradable components can be degraded along with the time, so that the original compact structure is broken, and the salinized substance can be smoothly released.
The invention has the beneficial effects that:
the antifreeze material with the degradable characteristic prepared by the invention can adapt to long-time stirring of a concrete mixing tank without releasing the ice melting component, and the film material can be partially decomposed along with the passage of time when the antifreeze material is paved in a road, so that the ice melting component is released, and the effects of melting snow and ice are achieved. The material cost of the invention is low, the invention is mature industrial product, the invention is convenient for large-scale production and use, and has strong application value.
Detailed Description
The present invention is further described below with reference to examples, but is not limited thereto.
Example 1
(1) 100g of powdered anhydrous calcium chloride was weighed. Heating and stirring at 70 ℃, adding 2g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) Heating and stirring 1g of polylactic acid with the molecular weight of 70000 and 2.35g of bisphenol F/A copolymerized epoxy resin NPEF-175 at 155 ℃, adding the blend prepared in the step (1) into the mixture and stirring the mixture for 3min after the polylactic acid is completely melted, adding 2.35g of dicyclohexylmethane diisocyanate (HMDI) at the reaction temperature of 155 ℃, stirring the mixture for 5min, finally adding 0.23g of tung oil and continuously stirring the mixture for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making the degradable antifreezing material for cement concrete road.
Example 2
(1) 80g of sodium chloride is weighed and crushed to 200 meshes, and then 20g of powdered calcium acetate is added. Heating and stirring at 70 ℃, adding 1g of silane coupling agent KH-560, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) Heating and stirring 1g of polylactic acid with the molecular weight of 40000 and 3g of bisphenol A epoxy resin NPEL128 at 155 ℃, adding the blend prepared in the step (1) into the mixture and stirring the mixture for 3min after the polylactic acid is completely melted, adding 2.5g of diphenylmethane diisocyanate (MDI) at the reaction temperature of 155 ℃, stirring the mixture for 5min, finally adding 0.15g of tung oil and continuously stirring the mixture for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making into degradable antifreezing material for cement concrete road surface.
Example 3
(1) 80g of magnesium chloride and 20g of potassium acetate are weighed, crushed and ground to 200 meshes. Heating and stirring at 70 ℃, adding 2g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) Heating and stirring 0.9g of polylactic acid with the molecular weight of 60000 and 3g of bisphenol F type epoxy resin NPEF-170 at 155 ℃, adding the blend prepared in the step (1) into the mixture and stirring the mixture for 3min after the polylactic acid is completely melted, adding 1.85g of toluene diisocyanate at the reaction temperature of 155 ℃, stirring the mixture for 5min, finally adding 0.15g of tung oil and continuously stirring the mixture for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making into degradable antifreezing material for cement concrete road surface.
Example 4
(1) 70g of potassium acetate and 30g of magnesium acetate are weighed, crushed and ground to 200 meshes. Heating and stirring at 70 ℃, adding 1g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) Heating and stirring 0.6g of polylactic acid with the molecular weight of 50000 and 2g of bisphenol A epoxy resin E44 at 155 ℃, adding the blend prepared in the step (1) into the mixture and stirring the mixture for 3min after the polylactic acid is completely melted, adding 2g of Hexamethylene Diisocyanate (HDI) at the reaction temperature of 155 ℃, stirring the mixture for 5min, finally adding 0.2g of tung oil and continuously stirring the mixture for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) And (3) placing the flaky anti-freezing material for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making the degradable antifreezing material for cement concrete road.
Example 5
(1) 70g of potassium acetate and 30g of magnesium acetate are weighed, crushed and ground to 200 meshes. Heating and stirring at 70 ℃, adding 1g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) Heating and stirring 1.41g of polycaprolactone with the molecular weight of 50000 and 3.14g of bisphenol A epoxy resin E44 at 155 ℃, adding the blend prepared in the step (1) into the mixture and stirring the mixture for 3min after the polycaprolactone is completely melted, adding 2g of Hexamethylene Diisocyanate (HDI) at the reaction temperature of 155 ℃, stirring the mixture for 5min, finally adding 0.31g of tung oil and continuously stirring the mixture for 10min to prepare the blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making the degradable antifreezing material for cement concrete road.
Comparative example 1
(1) 100g of powdered anhydrous calcium chloride was weighed. Heating and stirring at 70 ℃, adding 2g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) Heating and stirring 1.0g of polylactic acid with the molecular weight of 70000 and 2.35g of bisphenol F/A copolymerized epoxy resin NPEF-175 at 155 ℃, adding the blend prepared in the step (1) into the mixture and stirring for 3min after the polylactic acid is completely melted, adding 0.23g of tung oil and continuously stirring for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making the degradable antifreezing material for cement concrete road.
Comparative example 2
(1) 100g of powdered anhydrous calcium chloride was weighed. Heating and stirring at 70 ℃, adding 2g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) 1g of polylactic acid with the molecular weight of 70000 and 2.465g of bisphenol F/A copolymerized epoxy resin NPEF-175 are heated and stirred at the temperature of 155 ℃, the blend prepared in the step (1) is added and stirred for 3min after the polylactic acid is completely melted, 2.465g of dicyclohexyl methane diisocyanate (HMDI) is added at the reaction temperature of 155 ℃, and the mixture is stirred for 5min, so that a blend 2 is prepared.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making the degradable antifreezing material for cement concrete road.
Comparative example 3
(1) 100g of powdered anhydrous calcium chloride was weighed. Heating and stirring at 70 ℃, adding 2g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) 2.85g bisphenol F/A copolymer epoxy resin NPEF-175 is heated and stirred for 3min at 155 ℃, 2.85g dicyclohexylmethane diisocyanate (HMDI) is added at 155 ℃ for stirring for 5min, and finally 0.23g tung oil is added for continuous stirring for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making the degradable antifreezing material for cement concrete road.
Comparative example 4
(1) 100g of powdered anhydrous calcium chloride was weighed. Heating and stirring at 70 ℃, adding 2g of silane coupling agent KH-550, stirring at constant temperature, stirring for 5min, naturally cooling, and standing for 30min to obtain blend 1.
(2) 2.7g of polylactic acid with the molecular weight of 70000 and 1.5g of bisphenol F/A copolymerized epoxy resin NPEF-175 are heated and stirred at the temperature of 155 ℃, the blend prepared in the step (1) is added and stirred for 3min after the polylactic acid is completely melted, 1.5g of dicyclohexyl methane diisocyanate (HMDI) is added at the reaction temperature of 155 ℃, the mixture is stirred for 5min, and finally 0.23g of tung oil is added and continuously stirred for 10min to prepare a blend 2.
(3) Blend 2 was placed into a tablet press and compressed for 180 seconds at a pressure of 3KN per square centimeter.
(4) The flaky anti-freezing material is placed for 24 hours at normal temperature.
(5) Crushing to obtain 0.5-1.5mm size grains, and making into degradable antifreezing material for cement concrete road surface.
Experiment 1 the hardness test of the degradable antifreeze material according to the invention results from table 1.
Respectively crushing and screening the embodiment and the comparative example of the degradable antifreeze material, performing hardness test on particles with different particle sizes, randomly sampling a test sample by using a hardness tester, measuring 20 hardness and taking an average value, wherein the results are as follows:
TABLE 1 hardness of each of examples and comparative examples
Wherein, the film material liquid flows out in the extrusion process without adding the isocyanate curing agent, and the test piece has almost no hardness. Besides polylactic acid, other components can effectively improve the hardness of the anti-freezing material after tabletting. Too low an amount of epoxy resin in comparative example 4 has significantly affected the strength of the pellets.
Experiment 2 the results of the release performance tests of the degradable antifreeze material of the invention are shown in table 2.
Respectively carrying out crushing and screening on the degradable antifreeze material embodiment and the comparative example, carrying out a slow release test on a sample of 0.5mm-1.5mm, adding 10g of the sample into 100mL of water under a stirring state, titrating the release of chloride ions by adopting silver nitrate, and measuring the release of acetate ions and chloride ions by adopting a calibrated conductivity curve.
Table 2 release profile of each example and comparative example
Among them, the film material liquid flows out in the extrusion process without adding the isocyanate curing agent, and the test piece has almost no hardness and can hardly be molded, so the release rate is not listed. The result shows that the substances which obviously play a slow release role are epoxy resin and then tung oil, and the slow release performance of the material is seriously influenced by the reduction of the using amounts of the epoxy resin and the tung oil, because the cured material has a compact structure and has stronger hydrophobic property. The reason for the initial release is that some of the salt is exposed during the crushing process.
Experiment 3 the results of the release properties of the degradable antifreeze material of the present invention after a long period of standing are shown in table 3.
The examples and comparative examples were each subjected to the degradation performance after long-term storage, and the long-term release performance in a microbial environment in an aqueous solution state in a vacuum state was measured. And (3) measuring the release performance of the degradable antifreeze material in water by adding 10g of the degradable antifreeze material into 100mL of water under the stirring state and adopting silver nitrate titration and combining with the conductivity.
TABLE 3 degradation Release for the examples and comparative examples
As can be seen from the comparison results, the sample of comparative example 3, which has no polylactic acid, and the sample of comparative example 1 has accelerated release after 60 days in any environment, has excellent slow release performance during long-term storage, and is not beneficial to long-term melting of ice and snow on roads. The sample of comparative example 3, which did not contain tung oil, exhibited an overall faster release, but its hardness at formation was lower and the early release was also faster.
As can be seen from the table, the examples can achieve good degradation and release effects in a microbial environment, and the higher the hydrophobic component is, the better the slow release effect response is. The embodiment has obvious advantages by combining hardness, early water slow release performance and long-term degradation release performance.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (5)
1. A degradable antifreezing material for a cement concrete pavement is characterized in that the antifreezing material is prepared from an anti-icing core material and a degradable membrane material, wherein the core material is one or more of calcium chloride, sodium chloride, magnesium chloride, calcium acetate, magnesium acetate or potassium acetate, and the degradable membrane material is composed of a silane coupling agent, epoxy resin, tung oil, a degradable component and an isocyanate curing agent;
the silane coupling agent is one or a mixture of two of gamma-aminopropyltriethoxysilane (KH-550) and gamma- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560);
the epoxy resin is one or a mixture of two of bisphenol A epoxy resin, bisphenol F epoxy resin and bisphenol F/A copolymerized epoxy resin;
the degradable component is one of polylactic acid or polycaprolactone, wherein the molecular weight of the polylactic acid is 40000-70000;
the isocyanate curing agent is one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI) and Hexamethylene Diisocyanate (HDI);
the mass ratio of the anti-freezing core material to the degradable membrane material is as follows: 1:0.06-0.08, wherein the mass ratio of the anti-icing core material to the silane coupling agent is 1:0.01-0.02, wherein the mass ratio of the epoxy resin to the degradable components is 1:0.3-0.45, wherein the mass ratio of the epoxy resin to the tung oil is 1:0.05-0.1, and the mass ratio of the epoxy resin to the isocyanate is 1.
2. The degradable antifreeze material of claim 1 wherein said anti-icing core material has a particle size of no greater than 200 mesh and requires comminution of a large particle core material.
3. A preparation method of a degradable anti-freezing material for a cement concrete pavement is characterized by comprising the following steps:
(1) Heating the anti-freezing ice core material to a reaction temperature, adding a silane coupling agent, stirring at a constant temperature, naturally cooling and standing after stirring to prepare a blend 1;
the core material is one or more of calcium chloride, sodium chloride, magnesium chloride, calcium acetate, magnesium acetate or potassium acetate;
the silane coupling agent is one or a mixture of two of gamma-aminopropyltriethoxysilane (KH-550) and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane (KH-560);
(2) Heating the degradable component and the epoxy resin to a reaction temperature, adding the blend 1 prepared in the step (1) after the degradable component is completely melted, stirring, adding an isocyanate curing agent, continuously stirring for reaction, and finally adding tung oil, continuously stirring to prepare a blend 2;
the degradable component is one of polylactic acid or polycaprolactone, wherein the molecular weight of the polylactic acid is 40000-70000;
the epoxy resin is one or a mixture of two of bisphenol A epoxy resin, bisphenol F epoxy resin and bisphenol F/A copolymer epoxy resin;
the isocyanate curing agent is one of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI) and Hexamethylene Diisocyanate (HDI);
(3) Pouring the blend 2 prepared in the step (2) into a tablet machine die for tabletting to prepare a flaky anti-freezing material, and naturally cooling the flaky anti-freezing material;
(4) And (4) crushing the flaky anti-freezing material prepared in the step (3), and taking particles with the particle size of 0.5-2 mm to prepare the degradable anti-freezing material for the cement concrete pavement.
4. The method according to claim 3, wherein the reaction temperature in the step (1) is 70-80 ℃, the stirring time is 5-15min, and the standing time is 30-40min; the reaction temperature in the step (2) is 130-155 ℃, the first stirring time is 3-5min, the second stirring time is 5-10min, and the third stirring time is 10-15min; and (4) performing tabletting operation in the step (3), wherein the unit square centimeter pressure is not less than 3KN, and the tabletting time is not less than 180 seconds.
5. Use of the degradable antifreeze material of claim 1 for ice and snow suppression on cement concrete pavement.
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| CN112266769A (en) | 2021-01-26 |
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