CN113308226A - Pavement humectant and preparation method thereof - Google Patents
Pavement humectant and preparation method thereof Download PDFInfo
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- CN113308226A CN113308226A CN202110632850.3A CN202110632850A CN113308226A CN 113308226 A CN113308226 A CN 113308226A CN 202110632850 A CN202110632850 A CN 202110632850A CN 113308226 A CN113308226 A CN 113308226A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/22—Materials not provided for elsewhere for dust-laying or dust-absorbing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/60—Planning or developing urban green infrastructure
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Abstract
The invention relates to the field of road moisturizing, and provides a road moisturizing agent aiming at the problem that spraying liquid on a road surface is easy to evaporate. The water adsorbed by the temperature-sensitive hydrogel is not easy to evaporate, and can stay on the road surface for a long time until the external temperature exceeds the LCST of the road surface, and the temperature-sensitive hydrogel shrinks to release the contained water so as to carry out secondary moisture preservation on the road surface. The invention also provides a preparation method of the pavement humectant.
Description
Technical Field
The invention relates to the field of road moisturizing, in particular to a pavement moisturizing agent and a preparation method thereof.
Background
Nowadays, the urbanization process is accelerated continuously, the urban population is increased day by day, and the dust raising amount on the road surface is increased continuously. The influence of large-particle floating pollutants on the air quality of cities in China is huge, and the large-particle floating pollutants are the leading causes of air pollution of most cities. At present, the measures for reducing road raised dust and inhalable particles are mainly water spraying treatment, the method has the advantages of simplicity and easy implementation, and the defects of short dust fall retention time and large water consumption, and according to survey data, the dust concentration can reach 2mg/m when the humidity of the road surface of the crushed stone in the automobile transportation reaches 8-9 percent3The water consumption reaches 1.5-2L per square meter, the effective time of one-time water spraying is only 10-15 minutes, particularly, the temperature in summer of part of cities in China is high, the evaporation speed is higher, and therefore, the application of water spraying and dust suppression is greatly limited.
Patent CN104073222A discloses a road dust suppressant for treating inhalable particles in near-surface gas and a preparation method thereof, wherein a calcium magnesium acetate aqueous solution is applied to the road dust suppressant, but the road dust suppressant has short moisture retention and absorption time and unobvious continuous application time, and is constructed step by step and complicated in steps. In patent CN102660227A, CN103305188A, CN103965834A, etc., carboxymethyl cellulose film-forming substances are used in the formula to retard the evaporation rate of water, but in practical road applications, such substances may increase the slipperiness, reduce the road resistance, and possibly increase the road safety hazard. Accordingly, an ideal solution is needed.
Disclosure of Invention
The invention provides a pavement humectant which aims to solve the problem that spray liquid on a pavement is easy to evaporate and comprises temperature-sensitive hydrogel.
In order to achieve the purpose, the invention adopts the following technical scheme:
a pavement humectant comprises temperature-sensitive hydrogel and water, wherein the temperature-sensitive hydrogel is an N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer. The temperature-sensitive hydrogel can perform reversible sol-gel conversion along with temperature change, is in a sol state (like liquid) when the temperature is reduced, and forms hydrogel when the temperature is higher. The temperature-sensitive hydrogel and water are used as the road surface humectant, and before spraying, the temperature-sensitive hydrogel is mutually dissolved with the water to absorb and contain a large amount of water; most water and ordinary watering liquid after spraying just have limited coverage road surface, play the effect of suppressing dust, and the water that is adsorbed by temperature sensitive aquogel is difficult to evaporate, can stop on the road surface for a long time, and until ambient temperature surpasses its phase transition temperature LCST, the gel sudden change of hydrophilicity becomes hydrophobic state, contracts into hydrophobic hard ball structure, releases the moisture that contains, carries out the secondary to the road surface and moisturizes. More importantly, the transformation of the temperature-sensitive hydrogel is reversible, the temperature-sensitive hydrogel which releases moisture and walks on the road surface can absorb moisture again when meeting rainy days or sprinkling water next time, and the process is repeated, so that the environment is friendly.
Preferably, the amount of acrylic acid is 10-15% by mass of N-isopropylacrylamide. The temperature-sensitive hydrogel is formed by copolymerizing N-isopropylacrylamide-acrylic acid-phenyl acrylate, wherein the N-isopropylacrylamide plays a temperature-sensitive role and is the most main chain segment. However, the LCST of the N-isopropyl acrylamide hydrogel is about 32 ℃, which is not in line with the use scene, so the LCST is adjusted by adding an acrylic acid chain segment. The amount of acrylic acid used has a decisive effect.
Preferably, the phenyl acrylate is used in an amount of 1 to 3% by mass based on the N-isopropylacrylamide. The N-isopropyl acrylamide hydrogel is very sensitive to temperature, and the volume can be rapidly contracted when the external temperature exceeds LCST (lower temperature limit), and in order to delay the release speed of water in the N-isopropyl acrylamide hydrogel, a phenyl acrylate chain segment is added, and the shrinkage of the temperature-sensitive hydrogel is hindered due to the existence of a benzene ring structure. But the dosage of the phenyl acrylate is not excessive, so that the temperature sensitivity of the N-isopropylacrylamide hydrogel is not excessively influenced. Furthermore, the addition of phenyl acrylate segments has an effect on the LCST, so that the amounts of acrylic acid and phenyl acrylate have to be coordinated with one another.
Preferably, the temperature-sensitive hydrogel has a minimum critical solution temperature LCST of 40-55 ℃. Considering that the pavement temperature in summer can reach 40-60 ℃, in order to make the temperature sensitive hydrogel play a better role, the LCST of the temperature sensitive hydrogel is adjusted to 40-55 ℃ by adjusting the monomer proportion.
Preferably, the pavement humectant consists of 80-90 parts of water and 10-20 parts of the temperature-sensitive hydrogel by mass. In consideration of economy, most of the pavement moisturizing agent is water which can be common river water and the like, the part of water preferentially soaks the pavement during spraying to play a role in dedusting, and the temperature-sensitive hydrogel absorbs part of water to be automatically released at high temperature so as to perform secondary moisturizing.
The invention also provides a preparation method of the pavement humectant, which comprises the following steps: uniformly mixing and dispersing phenyl acrylate and water, adding potassium persulfate, and stirring and reacting for 1-2h at 50-60 ℃; adding water dispersion of N-isopropyl acrylamide, a cross-linking agent, sodium dodecyl sulfate and potassium persulfate, heating to 70-80 ℃ and reacting for 3-5 h; then adding acrylic acid and potassium persulfate, and reacting for 1-2h to obtain the N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer. According to the invention, three monomers are added respectively, and the next monomer is added after polymerization to a certain degree, so that the chain segments are distributed more uniformly, and the overall temperature sensitivity is ensured.
Preferably, the crosslinking agent is polyethylene glycol 1200, and the mass of the crosslinking agent is 2-4% of that of the N-isopropylacrylamide. The consumption of the cross-linking agent is too small, the temperature-sensitive hydrogel particles are small, and the adsorption to water is limited; however, the dosage of the cross-linking agent is too large, the cross-linking of the temperature-sensitive hydrogel is too dense, and water molecules are difficult to enter the system, so the dosage of the cross-linking agent needs to be controlled within a reasonable range.
Preferably, the mass of the sodium dodecyl sulfate is 10-20% of that of the N-isopropylacrylamide.
Preferably, the treatment steps after the reaction are as follows: the reaction product is centrifugally precipitated by methanol, dialyzed and dried in vacuum.
Therefore, the beneficial effects of the invention are as follows: (1) the pavement humectant comprises temperature-sensitive hydrogel, water adsorbed by the temperature-sensitive hydrogel is not easy to evaporate, and can stay on the pavement for a long time until the external temperature exceeds the LCST of the pavement, and the temperature-sensitive hydrogel shrinks to release contained water to carry out secondary moisture preservation on the pavement; (2) adding an acrylic acid chain segment to adjust the LCST of the N-isopropyl acrylamide hydrogel to be between 40 and 55 ℃, so that the N-isopropyl acrylamide hydrogel is suitable for roads; (3) the N-isopropyl acrylamide hydrogel is very sensitive to temperature, and the volume can be rapidly contracted when the external temperature exceeds LCST (lower temperature limit), and in order to delay the release speed of water in the N-isopropyl acrylamide hydrogel, a phenyl acrylate chain segment is added, and the shrinkage of the temperature-sensitive hydrogel is hindered due to the existence of a benzene ring structure.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
The pavement humectant consists of 80 parts of water and 20 parts of temperature-sensitive hydrogel in parts by weight, wherein the temperature-sensitive hydrogel is an N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer, the using amount of acrylic acid is 12% of the mass of the N-isopropylacrylamide, the using amount of phenyl acrylate is 2% of the mass of the N-isopropylacrylamide, and the lowest critical solution temperature LCST of the temperature-sensitive hydrogel is 50 ℃.
The preparation method of the pavement humectant comprises the following steps: 2g of phenyl acrylate and water are mixed and dispersed uniformly, 0.2g of potassium persulfate is added, and the mixture is stirred and reacted for 2 hours at the temperature of 50 ℃; then 100g N-isopropyl acrylamide, 3g of cross-linking agent polyethylene glycol 1200, 15g of sodium dodecyl sulfate and 1g of aqueous dispersion of potassium persulfate are added, and the mixture is heated to 70 ℃ to react for 4 hours; then adding 12g of acrylic acid and 0.2g of potassium persulfate to continue reacting for 1 hour, finishing the reaction, centrifugally precipitating the product by using methanol, dialyzing, and drying in vacuum to obtain the product N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer.
Example 2
The pavement humectant consists of 90 parts of water and 10 parts of temperature-sensitive hydrogel in parts by mass, wherein the temperature-sensitive hydrogel is an N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer, the using amount of acrylic acid is 10% of the mass of the N-isopropylacrylamide, the using amount of phenyl acrylate is 3% of the mass of the N-isopropylacrylamide, and the lowest critical solution temperature LCST of the temperature-sensitive hydrogel is 49 ℃.
The preparation method of the pavement humectant comprises the following steps: 3g of phenyl acrylate and water are mixed and dispersed uniformly, 0.2g of potassium persulfate is added, and the mixture is stirred and reacted for 1 hour at the temperature of 60 ℃; then 100g N-isopropyl acrylamide, 2g of cross-linking agent polyethylene glycol 1200, 10g of sodium dodecyl sulfate and 1g of aqueous dispersion of potassium persulfate are added, and the mixture is heated to 80 ℃ to react for 3 hours; then 10g of acrylic acid and 0.2g of potassium persulfate are added to continue to react for 2 hours, the reaction is finished, the product is centrifugally precipitated by methanol, and the product N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer is obtained after dialysis and vacuum drying.
Example 3
The pavement humectant consists of 85 parts of water and 15 parts of temperature-sensitive hydrogel in parts by mass, wherein the temperature-sensitive hydrogel is an N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer, the acrylic acid is 15% of the mass of the N-isopropylacrylamide, the phenyl acrylate is 1% of the mass of the N-isopropylacrylamide, and the Lowest Critical Solution Temperature (LCST) of the temperature-sensitive hydrogel is 51 ℃.
The preparation method of the pavement humectant comprises the following steps: 2g of phenyl acrylate and water are mixed and dispersed uniformly, 0.2g of potassium persulfate is added, and the mixture is stirred and reacted for 2 hours at the temperature of 50 ℃; then 100g N-isopropyl acrylamide, 4g of cross-linking agent polyethylene glycol 1200, 15g of sodium dodecyl sulfate and 1g of aqueous dispersion of potassium persulfate are added, and the mixture is heated to 70 ℃ to react for 5 hours; then adding 15g of acrylic acid and 0.2g of potassium persulfate to continue reacting for 1 hour, finishing the reaction, centrifugally precipitating the product by using methanol, dialyzing, and drying in vacuum to obtain the product N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer.
Example 4
The difference from example 1 is that: the amount of the acrylic acid is 6 percent of the mass of the N-isopropylacrylamide.
Example 5
The difference from example 1 is that: the dosage of the acrylic acid is 18 percent of the mass of the N-isopropylacrylamide.
Example 6
The difference from example 1 is that: the dosage of the phenyl acrylate is 5 percent of the mass of the N-isopropylacrylamide.
Example 7
The difference from example 1 is that: phenyl acrylate was not used.
Example 8
The difference from example 1 is that: the mass of the crosslinking agent polyethylene glycol 1200 is 6% of the N-isopropylacrylamide.
Example 9
The difference from example 1 is that: the mass of the crosslinking agent polyethylene glycol 1200 is 0.8% of that of the N-isopropylacrylamide.
Comparative example
Common N-isopropyl acrylamide temperature sensitive hydrogel.
Results testing
(1) Measurement of swelling Rate
3-5 mg of xerogel (Wd) prepared in each example was added to three 10mL small saline bottles, 8mL of Milli-Q ultrapure water was added, and the materials were placed in a room temperature water bath for 24h to reach swelling equilibrium. Finally, the fully swollen hydrogel is removed and its surface is blotted dry with wet filter paper and weighed (We). The Equilibrium Swelling Ratio (ESR) of the hydrogel at different temperatures can be calculated by the formula ESR ═ (We-Wd)/Wd.
(2) Measurement of shrinkage
Deswelling kinetics of hydrogels were measured using a weighing method: the hydrogel reached swelling equilibrium at room temperature, then the hydrogel in swelling equilibrium was quickly transferred to a beaker containing water at a temperature of 53 ℃ and the weight of the hydrogel was measured at the set time point. When the weight of the hydrogel was measured, the hydrogel was carefully taken out of the water, the water on the surface of the hydrogel was sucked off with filter paper and weighed, then the hydrogel was put back into the beaker, the weight was measured again after 2 hours, and the shrinkage was calculated.
The test results are shown in the table below, and it can be seen that the temperature-sensitive hydrogel prepared by the invention has the response temperature of 40-55 ℃, the water absorption swelling ratio is high, and the response speed is reasonable. Examples 4 and 5 show the effect of the amount of acrylic acid used to increase the LCST on the LCST of the temperature-sensitive hydrogel, compared to example 1, so that the LCST is lower when the amount is too small and higher when the amount is too large. Examples 6 and 7 reflect the influence of phenyl acrylate on the response speed of the temperature-sensitive hydrogel, and phenyl acrylate reduces the shrinkage sensitivity of the temperature-sensitive hydrogel through a macromolecular benzene ring, so that the dosage of phenyl acrylate is not excessive; as is clear from example 6, phenyl acrylate also lowers the LCST of the temperature-sensitive hydrogel, and therefore, when acrylic acid and phenyl acrylate are used together, the ratio of these two components needs to be controlled. Examples 8 and 9 reflect the influence of the amount of the cross-linking agent on the adsorption amount of the temperature-sensitive hydrogel, and the cross-linking agent is used in a small amount, the temperature-sensitive hydrogel has small particles and limited adsorption to water; however, the dosage of the cross-linking agent is too large, the cross-linking of the temperature-sensitive hydrogel is too dense, and water molecules are difficult to enter the system, so the dosage of the cross-linking agent needs to be controlled within a reasonable range.
| Group of | LCST/℃ | Equilibrium swelling ratio% | Shrinkage ratio% |
| Example 1 | 50 | 586 | 15 |
| Example 2 | 49 | 573 | 15 |
| Example 3 | 51 | 569 | 15 |
| Example 4 | 38 | ||
| Example 5 | 57 | ||
| Example 6 | 42 | 10 | |
| Example 7 | 52 | 25 | |
| Example 8 | 53 | 460 | |
| Example 9 | 51 | 455 | |
| Comparative example | 32 | 400 | 28 |
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The pavement humectant is characterized by comprising temperature-sensitive hydrogel and water, wherein the temperature-sensitive hydrogel is an N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer.
2. The pavement humectant according to claim 1, wherein the amount of acrylic acid is 10 to 15% by mass of N-isopropylacrylamide.
3. The pavement humectant according to claim 1 or 2, wherein the phenyl acrylate is used in an amount of 1 to 3% by mass based on the N-isopropylacrylamide.
4. The pavement humectant according to claim 1, wherein the temperature-sensitive hydrogel has a minimum critical solution temperature LCST of 40 to 55 ℃.
5. The pavement humectant according to claim 1, wherein the pavement humectant consists of 80-90 parts by weight of water and 10-20 parts by weight of the temperature-sensitive hydrogel.
6. A method for preparing a road surface moisturizing agent as claimed in any one of claims 1 to 5, comprising the steps of: uniformly mixing and dispersing phenyl acrylate and water, adding potassium persulfate, and stirring and reacting for 1-2h at 50-60 ℃; adding water dispersion of N-isopropyl acrylamide, a cross-linking agent, sodium dodecyl sulfate and potassium persulfate, heating to 70-80 ℃ and reacting for 3-5 h; then adding acrylic acid and potassium persulfate, and reacting for 1-2h to obtain the N-isopropylacrylamide-acrylic acid-phenyl acrylate copolymer.
7. The method for preparing a pavement humectant according to claim 6, wherein the cross-linking agent is polyethylene glycol 1200, and the mass of the polyethylene glycol is 2-4% of that of N-isopropylacrylamide.
8. The method for preparing a road surface humectant according to claim 6 or 7, wherein the mass of the sodium lauryl sulfate is 10-20% of that of the N-isopropylacrylamide.
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