CN114806505A - Self-melting ice preparation process of sustained-release microcapsules - Google Patents
Self-melting ice preparation process of sustained-release microcapsules Download PDFInfo
- Publication number
- CN114806505A CN114806505A CN202210565997.XA CN202210565997A CN114806505A CN 114806505 A CN114806505 A CN 114806505A CN 202210565997 A CN202210565997 A CN 202210565997A CN 114806505 A CN114806505 A CN 114806505A
- Authority
- CN
- China
- Prior art keywords
- self
- agent
- melting ice
- melting
- modified
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a self-thawing preparation process of a sustained-release microcapsule, which comprises the steps of preparing an S1 material; s2 is prepared from the ice melting agent matrix; s3, adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture; s4, drying and dispersing the mixture obtained in S3 to obtain the self-melting ice agent to be modified; s5, preparing a capsule wall; and S6, modifying the self-melting ice agent. The method comprises the steps of adsorbing a core material into a pore by using blast furnace slag powder, extracting and synthesizing the core material by furfural or plant straw pyrolysis waste liquid to prepare sodium acetate, extracting and synthesizing environment-friendly non-chlorine salt from biomass waste liquid, carrying out macromolecular capsule wall modification treatment on the surface of the core material to form a microcapsule functional material with a slow release effect, and doping the microcapsule functional material into the surface layer of the hot-mix asphalt concrete pavement to realize the active snow-melting and deicing functions of the asphalt pavement.
Description
Technical Field
The invention relates to the technical field of active snow melting and deicing of hot-mix asphalt pavements, in particular to a preparation process for self-melting ice by slow-release microcapsules.
Background
The scale of the road network in China leaps the first in the world, the north is in an area with frequent ice and snow, and the south is always in a sleet weather, so that road traffic safety accidents are easily caused.
Patent publication is CN206164052U, discloses an external insulation removes ice and snow instrument, including insulating bar and remove ice and snow cutter body, this insulating bar one end with remove ice and snow cutter body and be connected, its technical characterstic is: the other end of the insulating operating rod is connected with an electric heating blower, and the other end of the electric heating blower is connected with an ice scraper. The utility model combines two modes of mechanical ice and snow removal and thermal ice and snow removal, thereby not only having convenient operation, but also improving the ice and snow removal efficiency and ensuring the ice and snow removal effect; meanwhile, the rubber soft pad is arranged on the wedge-shaped scraper blade of the ice scraper, so that the blade can be prevented from damaging the outer insulating surface, and the heating wire is also arranged on the ice scraper, so that the ice body can be accelerated to melt in a heating mode, and the effects of removing ice and snow and preventing re-icing are achieved; the insulating property of insulating bar has been improved, the rain-proof requirement of antiskid is satisfied, the phenomenon of taking off the hand and electrocute that appears when can effectively avoiding the user to remove ice and snow has guaranteed user's personal safety.
Patent publication No. CN102635084A discloses a hidden airport runway ice and snow removing system. The system mainly comprises: the intelligent detection spraying mechanism, the runway slide rail, the command control room, the snow removing agent recovery device, the snow shoveling mechanism, the snow sweeping mechanism, the snow blowing and steam snow removing mechanism and the equipment slide rail. The invention discloses a hidden type airport runway ice and snow removing system, wherein equipment is hidden underground at two sides of an airport runway and one end of the runway, under the ice and snow weather, the equipment can be automatically opened in a snow removing period by matching with a command of a tower to an airplane, the system selects different snow removing devices and mechanisms hidden underground according to the snow condition, a spraying mechanism is provided with a plurality of groups of sensors, the snow removing mechanism can quickly operate on a slide rail, all the equipment automatically retracts underground after the operation is finished, the equipment such as a snow remover and the like is saved, manpower and material resources are reduced, the efficiency is high, the spraying is uniform, and the taking-off safety is better ensured.
The two documents respectively adopt a manual mechanical clearing method and a chlorine salt snow melting agent spreading method, and manual clearing and mechanical clearing of accumulated snow and ice are passive snow removing technologies, so that the workload is concentrated, the road needs to be closed, snow removal is realized, and the deicing efficiency is low; the spreading of the chlorine salt snow-melting agent can salinize soil and corrode concrete structures such as road guardrails, bridges and culverts and the like.
The technology for actively removing the ice and the snow comprises a thermal snow melting technology, a high-elasticity material embedded ice and snow melting technology, a salt storage filler added ice and snow melting technology and the like, wherein the thermal snow melting technology can adopt an electric power and geothermal snow melting technology, heating cables, hot water pipelines, electric heating wires and the like are laid on the road surface, the electric power is utilized to enable the cables and the electric heating wires to generate heat to achieve the effects of melting the snow and removing the ice, and hot water is injected into the pipelines to achieve the effects of melting the snow and removing the ice. The thermal snow melting construction process is complex, the energy consumption is large, the manufacturing cost is high, and the later maintenance engineering amount is large, so the application of the thermal snow melting is limited;
at present, the technology of mechanical snow removal and passive snow and ice removal by spreading a chlorine salt snow-melting agent is taken as the main in China, snow is removed within a specified time after snow is frequently needed to keep smooth traffic, lanes are occupied or traffic is closed in the snow and ice removal process, and the defects of large workload, low efficiency, corrosion to concrete, salinized soil and the like exist, so that a preparation process of slow-release microcapsules for self-melting ice is provided, and the problems are solved by using liquid-solid waste and active novel materials and novel technologies for snow and ice removal with low carbon, energy conservation and environmental protection.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation process of a slow-release microcapsule self-melting ice.
The invention provides a self-thawing preparation process of a sustained-release microcapsule, which comprises the following steps:
s1: preparing materials: the materials required by the self-melting ice of the sustained-release microcapsule are sodium acetate, an active agent OP-10 and a dispersant nano SiO which are extracted and synthesized from furfural or plant straw pyrolysis waste liquid 2 Porous solid waste carrier blast furnace slag powder and corrosion inhibitor NaHCO 3 Monomer X, methyl acrylate, butyl acrylate, styrene, an initiator, a coupling agent and water;
s2: preparing a self-melting ice agent matrix: preparing saturated sodium acetate solution, adding activator OP-10 accounting for 3 percent of the mass of the saturated sodium acetate solution and dispersing agent nano SiO accounting for 1 percent of the mass of the saturated sodium acetate solution 2 Adding a corrosion inhibitor NaHCO with the mass of 5 percent of sodium acetate solution 3 Obtaining a mixed solution for later use; NaHCO 2 3 The addition amount of (A) is 5% of the mass of the sodium acetate solution.
S3: adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture;
s4: drying and dispersing the mixture obtained in the step S3 to obtain the self-melting ice agent to be modified;
s5, capsule wall preparation: mixing a monomer X, methyl acrylate, butyl acrylate and styrene to obtain a monomer mixed solution;
adding an initiator and a coupling agent into the monomer mixed solution, then dropwise adding the mixture into a solvent preheated to 110 ℃, and polymerizing for 3 hours to obtain a modified capsule wall solution;
s6, modifying the self-melting ice agent: coating and modifying the self-melting ice agent to be modified prepared by S4 by using the modified capsule wall solution;
fully mixing the modified capsule wall solution, water and the self-melting ice agent to be modified to form paste;
drying, crushing and sieving the paste to obtain the self-melting ice of the sustained-release microcapsule.
Preferably, in the S3, the mass ratio of the mixed solution to the porous solid waste carrier is 1: 2-2.3. Preferably, the mixing and stirring time in the S3 is 1-1.5 h; the mixture was dried at 120-130 ℃ to constant weight in S4.
Preferably, in S5, the solvent: a monomer X: methyl acrylate: butyl acrylate: the mass ratio of styrene was set to 50:1:25:18: 8.
Preferably, the solvent in S5 is isopropanol, and the monomer X is acrylic acid.
Preferably, in S5, the initiator is set to AIBN and the coupling agent is set to silane coupling agent KH-570.
Preferably, in S5, AIBN accounting for 2.5% by mass of the monomer mixture and KH-570, a silane coupling agent accounting for 0.8% by mass of the monomer mixture, are added to the monomer mixture.
The initiator is added to the monomer mixture, which is simply understood to be catalytic polymerization, 2.5% of the total mass of the four monomers of acrylic acid, methyl acrylate, butyl acrylate and styrene is 2.5%, and 0.8% of the total mass of the four monomers of acrylic acid, methyl acrylate, butyl acrylate and styrene is 0.8%.
Preferably, the mass ratio of the modified capsule wall solution, the water and the self-melting ice agent to be modified in S6 is 1:0.6: 3.
The invention has the beneficial effects that: the porous solid waste carrier blast furnace slag powder absorbs environment-friendly organic non-chlorine salt snow melting core materials extracted from liquid waste into pores, sodium acetate extracted and synthesized from furfural or plant straw pyrolysis waste liquid is used as an ice and snow inhibiting component, and the surface of the carrier after absorbing the core materials is subjected to high-molecular capsule wall modification treatment to form a microcapsule structure, so that a slow release effect is realized, and the carrier has good self-melting ice rate, low moisture absorption rate and salt release rate and good thermal stability of a hot-mix asphalt mixture. The utilization of liquid waste, solid waste and organic non-chlorine environment-friendly salt enables the invention to have remarkable energy-saving emission-reduction, green, low-carbon and environment-friendly performances.
Drawings
FIG. 1 shows SEM100 times material morphology of a self-made slow-release microcapsule self-melting ice agent;
FIG. 2 is a SEM500 times material morphology of the self-made slow-release microcapsule self-melting ice agent;
FIG. 3 shows the shape of a material SEM200 times of a salt storage mixture material of the slow-release microcapsule self-melting ice agent;
FIG. 4 shows the shape of a material SEM200 times of a salt storage mixture material of the slow-release microcapsule self-melting ice agent;
FIG. 5 is an XRD (X-ray diffraction) spectrum of the self-melting ice agent powder of the sustained-release microcapsule;
FIG. 6 is an infrared spectroscopic analysis spectrum of the sustained-release microcapsule self-melting ice agent;
FIG. 7 is a thermogravimetric result of an unmodified self-melting ice agent;
FIG. 8 is a graph of thermogravimetric results of the modified self-melting ice agent.
Detailed Description
The invention is further illustrated by the following specific examples, wherein the mass units in the examples are grams and the proportions are mass ratios.
Example one
The embodiment provides a self-thawing preparation process of a sustained-release microcapsule, which comprises the following steps:
s1: preparing materials: the materials required by the self-melting ice of the sustained-release microcapsule are prepared by extracting furfural or plant straw pyrolysis waste liquid and synthesizing sodium acetate, an active agent OP-10 and a dispersant nano SiO 2 Porous solid waste carrier blast furnace slag powder and corrosion inhibitor NaHCO 3 Monomer X, methyl acrylate, butyl acrylate, styrene, an initiator, a coupling agent and water;
s2, preparing the self-melting ice agent matrix: preparing saturated sodium acetate solution, adding activator OP-10 accounting for 3 percent of the mass of the saturated sodium acetate solution and dispersing agent nano SiO accounting for 1 percent of the mass of the saturated sodium acetate solution 2 Adding a corrosion inhibitor NaHCO with the mass of 5 percent of sodium acetate solution 3 Obtaining a mixed solution for later use; s3, adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture;
s4, drying and dispersing the mixture obtained in S3 to obtain the self-melting ice agent to be modified;
s5, preparing capsule wall: mixing a monomer X, methyl acrylate, butyl acrylate and styrene to obtain a monomer mixed solution;
adding an initiator and a coupling agent into the monomer mixed solution, then dropwise adding the mixture into a solvent preheated to 110 ℃, and polymerizing for 3 hours to obtain a modified capsule wall solution;
s6, modifying the self-melting ice agent: coating and modifying the self-melting ice agent to be modified prepared by S4 by using the modified capsule wall solution;
fully mixing the modified capsule wall solution, water and the self-melting ice agent to be modified to form paste;
drying, crushing and sieving the paste to obtain the self-melting ice of the sustained-release microcapsule.
In this example, the stirring time in S3 was 1h, and the mixture was dried to constant weight in S4 at 120 ℃, solvent: a monomer X: methyl acrylate: butyl acrylate: styrene was set to 50:1:25:18:8 for example, the solvent in S5 was isopropanol, the monomer X was acrylic acid, the initiator was AIBN, the coupling agent was silane coupling agent KH-570, AIBN was added to the monomer mixture in an amount of 2.5% by mass of the monomer mixture and silane coupling agent KH-570 was added to the monomer mixture in an amount of 0.8% by mass of the monomer mixture in S5. In S6, the ratio of the modified capsule wall solution, water and the self-melting ice agent to be modified is 1:0.6:3, and the porous solid waste carrier is set as blast furnace slag powder.
Example two
The embodiment provides a self-thawing preparation process of a sustained-release microcapsule, which comprises the following steps:
s1: preparing materials: the materials required by the self-melting ice of the sustained-release microcapsule are furfural or plant straw pyrolysis waste liquid extraction and synthesis for preparing sodium acetate, an active agent OP-10 and a dispersant nano SiO 2 Porous solid waste carrier and corrosion inhibitor NaHCO 3 Monomer X, methyl acrylate, butyl acrylate, styrene, an initiator, a coupling agent and water;
s2, preparing the self-melting ice agent matrix: preparing saturated sodium acetate solution, adding activator OP-10 with the mass of 3 percent of the saturated sodium acetate solution and the saturated sodium acetate solution1% of dispersant nano SiO 2 Adding a corrosion inhibitor NaHCO with the mass of 5 percent of sodium acetate solution 3 Obtaining a mixed solution for later use; s3, adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture;
s4, drying and dispersing the mixture obtained in S3 to obtain the self-melting ice agent to be modified;
s5, capsule wall preparation: mixing a monomer X, methyl acrylate, butyl acrylate and styrene to obtain a monomer mixed solution;
adding an initiator and a coupling agent into the monomer mixed solution, then dropwise adding the mixture into a solvent preheated to 110 ℃, and polymerizing for 3 hours to obtain a modified capsule wall solution;
s6, modifying the self-melting ice agent: coating and modifying the self-melting ice agent to be modified prepared by S4 by using the modified capsule wall solution;
fully mixing the modified capsule wall solution, water and the self-melting ice agent to be modified to form paste;
drying, crushing and sieving the paste to obtain the self-melting ice of the sustained-release microcapsule.
In this example, the stirring time in the paste was 1.2h in S3, and the constant weight of the mixture dried at 125 ℃ in S4, solvent: a monomer X: methyl acrylate: butyl acrylate: styrene is set to be 50:1:25:18:8 for example, the solvent in S5 is isopropanol, the monomer X is acrylic acid, the initiator is AIBN, and the coupling agent is silane coupling agent KH-570, wherein AIBN accounting for 2.5% of the mass of the monomer mixed liquid and silane coupling agent KH-570 accounting for 0.8% of the mass of the monomer mixed liquid are added into the monomer mixed liquid in S5. The ratio of the modified capsule wall solution, water and the self-melting ice agent to be modified in S6 is 1:0.6: 3.
EXAMPLE III
The embodiment provides a self-thawing preparation process of a sustained-release microcapsule, which comprises the following steps:
s1: preparing materials: the materials required by the self-melting ice of the sustained-release microcapsule are furfural or plant straw pyrolysis waste liquid extraction and synthesis for preparing sodium acetate, an active agent OP-10 and a dispersant nano SiO 2 Porous solid waste carrier and corrosion inhibitor NaHCO 3 Monomer, monomerX, methyl acrylate, butyl acrylate, styrene, an initiator, a coupling agent and water;
s2, preparing the self-melting ice agent matrix: preparing saturated sodium acetate solution, adding activator OP-10 accounting for 3 percent of the mass of the saturated sodium acetate solution and dispersing agent nano SiO accounting for 1 percent of the mass of the saturated sodium acetate solution 2 Adding a corrosion inhibitor NaHCO with the mass of 5 percent of sodium acetate solution 3 Obtaining a mixed solution for later use; s3, adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture;
s4, drying and dispersing the mixture obtained in S3 to obtain the self-melting ice agent to be modified;
s5, capsule wall preparation: mixing a monomer X, methyl acrylate, butyl acrylate and styrene to obtain a monomer mixed solution;
adding an initiator and a coupling agent into the monomer mixed solution, then dropwise adding the mixture into a solvent preheated to 110 ℃, and polymerizing for 3 hours to obtain a modified capsule wall solution;
s6, modifying the self-melting ice agent: coating and modifying the self-melting ice agent to be modified prepared by S4 by using the modified capsule wall solution;
fully mixing the modified capsule wall solution, water and the self-melting ice agent to be modified to form paste;
drying, crushing and sieving the paste to obtain the self-melting ice of the sustained-release microcapsule.
In this example, the stirring time in the paste was 1.5h in S3, and the constant weight of the mixture dried at 130 ℃ in S4, solvent: a monomer X: methyl acrylate: butyl acrylate: styrene is set to be 50:1:25:18:8 for example, the solvent in S5 is isopropanol, the monomer X is acrylic acid, the initiator is AIBN, and the coupling agent is silane coupling agent KH-570, wherein AIBN accounting for 2.5% of the mass of the monomer mixed liquid and silane coupling agent KH-570 accounting for 0.8% of the mass of the monomer mixed liquid are added into the monomer mixed liquid in S5. The mass ratio of the modified capsule wall solution, the water and the self-melting ice agent to be modified in the S6 is 1:0.6: 3. Example four
The embodiment provides a self-thawing preparation process of a sustained-release microcapsule, which comprises the following steps:
s1: preparing materials: the materials required by the self-melting ice of the sustained-release microcapsule are furfural or plant straw pyrolysis waste liquid extraction and synthesis for preparing sodium acetate, an active agent OP-10 and a dispersant nano SiO 2 Porous solid waste carrier and corrosion inhibitor NaHCO 3 Monomer X, methyl acrylate, butyl acrylate, styrene, an initiator, a coupling agent and water;
s2, preparing the self-melting ice agent matrix: preparing saturated sodium acetate solution, adding activator OP-10 accounting for 3 percent of the mass of the saturated sodium acetate solution and dispersing agent nano SiO accounting for 1 percent of the mass of the saturated sodium acetate solution 2 Adding a corrosion inhibitor NaHCO with the mass of 5 percent of sodium acetate solution 3 Obtaining a mixed solution for later use; s3, adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture;
s4, drying and dispersing the mixture obtained in S3 to obtain the self-melting ice agent to be modified;
s5, capsule wall preparation: mixing a monomer X, methyl acrylate, butyl acrylate and styrene to obtain a monomer mixed solution;
adding an initiator and a coupling agent into the monomer mixed solution, then dropwise adding the mixture into a solvent preheated to 110 ℃, and polymerizing for 3 hours to obtain a modified capsule wall solution;
s6, modifying the self-melting ice agent: coating and modifying the self-melting ice agent to be modified prepared by S4 by using the modified capsule wall solution;
fully mixing the modified capsule wall solution, water and the self-melting ice agent to be modified to form paste;
drying, crushing and sieving the paste to obtain the self-melting ice of the sustained-release microcapsule.
In this example, the mass ratio of the solution in S3 to the porous solid waste carrier was 1:2.3, the stirring time in the paste was 1h in S3, and the constant weight of the mixture dried at 130 ℃ in S4, solvent: a monomer X: methyl acrylate: butyl acrylate: styrene is set to be 50:1:25:18:8 for example, the solvent in S5 is isopropanol, the monomer X is acrylic acid, the initiator is AIBN, and the coupling agent is silane coupling agent KH-570, wherein AIBN accounting for 2.5% of the mass of the monomer mixed liquid and silane coupling agent KH-570 accounting for 0.8% of the mass of the monomer mixed liquid are added into the monomer mixed liquid in S5.
The mass ratio of the modified capsule wall solution, the water and the self-melting ice agent to be modified in the S6 is 1:0.6: 3.
Extracting furfural or plant straw waste liquid and synthesizing to prepare sodium acetate, wherein the porous carrier is solid waste blast furnace slag powder, and the corrosion inhibitor is NaHCO 3 。
In the embodiment, the slow-release microcapsule self-melting ice replaces mineral powder to be used for a hot-mix asphalt mixture and is paved on an asphalt concrete surface layer, ice and snow inhibiting components are gradually separated out to an asphalt pavement under the capillary action, the pumping action generated by vehicle running and the coupling action of the environment, moisture in the air is absorbed to form a solution, the solution and the ice and snow have a vapor pressure difference, the ice and snow have the tendency that the vapor pressure is reduced to be converged to the liquid vapor pressure, the ice and snow on the contact surface are melted to reduce the adhesive force between the pavement and the ice layer, and the effect of actively inhibiting the ice and snow on the asphalt pavement is realized.
In the embodiment, in the analysis of a scanning electron microscope, the scanning electron microscope is used for observing the appearance and the characteristics of solid particles of the powder, typical substance morphology comparison is performed, and the phase of the material is determined by the scanning electron microscope, as can be seen from fig. 1-2, the self-made slow-release microcapsule self-melting ice agent is in a powder shape, and under the observation of the scanning electron microscope, the self-melting ice agent presents an irregular particle state, the surface of the material is rough, and the material meets the condition of being used as asphalt mixture filler; as can be seen from FIGS. 3-4, the slow-release microcapsule self-melting ice agent is used as a filler to replace mineral powder to prepare the asphalt mixture, and is distributed uniformly in the mixture, which indicates that the material has better compatibility in the mixture;
in the embodiment, in the X-ray diffraction analysis, an XRD test result is shown in fig. 5, a wider dispersion peak exists at 25-35 ° in the spectrum, which indicates that no shaped structure exists in the structure of the sample, the self-melting ice agent matrix is irregular particles with a large specific surface area, the material is still irregular after the self-melting ice agent is coated and modified by the modified capsule wall solution capsule wall emulsion, the particle size of the dried, dispersed and sieved sustained-release microcapsule self-melting ice agent is 0.075mm, and a wider dispersion peak appears in XRD; a peak appears at 28 degrees and is C element; two absorption peaks appear at 33 degrees and 45 degrees respectively, and Na element compounds are arranged at 33 degrees and 45 degrees respectively, which indicates that sodium acetate is a main component in the slow-release microcapsule self-melting ice agent and is also a main material for playing the ice and snow inhibition functions;
in the embodiment, in the infrared spectroscopic analysis, the infrared spectroscopic analysis result is shown in fig. 6, and the infrared spectrum of the sustained-release microcapsule self-melting ice agent is 2952.4cm above -1 Peak is methyl CH 3 The methyl group is the most common group in organic polymers; 1734.14cm -1 The peak is carbonyl-C = O stretching vibration peak, the ratio of carbonyl is the largest according to the spectrum, the carbonyl is non-hydrophilic group, and the non-hydrophilic group is mainly used in the visible macromolecule capsule wall; 1448.33cm -1 The peak is the variable angle vibration peak in the methyl plane, 1165.35cm -1 The peak is a carbon-oxygen-carbon antisymmetric stretching vibration peak, the carbon-oxygen-carbon is a ketone group, the carbon-oxygen-carbon in the polymer is provided with hydroxyl to form carboxyl-COOH, the carboxyl is a hydrophilic group, and the carboxyl is used as a microcapsule surface channel in a high-molecular capsule wall material, so that moisture can permeate and a non-chlorine salt core material can be released;
in the embodiment, in the application process of the thermogravimetric analysis self-made sustained-release microcapsule self-melting ice agent, part of mineral powder in the asphalt pavement aggregate is replaced and mixed into the asphalt mixture, the SMA-13 asphalt mixture mixing process is in a relatively high-temperature environment, the SMA-13 asphalt mastic broken stone pavement which is the same as the actual engineering is used as an application object, SBS (I-D) modified asphalt is used, and the mixing temperature of the asphalt mixture is 185 ℃. The microcapsule wall is a high-molecular polymer material, the thermal stability of the microcapsule is researched, a thermogravimetric analyzer (TGA) is adopted to research the related properties of the self-melting ice agent of the self-made slow-release microcapsule along with the temperature change, the purging gas is selected as nitrogen in the test, and the temperature is slowly increased according to the setting of the thermogravimetric analyzer at the speed of 5 ℃/min. The test results are shown in fig. 7 and 8.
The curve in the thermogravimetric test result is the mass change trend of the test sample along with the rise of the test temperature. FIG. 7 shows the results of thermogravimetric tests before modification without the use of wall material. The test result shows that the mass loss of the inorganic material is started at 357 ℃, and heat loss is generated at the temperature, so that the use of the material in application is not influenced; FIG. 8 shows that the slow-release microcapsule self-melting ice agent sample has slight mass loss at 27 ℃, and the mass loss at the first stage when the temperature is raised to 60 ℃ is 6.9%, which is the evaporation of water in the material; the mass of the sample material is substantially unchanged during the 60 ℃ to 357 ℃ stage; the sample is decomposed from 357 ℃ to generate continuous mass loss, so that the decomposition temperature of the material is 357 ℃, the mixing temperature of the asphalt mixture is 180-185 ℃, the slow-release microcapsule self-melting ice agent has good thermal stability, and the decomposition temperature meets the preparation and use requirements of the mixture.
According to the invention, the blast furnace slag powder adsorbs the self-snow-melting core material into the pores, the snow-melting core material is furfural or plant straw pyrolysis waste liquid, the furfural or plant straw pyrolysis waste liquid is extracted and synthesized to prepare sodium acetate, and the surface of the adsorption core material carrier is subjected to macromolecular capsule wall modification treatment to form a microcapsule structure, so that a slow release effect is realized, and the self-snow-melting core material has good ice melting rate, moisture absorption rate and salt release amount and good thermal stability.
The self-melting ice performance of the sustained-release microcapsules obtained in the above examples is shown in the table;
| examples | Example one | Example two | EXAMPLE III | Example four |
| Ice melting ability (%) | 90.2 | 90.3 | 90.6 | 90.8 |
| Moisture absorption Rate (%) | 0.61 | 0.61 | 0.62 | 0.64 |
| Thermal stabilization | Good effect | Good effect | Good effect | Good effect |
While the invention has been described with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A self-thawing preparation process of sustained-release microcapsules is characterized by comprising the following steps:
s1, material preparation: the material required by the self-melting ice of the sustained-release microcapsule is furfural or acetic acid extracted and purified from plant straw pyrolysis waste liquid, and sodium acetate, an active agent OP-10 and a dispersant nano SiO are synthesized and prepared 2 Porous solid waste carrier blast furnace slag powder and corrosion inhibitor NaHCO 3 Monomer X, methyl acrylate, butyl acrylate, styrene, an initiator, a coupling agent and water;
s2, preparing the self-melting ice agent matrix: preparing saturated sodium acetate solution, adding activator OP-10 accounting for 3 percent of the mass of the saturated sodium acetate solution and dispersing agent nano SiO accounting for 1 percent of the mass of the saturated sodium acetate solution 2 Adding a corrosion inhibitor NaHCO with the mass of 5 percent of sodium acetate solution 3 Obtaining a mixed solution for later use;
s3, adding the mixed solution obtained in the step S2 and the porous solid waste carrier into a stirring mechanism for fully mixing and stirring to obtain a mixture;
s4, drying and dispersing the mixture obtained in S3 to obtain the self-melting ice agent to be modified;
s5, capsule wall preparation: mixing a monomer X, methyl acrylate, butyl acrylate and styrene to obtain a monomer mixed solution; adding an initiator and a coupling agent into the monomer mixed solution, then dropwise adding the mixture into a solvent preheated to 110 ℃, and polymerizing for 3 hours to obtain a modified capsule wall solution;
s6, modifying the self-melting ice agent: coating and modifying the self-melting ice agent to be modified prepared by S4 by using the modified capsule wall solution;
fully mixing the modified capsule wall solution, water and the self-melting ice agent to be modified to form paste;
drying, crushing and sieving the paste to obtain the self-melting ice of the sustained-release microcapsule.
2. The self-thawing preparation process of slow-release microcapsules of claim 1, wherein in the step S3, the mass ratio of the mixed solution to the porous solid waste carrier is 1: 2-2.3.
3. The self-thawing ice preparation process of sustained-release microcapsules according to claim 1, wherein the mixing and stirring time in the S3 is 1-1.5 h; the mixture was dried at 120-130 ℃ to constant weight in S4.
4. The self-thawing ice preparation process of slow-release microcapsules according to claim 1, wherein in S5, the ratio of the solvent: a monomer X: methyl acrylate: butyl acrylate: the mass ratio of styrene was set to 50:1:25:18: 8.
5. The self-thawing preparation process of claim 1, wherein a solvent in the S5 is isopropanol, and the monomer X is acrylic acid.
6. The self-melting ice preparation process of slow-release microcapsules of claim 1, wherein in S5, the initiator is AIBN and the coupling agent is silane coupling agent KH-570.
7. The self-melting ice preparation process of slow-release microcapsules according to claim 6, wherein AIBN accounting for 2.5% of the mass of the monomer mixed solution and a silane coupling agent KH-570 accounting for 0.8% of the mass of the monomer mixed solution are added to the monomer mixed solution in S5.
8. The self-melting ice preparation process of the sustained-release microcapsule according to claim 1, wherein the mass ratio of the modified capsule wall solution in S6, water and the self-melting ice agent to be modified is 1:0.6: 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210565997.XA CN114806505B (en) | 2022-05-24 | 2022-05-24 | Self-melting ice preparation process of sustained-release microcapsules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210565997.XA CN114806505B (en) | 2022-05-24 | 2022-05-24 | Self-melting ice preparation process of sustained-release microcapsules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114806505A true CN114806505A (en) | 2022-07-29 |
| CN114806505B CN114806505B (en) | 2023-02-28 |
Family
ID=82516378
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210565997.XA Active CN114806505B (en) | 2022-05-24 | 2022-05-24 | Self-melting ice preparation process of sustained-release microcapsules |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114806505B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010045160A (en) * | 1999-11-03 | 2001-06-05 | 정숭렬 | Chloride-free deicer composition and process for preparation thereof |
| WO2012129742A1 (en) * | 2011-03-30 | 2012-10-04 | 中交第一公路勘察设计研究院有限公司 | Eco-friendly road surface coating material for thawing ice and snow and methods of preparing and using the same |
| CN105565853A (en) * | 2015-12-16 | 2016-05-11 | 曾宪沅 | Ice melting particles |
| CN106047293A (en) * | 2016-07-01 | 2016-10-26 | 黄山九星环保科技有限公司 | Special carbon fiber composite snow-melting deicing agent for airports and manufacturing method thereof |
| CN108893095A (en) * | 2018-09-11 | 2018-11-27 | 重庆交通大学 | A kind of polymer shell cladding material, polymer wrapped delay-released inorganic salt and preparation method |
| CN109054415A (en) * | 2018-09-11 | 2018-12-21 | 河南省济阳高速公路建设有限公司 | A kind of active snow melt deicing asphalt and preparation method thereof |
| CN113429884A (en) * | 2021-05-29 | 2021-09-24 | 山东哈力克新材料科技有限公司 | Anti-freezing coating material for road and preparation method thereof |
| CN113528087A (en) * | 2021-08-16 | 2021-10-22 | 华北水利水电大学 | Environment-friendly slow-release snow-melting agent, preparation method thereof and application thereof in micro-surfacing mixture |
| CN114149788A (en) * | 2021-12-29 | 2022-03-08 | 南京兴佑交通科技有限公司 | Slow-release ice and snow melting agent, preparation method thereof and thin-layer cover material containing slow-release ice and snow melting agent |
-
2022
- 2022-05-24 CN CN202210565997.XA patent/CN114806505B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010045160A (en) * | 1999-11-03 | 2001-06-05 | 정숭렬 | Chloride-free deicer composition and process for preparation thereof |
| WO2012129742A1 (en) * | 2011-03-30 | 2012-10-04 | 中交第一公路勘察设计研究院有限公司 | Eco-friendly road surface coating material for thawing ice and snow and methods of preparing and using the same |
| CN105565853A (en) * | 2015-12-16 | 2016-05-11 | 曾宪沅 | Ice melting particles |
| CN106047293A (en) * | 2016-07-01 | 2016-10-26 | 黄山九星环保科技有限公司 | Special carbon fiber composite snow-melting deicing agent for airports and manufacturing method thereof |
| CN108893095A (en) * | 2018-09-11 | 2018-11-27 | 重庆交通大学 | A kind of polymer shell cladding material, polymer wrapped delay-released inorganic salt and preparation method |
| CN109054415A (en) * | 2018-09-11 | 2018-12-21 | 河南省济阳高速公路建设有限公司 | A kind of active snow melt deicing asphalt and preparation method thereof |
| CN113429884A (en) * | 2021-05-29 | 2021-09-24 | 山东哈力克新材料科技有限公司 | Anti-freezing coating material for road and preparation method thereof |
| CN113528087A (en) * | 2021-08-16 | 2021-10-22 | 华北水利水电大学 | Environment-friendly slow-release snow-melting agent, preparation method thereof and application thereof in micro-surfacing mixture |
| CN114149788A (en) * | 2021-12-29 | 2022-03-08 | 南京兴佑交通科技有限公司 | Slow-release ice and snow melting agent, preparation method thereof and thin-layer cover material containing slow-release ice and snow melting agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114806505B (en) | 2023-02-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103865487B (en) | Temperature-control released snow-melting agent microcapsule and preparation method thereof | |
| CN108559449B (en) | High-dilution-ratio aqueous liquid dust suppressant and preparation and use methods thereof | |
| CN105408280A (en) | Room-temperature circulation asphalt composition and road paving method using the same | |
| US20130330469A1 (en) | Eco-friendly road surface coating material for thawing ice and snow and methods of preparing and using the same | |
| CN102092978B (en) | Environmental-protection self-snow-melting asphalt pavement admixture and preparation method thereof | |
| CN109021598B (en) | Preparation method of hydrophobic anti-icing organic montmorillonite-SBS composite modified asphalt | |
| CN108893095B (en) | Polymer shell coating material, polymer-coated slow-release inorganic salt and preparation method | |
| CN102127365A (en) | Hydrophobic coating capable of lowering adhesion of ice layers for asphalt pavements | |
| CN106675055B (en) | Asphalt warm-mixing modifier and preparation method thereof | |
| CN114149788A (en) | Slow-release ice and snow melting agent, preparation method thereof and thin-layer cover material containing slow-release ice and snow melting agent | |
| CN111423157A (en) | Pavement material capable of automatically adjusting temperature of pavement and preparation method thereof | |
| CN111548771A (en) | Method for preparing low-temperature phase-change material by utilizing tetradecane and expanded graphite | |
| CN111592303A (en) | Preparation method of tetradecane expanded graphite low-temperature phase-change cement mortar | |
| CN102173645B (en) | Salt granule for inhibiting ice/snow on road pavement from freezing and preparation method thereof | |
| CN114806505B (en) | Self-melting ice preparation process of sustained-release microcapsules | |
| CN109534734B (en) | Anti-freezing micro-surfacing maintenance material and preparation method thereof | |
| CN110451848A (en) | The modified pitch and its preparation method that gather materials towards poor quality and application | |
| CN114988742A (en) | Slow-release long-acting type anti-freezing material and preparation method thereof | |
| CN102863805A (en) | Modified Qingchuan rock asphalt and preparation method thereof | |
| Zhao et al. | Preparation of a green sustained-release microcapsule-type anti-icing agent for asphalt pavement and its application demonstration project | |
| CN104877307A (en) | Salinization product granules for ultra-thin wearing layer of bituminous pavement and preparation method of salinization product granules | |
| CN111518516B (en) | Road surface anti-icing composition and manufacturing method thereof | |
| CN113897134A (en) | Energy-absorbing super-hydrophobic super-oleophobic anti-icing coating for power transmission line and preparation method thereof | |
| CN107793774A (en) | A kind of processes of rock asphalt modified asphalt oil abrasion method processing technology | |
| CN106400641B (en) | A kind of environmental protection of pavement material and its preparation easily dewatering type permeable pavement structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |