CN113583633A - Preparation method of phase change microcapsule with high coating rate - Google Patents
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Abstract
The invention discloses a preparation method of a phase-change microcapsule with high coating rate, which comprises the steps of taking melamine resin as a shell material and taking normal alkane as a core material to prepare the phase-change microcapsule by an in-situ polymerization method, firstly emulsifying the core material into emulsion drops with the diameter of 1-20 mu m by utilizing a reaction type emulsifier sodium lauroyl glutamate and an anionic emulsifier styrene-maleic anhydride, then adding a high-activity water-soluble melamine prepolymer to carry out coating, then adding a low-activity water-soluble melamine prepolymer to carry out secondary coating, adjusting the pH value of a system to be 3-5, carrying out gradient heating to completely crosslink and solidify the shell material, and carrying out spray drying on the obtained microcapsule emulsion to obtain fine and good-fluidity microcapsule powder. The phase change microcapsule prepared by the invention has smooth and monodisperse surface appearance, an enthalpy value of 198J/g, a coating rate of 95 percent, a compressive strength of 3MPa, no color change and oil leakage after being baked for 1h at 180 ℃, and a balance between a high enthalpy value and a high compressive strength of the phase change microcapsule is realized by a high coating rate, so that the phase change microcapsule can be widely applied to the fields of intelligent textile, consumer electronics and the like.
Description
Technical Field
The invention relates to the technical field of phase change energy storage materials, in particular to a preparation method of a phase change microcapsule with a high coating rate.
Background
The phase-change material is used as an energy storage carrier, can be converted back and forth between different phase states along with the change of the external environment temperature and releases or absorbs energy, so that the temperature of the phase-change material is not changed, the energy storage mode has high energy storage density, the energy can be repeatedly used, the volume change is small, the operation is simple, the attention of people is always paid, and the application of the phase-change material is greatly limited due to the easy leakage of the phase-change material in the phase-change process.
The microcapsule technology can encapsulate phase change materials in inorganic materials or high molecular polymers to prepare microcapsules with a core-shell structure, and the outer-layer capsule materials have a protection effect on the phase change materials in the inner layer, so that the stability and the repeated utilization rate of the phase change materials are improved, the phase change materials are widely applied to the fields of buildings, textiles, cold chains, electronics and the like, and the problems of energy conservation and energy storage are solved. At present, the preparation methods of microcapsules can be classified into three types, i.e., chemical methods, physical methods and physicochemical methods, wherein in-situ polymerization and interfacial polymerization in the chemical methods are the most common: (1) in the in-situ polymerization method, a monomer and a catalyst for synthesizing the wall material are added into a dispersion medium, and a polycondensation reaction is carried out on the surface of an emulsified core material under a certain condition to generate a high molecular polymer which is gradually deposited on the surface of the core material, so that the core material is encapsulated; (2) the interfacial polymerization method is to dissolve two monomers in immiscible solvents respectively, and when the two solvents are mixed and dispersed uniformly, a polymerization reaction occurs at the interface of a liquid phase, and a core material is coated to form a microcapsule.
The property of the microcapsule wall material directly determines the service performance of a microcapsule product, and simultaneously influences the preparation process of the microcapsule, and the melamine resin becomes a better capsule wall material due to the stable chemical property, good acid resistance, alkali resistance, difficult hydrolysis and the like. The Chinese patent application CN101113322B takes alkane with 5-50 carbon atoms as a core material, selects a non-ionic emulsifier for emulsification, takes a self-made water-soluble melamine prepolymer or urea-formaldehyde prepolymer as a capsule wall to obtain a monodisperse phase-change microcapsule with controllable size and controllable shape, adopts the core material emulsified by the non-ionic emulsifier, the surface of an emulsion drop of the core material is not charged, the prepolymer can not well coat the surface of the core material through the attraction effect between opposite charges, the coating rate of the capsule wall on the core material is greatly reduced, and the self-made melamine/urea-formaldehyde prepolymer is not modified by any etherification, and the molecular structure of the prepolymer hasA large number of hydroxymethyl bonds, the prepolymer has high reaction activity, and the prepolymer is easily self-polymerized into a high molecular polymer when not adsorbed on the surface of a core material in the process of coating the core material, so that the coating rate of the capsule wall is reduced. The Chinese patent application CN110479194A takes silicon carbide modified melamine resin subjected to hydrophobic treatment as a wall material, takes paraffin, fatty alcohol and fatty acid phase-change materials as core materials, and adopts an in-situ polymerization method to prepare the phase-change microcapsule, the mechanical property and the heat conductivity of the microcapsule are enhanced by introducing hydrophobic silicon carbide, but the hydrophobic silicon carbide is directly added into a phase-change material emulsion for dispersion, so that emulsion breaking of the emulsion is easily caused, part of the phase-change materials are separated out and cannot be coated by the capsule wall, the coating rate of the capsule wall is reduced, and the uncoated phase-change materials are subsequently washed and removed by petroleum ether or ethanol, so that raw material waste and environmental pollution are caused. Chinese patent application CN112604614A adopts melamine resin to C14-C12Alkane and nano-alumina are mixed for coating, and then carbon nano-tubes are added for modifying the capsule wall, so that the phase change microcapsule which can be used in the field of cold chain transportation is prepared, the supercooling degree is reduced by introducing the nano-alumina and the carbon nano-tubes, the thermal conductivity is improved, the compatibility of inorganic nano-particles and the alkane is poor, long-time ultrasonic dispersion is needed during blending and coating, the industrial amplification production is not favorably realized, the surface of the microcapsule becomes rough after the carbon nano-tubes are modified, and the monodispersity of the microcapsule is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a phase-change microcapsule with high coating rate, which aims to overcome the defects of the prior art, increases the adsorption capacity of a prepolymer on the surface of a core material by selecting an emulsifier, adopts prepolymers with high and low reaction activities to realize double-layer coating on the core material, realizes the balance of the strength and toughness of the microcapsule, and avoids the problems that the coating rate is low and the enthalpy value and the compressive strength are not influenced due to self-polymerization of a large amount of shell materials.
According to the invention, a reactive emulsifier sodium lauroyl glutamate and an anionic emulsifier styrene-maleic anhydride are compounded to emulsify a phase change core material, a high-activity melamine prepolymer is added to coat the phase change core material, the prepolymer is positively charged, the surface of emulsion droplets of the phase change core material is negatively charged due to the use of the anionic emulsifier, the prepolymer is enriched on the surface of the emulsion droplets due to mutual attraction between positive and negative charges, amino groups in the sodium lauroyl glutamate molecule and hydroxymethyl groups and aldehyde groups in the prepolymer can react with each other, the prepolymer is more firmly and rapidly coated on the surface of the phase change core material due to double acting forces of electrostatic attraction and chemical bonds, the prepolymer is prevented from self-aggregating into spheres in a system, and the coating rate of the core material by a wall material is obviously improved compared with the use of the anionic emulsifier, the nonionic emulsifier and the compounding of the anionic emulsifier and the nonionic emulsifier. After the high-activity melamine prepolymer is coated, the low-activity melamine prepolymer is added to form secondary coating, and the high-activity melamine prepolymer has more crosslinkable active groups such as hydroxymethyl and amino, so that excellent chemical resistance and strength can be provided after polymerization, but the shell material has large brittleness due to the rigid structure of a great amount of triazine rings generated by polymerization, so that the core material is easy to break when being impacted by external force by only using the high-activity melamine prepolymer as the shell material, the core material leaks, the low-activity melamine prepolymer with high etherification degree has more ether bonds in the molecules and good molecular flexibility, the shell formed by the low-activity melamine prepolymer is further coated on the outer layer, the toughness of the wall material can be obviously improved, the compressive strength of the microcapsule is enhanced, meanwhile, the low-activity melamine prepolymer has a low polymerization speed, and the prepolymer has enough time to migrate to the surface of the liquid drop for coating before polymerization, so that the coating rate of the wall material on the core material is improved.
In order to achieve the aim, the invention provides a preparation method of a phase-change microcapsule with high coating rate, which comprises the following steps:
1) preparing phase-change core material emulsion: adding acid into the emulsifier to adjust the pH value to 4-6, heating to 40-70 ℃, heating the phase-change core material to melt the phase-change core material into a liquid state, adding the liquid state into the emulsifier, and dispersing at a high speed for 5-30min to obtain a phase-change core material emulsion;
2) preparation of phase-change microcapsule emulsion: adding a high-activity melamine prepolymer solution with low degree of etherification into a phase-change core material emulsion for coating, reacting at 40-70 ℃ for 10-30min to complete coating, adding a low-activity melamine prepolymer solution for secondary coating, adding an acid to adjust the pH value of the system to be 4-5, keeping the temperature at 40-70 ℃ for 1-3h, heating to 60-80 ℃, continuing to perform heat preservation reaction for 1-3h, then continuing to heat to 80-95 ℃ for 1-2h, adding an acid to adjust the pH value of the system to be 3-4, keeping the temperature for 1-2h to fully solidify a shell material, and cooling to room temperature to obtain a phase-change microcapsule emulsion;
3) preparation of phase change microcapsule powder: dehydrating and drying the phase-change microcapsule emulsion to obtain phase-change microcapsule powder;
to further achieve the object of the present invention, preferably, the phase change core material is one or more of n-tetradecane, n-hexadecane, n-octadecane and n-docosane.
Preferably, the emulsifier is a compound of 1-10 mass percent of reactive emulsifier sodium lauroyl glutamate and 1-10 mass percent of anionic emulsifier styrene-maleic anhydride
Preferably, the anionic emulsifier styrene-maleic anhydride has one or more of molecular weights 520, 820, 1000.
Preferably, the acid used for adjusting the emulsification system pH 4-6 in the step 1) and the emulsion preparation process adjusting system pH 4-5 and pH 3-4 in the step 2) is one or more of citric acid, acrylic acid, acetic acid, dilute sulfuric acid and dilute hydrochloric acid.
Preferably, the addition amount of the emulsifier is 6-20% of the phase change core material.
Preferably, the low-activity melamine prepolymer is cyanite 350, and the higher-activity melamine prepolymer is cyanite 385.
Preferably, the solid content of the phase-change microcapsule emulsion prepared in the step 2) is 30-50%.
Preferably, the dehydration drying mode is one or more of oven drying and spray drying.
Furthermore, the air inlet amount is 100 percent, the air inlet temperature is 130-.
Compared with the prior art, the invention has the following outstanding effects:
1. the reactive emulsifier and the anionic emulsifier are compounded, so that the attraction of electrostatic attraction is removed when the wall material is coated on the surface of the core material, the wall material also has the function of chemical bonds, the difficulty of stacking and coating the wall material on the surface of the core material is reduced, and the coating rate is increased.
2. The high-activity melamine prepolymer is adopted for double-layer coating, the high-activity melamine prepolymer provides rigidity required by a wall material, the etherified and modified low-activity melamine prepolymer improves the flexibility of the wall material, simultaneously weakens the integral reaction activity of the melamine prepolymer, reduces the possibility that the wall material can form core by self polymerization before the wall material is not coated with the core material, and improves the coating rate of the wall material on the core material.
3. The coating rate of the wall material to the core material reaches 95%, the balance of the enthalpy value and the pressure resistance of the microcapsule is realized, the enthalpy value of the microcapsule reaches 198J/g, and the pressure resistance strength is 3 MPa.
Drawings
FIG. 1 is an SEM image of phase change microcapsules of example 4;
FIG. 2 is an optical microscope photograph of phase change microcapsules of example 4;
FIG. 3 is an optical microscope photograph of the phase change microcapsules of example 4 after being pressed by a tablet press with a pressure of 3MPa and a holding time of 1 min;
FIG. 4 is a DSC of the phase change microcapsules of example 4.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
1) Preparing phase-change core material emulsion: mixing 40g of sodium lauroyl glutamate with the mass fraction of 5% and 80g of SMA520 with the mass fraction of 5%, adding 10% of citric acid aqueous solution to adjust the pH to 4.3, heating to 50 ℃, adding 80g of n-octadecane into an emulsifier after melting into a liquid state at 50 ℃, and dispersing at a high speed of 4000rpm for 30min to obtain a phase change core material emulsion;
2) preparation of phase-change microcapsule emulsion: preparing 8g of high-activity melamine prepolymer cyanogen 385 into a 50% solution by using deionized water, adding the solution into a phase-change core material emulsion for coating, reacting at 70 ℃ for 15min to complete coating, adding 4.8g of low-activity melamine prepolymer solution cyanogen 350 with the mass fraction of 50% for secondary coating, adding 10% citric acid aqueous solution to adjust the pH of a system to be 5, keeping the temperature at 70 ℃ for 2h, heating to 80 ℃ for continuous heat preservation reaction for 2h, then continuously heating to 95 ℃ for heat preservation for 1h, adding 10% citric acid aqueous solution to adjust the pH of the system to be 3.4, keeping the temperature for 1h to fully solidify a shell material, and cooling to room temperature to obtain the phase-change microcapsule emulsion;
3) preparation of phase change microcapsule powder: diluting the prepared microcapsule emulsion with deionized water to 15%, and preparing microcapsule powder by spray drying equipment, wherein the air inlet amount is 100%, the air inlet temperature is 135 ℃, and the feeding rate is 40%.
Example 2
1) Preparing phase-change core material emulsion: mixing 60g of 5 mass percent sodium lauroyl glutamate and 80g of 5 mass percent SMA520, adding 10 percent citric acid aqueous solution to adjust the pH to 4.7, heating to 60 ℃, melting 80g of n-octadecane into liquid at 60 ℃, adding the liquid into an emulsifier, and dispersing at 3000rpm for 30min to obtain phase change core material emulsion;
2) preparation of phase-change microcapsule emulsion: preparing 12.4g of high-activity melamine prepolymer cyanogen 385 into a 50% solution by using deionized water, adding the solution into a phase-change core material emulsion for coating, reacting at 60 ℃ for 30min to complete coating, adding 2g of low-activity melamine prepolymer solution cyanogen 350 with the mass fraction of 50% for secondary coating, adding 10% citric acid aqueous solution to adjust the pH of a system to be 5, keeping the temperature at 60 ℃ for 3h, heating to 70 ℃ for continuous heat preservation reaction for 2h, then continuously heating to 90 ℃ for heat preservation for 2h, adding 10% citric acid aqueous solution to adjust the pH of the system to be 3.4, keeping the temperature for 2h to fully solidify a shell material, and cooling to room temperature to obtain the phase-change microcapsule emulsion;
3) preparation of phase change microcapsule powder: diluting the prepared microcapsule emulsion with deionized water to 15%, and preparing microcapsule powder by spray drying equipment, wherein the air inlet amount is 100%, the air inlet temperature is 135 ℃, and the feeding rate is 40%.
Example 3
1) Preparing phase-change core material emulsion: mixing 40g of sodium lauroyl glutamate with the mass fraction of 5% and 80g of SMA820 with the mass fraction of 5%, adding 10% of citric acid aqueous solution to adjust the pH to 5, heating to 70 ℃, melting 70g of n-octadecane and 10g of n-hexadecane into liquid at 70 ℃, adding the liquid into an emulsifier, and dispersing at high speed of 3000rpm for 30min to obtain phase change core material emulsion;
2) preparation of phase-change microcapsule emulsion: preparing 15g of high-activity melamine prepolymer cyanogen-tert 385 into a 50% solution by using deionized water, adding the solution into a phase-change core material emulsion for coating, reacting at 70 ℃ for 20min, then adding 4g of low-activity melamine prepolymer solution cyanogen-tert 350 with the mass fraction of 50% for secondary coating, adding 10% citric acid aqueous solution to adjust the pH of a system to be 4.5, keeping the temperature at 70 ℃ for 3h, heating to 80 ℃ for continuous heat preservation reaction for 2h, then continuously heating to 95 ℃ for heat preservation for 2h, adding 10% citric acid aqueous solution to adjust the pH of the system to be 3, keeping the temperature for 1h to fully solidify a shell material, and cooling to room temperature to obtain the phase-change microcapsule emulsion;
3) preparation of phase change microcapsule powder: diluting the prepared microcapsule emulsion with deionized water to 15%, and preparing microcapsule powder by spray drying equipment, wherein the air inlet amount is 100%, the air inlet temperature is 135 ℃, and the feeding rate is 40%.
Example 4
1) Preparing phase-change core material emulsion: mixing 60g of 5 mass percent sodium lauroyl glutamate and 80g of 5 mass percent SMA1000, adding 10 percent citric acid aqueous solution to adjust the pH value to 5.2, heating to 70 ℃, adding 80g of n-octadecane into an emulsifier after melting into a liquid state at 70 ℃, and dispersing at high speed of 5000rpm for 30min to obtain a phase change core material emulsion;
2) preparation of phase-change microcapsule emulsion: preparing 10g of high-activity melamine prepolymer cyanogen-tert 385 into a 50% solution by using deionized water, adding the solution into a phase-change core material emulsion for coating, reacting at 70 ℃ for 10min to complete coating, adding 3g of low-activity melamine prepolymer solution cyanogen-tert 350 with the mass fraction of 50% for secondary coating, adding 10% citric acid aqueous solution to adjust the pH of a system to be 4.2, keeping the temperature at 75 ℃ for 2h, heating to 80 ℃ for continuous heat preservation reaction for 2h, then continuously heating to 95 ℃ for heat preservation for 2h, adding 10% citric acid aqueous solution to adjust the pH of the system to be 4, keeping the temperature for 2h to fully solidify a shell material, and cooling to room temperature to obtain the phase-change microcapsule emulsion;
3) preparation of phase change microcapsule powder: diluting the prepared microcapsule emulsion with deionized water to 15%, preparing microcapsule powder with spray drying equipment, wherein the air inlet amount is 100%, the air inlet temperature is 135 deg.C, the feeding rate is 40%, and the optical micrograph of the finally obtained phase change microcapsule is shown in figure 1.
Comparative example
PCM28 phase change microcapsule powder produced by Microtek lab, USA
TABLE 1 examples and comparative examples Properties
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example | |
| Coating rate | 90％ | 88％ | 87％ | 95％ | 85％ |
| Enthalpy value | 191J/g | 186J/g | 182J/g | 198J/g | 179J/g |
| Compressive strength | 2MPa | 1MPa | 1MPa | 3MPa | 1MPa |
From the properties tested in table 1, the enthalpy values of the examples are superior to those of the comparative examples by achieving high coating ratios for the core material, meanwhile, the compression strength is superior to or equivalent to that of a comparative example, the enthalpy value of the prepared phase change microcapsule can reach 198J/g, the coating rate can reach 95 percent, the compression strength can reach 3MPa, the higher coating rate ensures that more wall materials form coating on the surface of the core material, but not self-nucleating in the system, as shown in figure 2, the SEM picture shows that the sphericity of the microcapsule is complete, the surface is smooth and has no any small particle adhesion, and the perfect coating of the wall material on the core material is also confirmed, so that the wall material in example 4 has higher compressive strength although the added amount of the wall material is small, while the addition of a smaller amount of wall material provides a higher enthalpy value for the microcapsules, example 4 has significant advantages in enthalpy value and compressive strength over the currently marketed products, as shown in figures 3 and 4.
Claims (10)
1. A preparation method of a phase-change microcapsule with high coating rate is characterized by comprising the following steps:
1) preparing phase-change core material emulsion: adding acid into the emulsifier to adjust the pH value to 4-6, heating to 40-70 ℃, heating the phase-change core material to melt the phase-change core material into a liquid state, adding the liquid state into the emulsifier, and dispersing at a high speed for 5-30min to obtain a phase-change core material emulsion;
2) preparation of phase-change microcapsule emulsion: adding a high-activity melamine prepolymer solution with low degree of etherification into a phase-change core material emulsion for coating, reacting at 40-70 ℃ for 10-30min to complete coating, adding a low-activity melamine prepolymer solution for secondary coating, adding an acid to adjust the pH value of the system to be 4-5, keeping the temperature at 40-70 ℃ for 1-3h, heating to 60-80 ℃, continuing to perform heat preservation reaction for 1-3h, then continuing to heat to 80-95 ℃ for 1-2h, adding an acid to adjust the pH value of the system to be 3-4, keeping the temperature for 1-2h to fully solidify a shell material, and cooling to room temperature to obtain a phase-change microcapsule emulsion;
3) preparation of phase change microcapsule powder: and dehydrating and drying the phase-change microcapsule emulsion to obtain phase-change microcapsule powder.
2. The method for preparing the phase-change microcapsule with high coating rate according to claim 1, wherein the method comprises the following steps: the phase change core material is one or more of n-tetradecane, n-hexadecane, n-octadecane and n-docosane.
3. The method for preparing phase-change microcapsules with high coating rate according to any one of claims 1 or 2, wherein: the emulsifier is prepared by compounding 1-10 mass percent of reactive emulsifier sodium lauroyl glutamate and 1-10 mass percent of anionic emulsifier styrene-maleic anhydride.
4. The method for preparing the phase-change microcapsule with high coating rate according to claim 3, wherein the method comprises the following steps: the molecular weight of the anionic emulsifier styrene-maleic anhydride is 520, 820 and 1000 or more.
5. The method for preparing the phase-change microcapsule with high coating rate according to claim 3, wherein the method comprises the following steps: the acid used for adjusting the pH in the step 1) and the step 2) is one or more of citric acid, acrylic acid, acetic acid, dilute sulfuric acid and dilute hydrochloric acid.
6. The method for preparing the phase-change microcapsule with high coating rate according to claim 3, wherein the method comprises the following steps: the addition amount of the emulsifier is 6-20% of the phase change core material.
7. The method for preparing the phase-change microcapsule with high coating rate according to claim 3, wherein the method comprises the following steps: the low-activity melamine prepolymer is Cyanote 350, and the higher-activity melamine prepolymer is Cyanote 385.
8. The method for preparing the phase-change microcapsule with high coating rate according to claim 3, wherein the method comprises the following steps: the solid content of the phase change microcapsule emulsion prepared in the step 2) is 30-50%.
9. The method for preparing the phase-change microcapsule with high coating rate according to claim 3, wherein the method comprises the following steps: the dehydration drying mode in the step 3) can adopt one or more of oven drying and spray drying.
10. The method for preparing the phase-change microcapsule with high coating rate according to claim 9, wherein: when the spray drying is used for preparing the powder, the air inlet air quantity is 100 percent, the air inlet temperature is 130-150 ℃, and the feeding speed is 30-60 percent.
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| CN116574421A (en) * | 2023-05-31 | 2023-08-11 | 安徽佐研化学科技有限公司 | Light heat-insulating paint and preparation method thereof |
| CN116574421B (en) * | 2023-05-31 | 2024-05-10 | 安徽佐研化学科技有限公司 | Light heat-insulating paint and preparation method thereof |
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