CN113694846A - MQ silicon resin coated phase-change microcapsule and preparation method and application thereof - Google Patents
MQ silicon resin coated phase-change microcapsule and preparation method and application thereof Download PDFInfo
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Abstract
The application belongs to the technical field of phase change energy storage materials, and particularly relates to an MQ silicon resin coated phase change microcapsule, and a preparation method and application thereof. The invention provides an MQ silicon resin coated phase change microcapsule, which comprises: MQ silicon resin and a phase-change material, wherein the MQ silicon resin coats the phase-change material; the MQ silicon resin is of a three-dimensional cross-linked network structure, can well adapt to the heat absorption expansion of the phase-change material, prevents the crack and other defects of the coating layer, improves the matching property with the thermal expansion rate of the phase-change material, relieves the leakage caused by volume expansion in the phase-change process of the phase-change material, and improves the leakage resistance of the phase-change microcapsule; the phase change microcapsule coated with the MQ silicon resin, and the preparation method and the application thereof can solve the technical problem that a phase change material in the phase change microcapsule prepared by the prior art is easy to leak.
Description
Technical Field
The application belongs to the technical field of phase change energy storage materials, and particularly relates to an MQ silicon resin coated phase change microcapsule, and a preparation method and application thereof.
Background
The solid-liquid phase change material is easy to flow after being heated and transformed into a liquid state, so that the use environment is polluted, and meanwhile, part of the phase change material has the defects of low heat conductivity coefficient, flammability and the like, so that the application range of the solid-liquid phase change material is limited; the phase-change material is prepared into micro-or nano-particles by a phase-change microencapsulation technology, and then a layer of stable molecular film is coated on the surface of the micro-or nano-particles, so that the micro-or nano-capsules with the core-shell structure can be obtained, the phase-change material is not influenced by the external environment and working media, and the problems that the phase-change material is easy to flow and pollutes the use environment after being heated and phase-changed into a liquid state can be solved.
The method for preparing the phase-change microcapsule in the prior art comprises an emulsion polymerization method, a spray drying method and a sol-gel method; the emulsion polymerization method comprises the steps of uniformly dispersing a phase-change material and a shell material in a reaction medium under the action of an emulsifier, polymerizing and coating the shell material outside the phase-change material, and the like, so that the step of preparing the phase-change microcapsule by the emulsion polymerization method is complicated; the spray drying method is characterized in that a mixed solution of a phase change material and a coating layer is sprayed into a heating chamber through a spray dryer, liquid drops are subjected to liquid evaporation, solute diffusion, drying, precipitation and other steps to finally form solid powder particles, however, the phase change material is easy to agglomerate in the spray drying process, the coating layer is easy to have uneven distribution and uneven thickness, even has no coating phenomenon, and the phase change material in the phase change microcapsule prepared by the spray drying method is easy to leak; the sol-gel method is a method of solidifying compounds (called precursors) with high chemical activity such as inorganic substances or metal alkoxides and the like through solution, sol and gel, and then forming the phase-change material microcapsule through heat treatment and drying, however, the aging time of the sol-gel method is too long, and in the process of forming the phase-change material microcapsule through heat treatment and drying, the shell layer is easy to have shape defects such as dent, wrinkle, crack, micropore, uneven thickness and the like, so that the time for preparing the phase-change microcapsule through the sol-gel method is long, and the phase-change material in the prepared phase-change microcapsule is easy to leak.
Disclosure of Invention
In view of the above, the application provides an MQ silicone resin coated phase-change microcapsule, and a preparation method and an application thereof, which can solve the technical problem that a phase-change material in a phase-change microcapsule prepared in the prior art is easy to leak.
The present application provides in a first aspect MQ silicone coated phase change microcapsules, the MQ silicone coated phase change microcapsules comprising: MQ silicone and phase change materials;
the MQ silicon resin coats the phase change material.
Preferably, the MQ silicone resin comprises any one, two or more of methyl MQ silicone resin, methyl hydrogen-containing MQ silicone resin, methyl phenyl MQ silicone resin, vinyl MQ silicone resin, phenyl MQ silicone resin and fluorine-containing MQ silicone resin.
Preferably, the MQ silicone resin is a methyl MQ silicone resin.
It should be noted that, the MQ silicon resin is a silicon resin composed of a monofunctional group Si-O unit (abbreviated as M unit) of the core layer and a tetrafunctional group Si-O unit (abbreviated as Q unit) of the shell layer, when all groups connected with the Si-O unit of the shell layer are methyl, the MQ silicon resin is called methyl MQ silicon resin, and since the methyl MQ silicon resin contains about 80% of silicon dioxide, the methyl MQ silicon resin has good thermal stability, on one hand, the flame retardant property of the phase change microcapsule coated by the MQ silicon resin can be improved, on the other hand, the methyl MQ silicon resin with good thermal stability is used as the shell layer, compared with the shell layer with poor thermal stability, the phase change material easily leaks due to decomposition of the shell layer with poor thermal stability in the heat absorption process of the phase change material can also be avoided.
Preferably, the phase change temperature of the phase change material is 20-170 ℃.
Preferably, the phase change material comprises any one, two or more of organic silicon wax, alcohol phase change material, ester phase change material and inorganic phase change material.
Preferably, the phase change material is paraffin.
The second aspect of the application provides a preparation method of the MQ silicon resin coated phase change microcapsule, which comprises the following steps:
step 1, placing a phase-change material, absolute ethyl alcohol and MQ silicon resin in a condensation reflux device, heating and stirring to obtain a phase-change microcapsule solution;
step 2, slowly dripping water until no precipitate is separated out from the phase change microcapsule solution to obtain a phase change microcapsule suspension;
and 3, carrying out suction filtration on the phase change microcapsule suspension to obtain the phase change microcapsule.
It should be noted that, the solubility of MQ silicone resin in ethanol is extremely low, so that MQ silicone resin can be dissolved in absolute ethanol, while the phase change material is a mixture of various hydrocarbons with a large number of carbon atoms, and is a nonpolar molecule, and absolute ethanol is a polar molecule, and according to the principle of similar compatibility, the phase change material is insoluble in absolute ethanol, so that the phase change material, absolute ethanol and MQ silicone resin are placed in a condensation reflux device for heating and stirring, so that MQ silicone resin is dissolved in absolute ethanol, while the phase change material is insoluble in absolute ethanol, thereby forming a mixed solution composed of an immiscible ethanol part and a phase change material part of MQ silicone resin; meanwhile, along with slowly dripping water, the MQ silicon resin is gradually separated out and wraps the phase change material, the phase change microcapsule is gradually separated out to form a phase change microcapsule suspension, and finally, the phase change microcapsule is obtained by suction filtration.
Preferably, the heating and stirring of the phase change material, the absolute ethyl alcohol and the MQ silicone resin in the condensing reflux device specifically comprises:
and the phase change material, absolute ethyl alcohol and MQ silicon resin are placed in a condensing reflux device for heating, stirring and ultrasonic treatment.
It should be noted that the solution can be oscillated by ultrasound, on one hand, the dissolution of the MQ silicone resin in the absolute ethyl alcohol can be promoted, on the other hand, droplets of the immiscible MQ silicone resin/ethanol solution part and the phase-change material solution part in the mixed solution can be reduced, the particle size of the phase-change microcapsule is reduced, and meanwhile, the MQ silicone resin ethanol solution part and the phase-change material solution part in the mixed solution are uniformly dispersed, and the size difference between the phase-change microcapsules is reduced.
Preferably, the phase change material, the absolute ethyl alcohol and the MQ silicon resin are placed in a condensing reflux device to be heated and stirred, and the obtained phase change microcapsule solution specifically comprises:
placing the phase change material, absolute ethyl alcohol and MQ silicon resin in a condensing reflux device, keeping the heating temperature above 60 ℃, and heating and stirring for 0.5-2h at the stirring speed of 500-1000r/min to obtain the phase change microcapsule solution.
Preferably, the phase-change microcapsule suspension comprises 10-100 parts of phase-change material, 20-150 parts of absolute ethyl alcohol and 10-100 parts of MQ silicone resin by mass.
The third aspect of the application provides the application of the above MQ silicon resin coated phase change microcapsule in the technical field of thermal management.
In summary, the present application provides MQ silicone resin coated phase change microcapsules and a method for preparing the same; the MQ silicone resin coated phase change microcapsule comprises: the phase change microcapsule comprises an MQ silicon resin shell layer and a phase change material core layer, wherein the MQ silicon resin is of a three-dimensional cross-linked network structure and can well adapt to the heat absorption expansion of the phase change material and prevent the coating layer from generating cracks and other defects, so that the matching property of the thermal expansion rate of the phase change material with the core layer is improved, the leakage caused by volume expansion in the phase change process of the phase change material of the core layer is relieved, and the leakage resistance of the phase change microcapsule is improved; the phase change microcapsule coated with the MQ silicon resin, and the preparation method and the application thereof can solve the technical problem that a phase change material in the phase change microcapsule prepared by the prior art is easy to leak.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a flow chart of preparation of MQ silicone phase change material microcapsules of the present application.
The specific implementation mode is as follows:
the application provides an MQ silicon resin coated phase change microcapsule, a preparation method and application thereof, which can solve the technical problem that phase change materials in the phase change microcapsules prepared in the prior art are easy to leak.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The reagents or raw materials used in the following examples are commercially available or self-made.
Example 1
This example 1 provides a first method for preparing MQ silicone resin-coated phase-change microcapsules, which includes the following steps.
Step 1, preparing an MQ silicon resin coated phase change microcapsule solution.
Step 101, respectively weighing 200g of absolute ethyl alcohol, 100g of paraffin and 100g of methyl MQ silicon resin, placing the weighed materials in a 1000ml three-neck flask, respectively installing a reflux condenser tube, a stirring device and a glass plug at the mouth of each of the three flasks, and finally placing the 1000ml three-neck flask in a water bath or oil bath;
and 102, controlling the heating temperature of the water bath or oil bath pot to be more than 60 ℃, controlling a stirring device to heat and stir at the stirring speed of 500r/min, and carrying out condensation reflux for 2 hours to obtain the MQ silicon resin coated phase change microcapsule solution.
And 2, preparing the MQ silicon resin coated phase change microcapsule suspension.
Step 201, after heating, taking out 1000ml of three-neck flask from a water bath or oil bath pot, and naturally cooling to room temperature after MQ silicon resin coated phase change microcapsule solution in the three-neck flask;
step 202, slowly adding water into the MQ silicon resin coated phase change microcapsule solution cooled to room temperature in a dropwise manner, gradually precipitating precipitates in the MQ silicon resin coated phase change microcapsule solution along with the dropwise addition of water, and finally stopping the dropwise addition of water when no precipitate is precipitated, thus obtaining the MQ silicon resin coated phase change microcapsule suspension.
And 3, preparing the MQ silicon resin coated phase change microcapsule.
Step 301, pouring the MQ silicone resin coated phase change microcapsule suspension in the three-neck flask into a Buchner funnel, performing suction filtration, and drying to obtain the MQ silicone resin coated phase change microcapsule.
Compared with the steps of firstly uniformly dispersing the phase change material and the shell material in the reaction medium through the emulsification of the emulsifier, and then carrying out polymerization reaction and coating on the shell material outside the phase change material, the method for coating the phase change microcapsule by the MQ silicone resin is synthesized by a one-pot method, so that the preparation process is simplified, and the resource waste is reduced; compared with the spray drying method that the phase change material is easy to agglomerate in the coating process, the coating layer is easy to have uneven distribution, different thickness and even no coating phenomenon, the phase change material and the MQ silicon resin in the method for coating the phase change microcapsule by the MQ silicon resin have good dispersibility in absolute ethyl alcohol and are not easy to agglomerate; compared with the sol-gel method that the shell layer is easy to have depressions, wrinkles, cracks, micropores and uneven thickness in the process of forming the phase-change material microcapsule by heat treatment and drying, the method for forming the MQ silicon resin coated phase-change microcapsule does not need heat treatment, so that the shell layer defect is not easy to occur, the coating property is good, and compared with the longer time for forming gel by aging of the sol-gel method, the method for forming the phase-change material microcapsule has short heating time and shortens the time for preparing the phase-change microcapsule; therefore, the method for coating the phase change microcapsule by the MQ silicon resin can solve the technical problems that the existing phase change microcapsule preparation method is complicated in steps and long in time, the coating effect of the shell layer is poor, the appearance defect of the shell layer is easy to occur, and the leakage is easy to occur.
Example 2
This example 2 provides a first method for preparing MQ silicone resin-coated phase-change microcapsules, which includes the following steps.
Step 1, preparing the MQ silicon resin coated phase change microcapsule solution.
Step 101, respectively weighing 200g of absolute ethyl alcohol, 100g of organic silicon wax and 100g of methyl MQ silicon resin, placing the weighed materials in a 1000ml three-neck flask, respectively installing a reflux condenser tube, a stirring device and a glass plug at the mouth of each of the three flasks, and finally placing the 1000ml three-neck flask in a water bath pot or an oil bath;
and 102, controlling the heating temperature of the water bath or oil bath pot to be more than 60 ℃, controlling a stirring device to heat and stir at the stirring speed of 500r/min, and carrying out condensation reflux for 2 hours to obtain the MQ silicon resin coated phase change microcapsule solution.
And 2, preparing the MQ silicon resin coated phase change microcapsule suspension.
Step 201, after heating, taking out 1000ml of three-neck flask from a water bath or oil bath pot, and naturally cooling to room temperature after MQ silicon resin coated phase change microcapsule solution in the three-neck flask;
step 202, slowly adding water into the MQ silicon resin coated phase change microcapsule solution cooled to room temperature in a dropwise manner, gradually precipitating precipitates in the MQ silicon resin coated phase change microcapsule solution along with the dropwise addition of water, and finally stopping the dropwise addition of water when no precipitate is precipitated, thus obtaining the MQ silicon resin coated phase change microcapsule suspension.
And 3, preparing the MQ silicon resin coated phase change microcapsule.
Step 301, pouring the MQ silicone resin coated phase change microcapsule suspension in the three-neck flask into a Buchner funnel, performing suction filtration, and drying to obtain the MQ silicone resin coated phase change microcapsule.
Example 3
This example 3 provides a first method for preparing MQ silicone resin-coated phase-change microcapsules, which includes the following steps.
Step 1, preparing the MQ silicon resin coated phase change microcapsule solution.
Step 101, respectively weighing 200g of absolute ethyl alcohol, 100g of paraffin and 100g of vinyl MQ silicon resin, placing the weighed materials in a 1000ml three-neck flask, respectively installing a reflux condenser tube, a stirring device and a glass plug at the mouth of each of the three flasks, and finally placing the 1000ml three-neck flask in a water bath or oil bath;
and 102, controlling the heating temperature of the water bath or oil bath kettle to be more than 60 ℃, controlling a stirring device to heat and stir at the stirring speed of 500/min, and carrying out condensation reflux for 2 hours to obtain the MQ silicon resin coated phase change microcapsule solution.
And 2, preparing the MQ silicon resin coated phase change microcapsule suspension.
Step 201, after heating, taking out 1000ml of three-neck flask from a water bath or oil bath pot, and naturally cooling to room temperature after MQ silicon resin coated phase change microcapsule solution in the three-neck flask;
step 202, slowly adding water into the MQ silicon resin coated phase change microcapsule solution cooled to room temperature in a dropwise manner, gradually precipitating precipitates in the MQ silicon resin coated phase change microcapsule solution along with the dropwise addition of water, and finally stopping the dropwise addition of water when no precipitate is precipitated, thus obtaining the MQ silicon resin coated phase change microcapsule suspension.
And 3, preparing the MQ silicon resin coated phase change microcapsule.
Step 301, pouring the MQ silicone resin coated phase change microcapsule suspension in the three-neck flask into a Buchner funnel, performing suction filtration, and drying to obtain the MQ silicone resin coated phase change microcapsule.
Example 4
This example 4 provides a first method for preparing MQ silicone resin-coated phase-change microcapsules, which includes the following steps.
Step 1, preparing an MQ silicon resin coated phase change microcapsule solution.
Step 101, respectively weighing 200g of absolute ethyl alcohol, 100g of paraffin and 100g of methyl MQ silicon resin, placing the weighed materials in a 1000ml three-neck flask, respectively installing a reflux condenser tube, a stirring device and a glass plug at the mouth of each of the three flasks, and finally placing the 1000ml three-neck flask in a water bath or oil bath pan for ultrasound;
and 102, controlling the heating temperature of the water bath or oil bath pot to be more than 60 ℃, controlling a stirring device to heat and stir at the stirring speed of 500r/min, and carrying out condensation reflux for 2 hours to obtain the MQ silicon resin coated phase change microcapsule solution.
And 2, preparing the MQ silicon resin coated phase change microcapsule suspension.
Step 201, after heating, taking out 1000ml of three-neck flask from a water bath or oil bath pot, and naturally cooling to room temperature after MQ silicon resin coated phase change microcapsule solution in the three-neck flask;
step 202, slowly adding water into the MQ silicon resin coated phase change microcapsule solution cooled to room temperature in a dropwise manner, gradually precipitating precipitates in the MQ silicon resin coated phase change microcapsule solution along with the dropwise addition of water, and finally stopping the dropwise addition of water when no precipitate is precipitated, thus obtaining the MQ silicon resin coated phase change microcapsule suspension.
And 3, preparing the MQ silicon resin coated phase change microcapsule.
Step 301, pouring the MQ silicone resin coated phase change microcapsule suspension in the three-neck flask into a Buchner funnel, performing suction filtration, and drying to obtain the MQ silicone resin coated phase change microcapsule.
Example 5
This example 5 provides a first method for preparing MQ silicone resin-coated phase-change microcapsules, which is different from example 1 in that this example 5 prepares a phase-change microcapsule solution comprising 150g of absolute ethanol, 10g of silicone wax and 10g of methyl MQ silicone resin in parts by mass.
Example 6
This example 6 provides a first method for preparing MQ silicone resin-coated phase-change microcapsules, which is different from example 1 in that the stirring speed of the stirring device in the phase-change microcapsule solution prepared in this example 6 is 1000r/min, and the condensing reflux time is 0.5 h.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. An MQ silicone coated phase change microcapsule, comprising: MQ silicone and phase change materials;
the MQ silicon resin coats the phase change material.
2. The MQ silicone coated phase change microcapsule of claim 1, wherein the MQ silicone comprises any one, two or more of methyl MQ silicone, methyl hydrogen-containing MQ silicone, methyl phenyl MQ silicone, vinyl MQ silicone, phenyl MQ silicone, fluorine-containing MQ silicone.
3. The MQ silicone coated phase change microcapsule of claim 1, wherein the MQ silicone is a methyl MQ silicone.
4. The MQ silicone coated phase change microcapsule according to claim 1, wherein the phase change temperature of the phase change material is 20 to 170 ℃.
5. The MQ silicone coated phase change microcapsule of claim 1, wherein the phase change material comprises any one, two or more of silicone wax, alcohol phase change material, ester phase change material and inorganic phase change material.
6. A preparation method of MQ silicon resin coated phase change microcapsules is characterized by comprising the following steps:
step 1, placing a phase-change material, absolute ethyl alcohol and MQ silicon resin in a condensation reflux device, heating and stirring to obtain a phase-change microcapsule solution;
step 2, slowly dripping water until no precipitate is separated out from the phase change microcapsule solution to obtain a phase change microcapsule suspension;
and 3, carrying out suction filtration on the phase change microcapsule suspension to obtain the phase change microcapsule.
7. The method for preparing MQ silicone coated phase change microcapsules of claim 6, wherein the heating and stirring the phase change material, the absolute ethyl alcohol and the MQ silicone in a condensing reflux device specifically comprises:
and the phase change material, absolute ethyl alcohol and MQ silicon resin are placed in a condensing reflux device for heating, stirring and ultrasonic treatment.
8. The method for preparing MQ silicone coated phase change microcapsules of claim 6, wherein the heating and stirring the phase change material, the absolute ethyl alcohol and the MQ silicone in a condensing reflux device specifically comprises:
placing the phase change material, absolute ethyl alcohol and MQ silicon resin in a condensing reflux device, keeping the heating temperature above 60 ℃, and heating and stirring for 0.5-2h at the stirring speed of 500-1000r/min to obtain the phase change microcapsule solution.
9. The method for preparing MQ silicone coated phase change microcapsules of claim 6, wherein the heating and stirring the phase change material, the absolute ethyl alcohol and the MQ silicone in a condensing reflux device specifically comprises:
according to parts by mass, 10-100 parts of phase change material, 20-150 parts of absolute ethyl alcohol and 10-100 parts of MQ silicon resin are placed in a condensation reflux device for heating and stirring.
10. Use of MQ silicone resin-coated phase-change microcapsules according to any one of claims 1 to 5 or of the preparation process according to any one of claims 6 to 9 for the preparation of MQ silicone resin-coated phase-change microcapsules in the field of thermal management technology.
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