CN113249097A - Polyacrylate phase-change microcapsule and preparation method thereof - Google Patents
Polyacrylate phase-change microcapsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyacrylate phase change microcapsule and a preparation method thereof. According to the invention, an organic anti-ultraviolet absorbent is combined with an acrylate monomer through a chemical reaction, an anti-ultraviolet modified polyacrylate is taken as a wall material, a low-melting-point phase-change material is taken as a core material, and the microcapsule with the anti-ultraviolet function and the intelligent temperature control function is prepared through a suspension polymerization method. The preparation method of the polyacrylate phase-change microcapsule is simple, the reaction condition is mild, the prepared phase-change microcapsule has uniform particle size distribution and good thermal stability, can be subjected to high-temperature heat setting treatment, and has good application prospect in the fields of multifunctional summer textiles and outdoor textiles.
Description
Technical Field
The invention belongs to the field of functional microcapsules, and particularly relates to a polyacrylate phase change microcapsule with ultraviolet resistance and intelligent temperature control functions and a preparation method thereof.
Background
Phase change materials are a class of materials that have good energy storage capabilities. During the phase transition process, a large amount of heat can be absorbed or released, the temperature of the heat-absorbing material can be kept approximately constant, and therefore energy storage and release can be achieved, and the heat-absorbing material can be used repeatedly. However, the phase change material is easy to leak in the phase change process and is easy to generate phase separation, so that the application of the phase change material is greatly limited. The microcapsule technology not only well overcomes the defect that the phase-change material is easy to leak, but also increases the heat transfer rate and the specific surface area of the phase-change material due to microencapsulation, so that the phase-change material has a better heat storage and energy storage effect.
In recent years, with the warming of climate and the increasing demand of people for living quality, intelligent textiles and protective articles with automatic temperature regulating function are concerned, and the introduction of phase-change microcapsules into the field of textile materials is an important way to endow the textile materials with intelligent temperature regulating function. The textile containing the phase-change microcapsules can build a transient thermal barrier for a user when the user encounters temperature mutation, and the function of adjusting the sensible heat comfort level of the body is achieved. In addition, the intelligent temperature-adjusting textile based on the phase-change microcapsule technology can provide necessary safety protection for working personnel operating in high-temperature fire field environments such as firemen. Proper ultraviolet radiation can help to generate vitamin D, and can prevent bone diseases such as rickets. Excessive uv exposure can cause damage to the skin, eyes and immune system of the human body. The garment can effectively reduce the radiation of ultraviolet rays to a human body, however, in summer with longer ultraviolet irradiation time and higher ultraviolet intensity, the garment fabric is often lighter and thinner and has poorer ultraviolet ray shielding effect, and in order to effectively improve the ultraviolet ray shielding effect of the garment, an ultraviolet-resistant absorbent needs to be added in the fabric after-finishing process. The phase change microcapsule wall material is modified by the uvioresistant absorbent, so that the microcapsule can be endowed with the effects of intelligent temperature control and uvioresistant, the subsequent processing technological process of the fabric is reduced, and the production cost is reduced.
For the preparation of the uvioresistant phase-change microcapsule, the prior literature reports that the reticular polyurethane phase-change microcapsule is prepared by adopting butyl stearate as a core material and isophorone diisocyanate and glycerol as reaction monomers and adopting an interfacial polymerization method, and nano TiO is adopted2The wall material of the phase change microcapsule is modified to obtain the phase change microcapsule with good heat storage property, photocatalysis property and ultraviolet absorption resistance. (e.g., Gaole. nano TiO)2Preparation and performance study of/reticular polyurethane phase-change microcapsules [ D]The master thesis of Yanshan university, 2020). There are patent documents that phase change microcapsules (such as: CN106833539A and CN108300421A) having photocatalytic properties and uv-resistant effect are prepared by coating phase change material with titanium dioxide, and the uv-resistant property of titanium dioxide is limited because the particle size of the prepared microcapsules is in submicron and micron level. In addition, researchers modify the nano titanium dioxide and then dope the modified nano titanium dioxide into the wall of the microcapsule to obtain the phase change microcapsule with the ultraviolet resistance function (such as Microencapsulated phase change materials with TiO, Zhaojing and the like)2-doped PMMA shell for thermal energy storage and UV-shielding[J].Solar Energy Materials&Solar Cells,2017,168: 62-68.). However, the shielding effect of the nano titanium dioxide on ultraviolet rays in UVA wave bands is weak, and the titanium dioxide alone cannot effectively shield the ultraviolet rays.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of polyacrylate phase change microcapsules, so that the preparation process of the polyacrylate phase change microcapsules is simple, the reaction conditions are mild, and the prepared phase change microcapsules have double functions of ultraviolet resistance and intelligent temperature control.
Therefore, the invention adopts the following technical scheme: a method of preparing a polyacrylate phase change microcapsule, comprising:
step 1), uniformly mixing a phase-change material with a melting point of 18-40 ℃, a polymerized monomer of methyl methacrylate, methacrylic acid, an organic anti-ultraviolet absorbent containing unsaturated double bonds, a cross-linking agent and a proper amount of initiator of azobisisobutyronitrile to form an oil phase, adding the oil phase into a water phase containing an emulsifier, and emulsifying to obtain an oil/water emulsion;
and 2), heating the oil/water emulsion to 80-85 ℃, and carrying out polymerization reaction for 4-6h under the protection of nitrogen to obtain the polyacrylate phase change microcapsule suspension.
The polyacrylate phase-change microcapsule is prepared by a suspension polymerization method by taking a phase-change material with a low melting point as a capsule core and taking polyacrylate modified by an ultraviolet-resistant absorbent as a capsule wall. According to the invention, an organic anti-ultraviolet absorbent containing unsaturated double bonds is polymerized with an acrylate monomer to obtain an organic anti-ultraviolet modified polyacrylate wall material, and the organic anti-ultraviolet absorbent is fixed in the capsule wall through double bond reaction, so that the excellent ultraviolet shielding function of the capsule wall of the microcapsule is given. When the external temperature changes, the coated phase-change material absorbs or releases a large amount of heat through phase transition, so that the microcapsule has a good temperature control effect.
Further, in the step 1), the emulsifier is 5-15 wt% of polyvinyl alcohol aqueous solution, and the using amount of the emulsifier is 25-35% of the total mass of the oil phase.
Further, in the step 1), the phase change material is any one or a mixture of n-hexadecane, n-octadecane, n-eicosane, n-dodecanol, n-tetradecanol, methyl palmitate, ethyl palmitate, butyl stearate and methyl myristate.
Further, in the step 1), the organic anti-ultraviolet absorbent containing an unsaturated double bond is any one or a mixture of 2-hydroxy-4-acryloyloxy benzophenone, 2-hydroxy-4- (methacryloyloxy) benzophenone, 2-hydroxy-4-acryloyloxy ethoxy benzophenone, 2-hydroxy-4- [2 '-hydroxy-3' - (methacryloyloxypropyl) ] benzophenone, and 2-hydroxy-4- [2 '-hydroxy-3' - (acryloyloxypropyl) ] benzophenone.
Further, in the step 1), the cross-linking agent is any one or a mixture of dipropylene glycol diacrylate, trimethylolpropane triacrylate and pentaerythritol tetraacrylate.
Further, in the step 1), the mass of the azobisisobutyronitrile accounts for 1-3% of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the crosslinking agent.
Further, in the step 1), the mass of the cross-linking agent accounts for 25-35% of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the cross-linking agent.
Further, in the step 1), the ratio of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the cross-linking agent to the total mass of the phase-change material is 1: 1-1: 4.
Further, in the step 1), the mass of the organic anti-ultraviolet absorbent accounts for 10-20% of the total mass of the methyl methacrylate, the methacrylic acid, the anti-ultraviolet absorbent and the crosslinking agent.
Further, in the step 1), the specific conditions of emulsification are as follows: emulsifying for 15-25min at the speed of 2500-3500r/min by using a high-speed shearing emulsifying machine.
The invention also aims to provide the polyacrylate phase-change microcapsule prepared by the preparation method, which takes the phase-change material as a capsule core and takes the polyacrylate modified by the organic ultraviolet-resistant absorbent as a capsule wall, wherein the capsule wall has an ultraviolet-resistant function, and the capsule core has an intelligent temperature control function.
The invention has the following beneficial effects:
(1) the phase-change material is coated by the capsule wall material with the ultraviolet resistance function, so that the composite microcapsule with the ultraviolet resistance function and the intelligent temperature control function is prepared, and the composite microcapsule has important application value in the fields of multifunctional summer textiles and outdoor products.
(2) According to the invention, the organic ultraviolet-resistant absorbent is fixed in the microcapsule wall through double bond polymerization reaction, so that the microcapsule has more excellent ultraviolet-resistant effect.
(3) The invention respectively endows the wall material and the core material with ultraviolet resistance and intelligent temperature control functions, realizes the dual functions of the microcapsule, and simultaneously does not influence the effective carrying capacity of the phase-change material of the core material.
(4) The preparation method is simple and easy to operate, and the prepared phase change microcapsule has the advantages of regular appearance, uniform particle size distribution, high thermal stability and high enthalpy value.
Detailed Description
The following detailed description is provided to further explain the embodiments of the present invention in order to make the technical solutions of the present invention easier to understand and master. It is to be understood that the specific embodiments described herein are merely illustrative of some, but not all, embodiments of the invention and that other embodiments may be devised by those skilled in the art without the use of the inventive faculty and the scope of the invention is to be protected.
Example 1
Firstly, 50g of octadecane, 27g of methyl methacrylate, 5.5g of methacrylic acid, 5g of 2-hydroxy-4-acryloxybenzophenone, 14g of dipropylene glycol diacrylate, 3.5g of trimethylolpropane triacrylate and 1.5g of azobisisobutyronitrile are uniformly mixed to form an oil phase, 35.5g of 10% of polyvinyl alcohol aqueous solution is added into 95g of deionized water to form an aqueous phase, the oil phase is added into the aqueous phase, and a high-speed shearing emulsifying machine is utilized to emulsify for 20min at the speed of 3000r/min to obtain uniform oil/water emulsion.
And then transferring the emulsion into a 500ml four-neck flask, heating to 80-85 ℃, and carrying out polymerization reaction for 5h under the protection of nitrogen to obtain the uvioresistant phase change microcapsule suspension. The solid content of the obtained microcapsule suspension is 47%, the particle size of the microcapsule is 5-10um, and the heat resistance stability is higher than 300 ℃.
The thermal properties of the microcapsules were tested using a differential scanning calorimeter (Q200, TA USA) (see Table 1 for specific data). The obtained difunctional microcapsules are applied to the all-cotton knitted fabric (the gram weight is 150 g/m) by adopting a padding method2) The microcapsule suspension was used in an amount of 200g/L, and the UV resistance of the fabric before and after finishing was measured using a UV transmittance analyzer (UV-2000F, Labsphere, USA) (see Table 2 for specific data))。
Example 2
Firstly, 50g of octadecane, 9.3g of methyl methacrylate, 2g of methacrylic acid, 5g of 2-hydroxy-4- [2 '-hydroxy-3' - (acryloyloxypropyl) ] benzophenone, 8.7g of dipropylene glycol diacrylate and 0.5g of azobisisobutyronitrile are uniformly mixed to form an oil phase, 20g of 10% of polyvinyl alcohol aqueous solution is added into 70g of deionized water to form an aqueous phase, the oil phase is added into the aqueous phase, and a high-speed shearing emulsifying machine is utilized to emulsify for 20min at the speed of 3000r/min to obtain uniform oil/water emulsion.
And then transferring the emulsion into a 500ml four-neck flask, heating to 80-85 ℃, and carrying out polymerization reaction for 5h under the protection of nitrogen to obtain the uvioresistant phase change microcapsule suspension. The solid content of the obtained microcapsule suspension is 47%, the particle size of the microcapsule is 5-10um, and the heat resistance stability is higher than 300 ℃.
The thermal properties of the microcapsules were tested using a differential scanning calorimeter (Q200, TA USA) (see Table 1 for specific data). The obtained difunctional microcapsules are applied to the all-cotton knitted fabric (the gram weight is 150 g/m) by adopting a padding method2) The amount of the microcapsule suspension was 200g/L, and the UV resistance of the fabric before and after finishing was measured using a UV transmittance analyzer (UV-2000F, Labsphere, USA) (see Table 2 for specific data).
Example 3
Firstly, 50g of methyl palmitate, 10.5g of methyl methacrylate, 2g of methacrylic acid, 5g of 2-hydroxy-4- [2 '-hydroxy-3' - (acryloyloxypropyl) ] benzophenone, 7.5g of trimethylolpropane triacrylate and 0.5g of azobisisobutyronitrile are uniformly mixed to form an oil phase, 20g of 10% of polyvinyl alcohol aqueous solution is added into 70g of deionized water to form an aqueous phase, the oil phase is added into the aqueous phase, and a high-speed shearing emulsifying machine is utilized to emulsify for 20min at the speed of 3000r/min to obtain uniform oil/water emulsion.
And then transferring the emulsion into a 500ml four-neck flask, heating to 80-85 ℃, and carrying out polymerization reaction for 5h under the protection of nitrogen to obtain the uvioresistant phase change microcapsule suspension. The solid content of the obtained microcapsule suspension is 47%, the particle size of the microcapsule is 5-10um, and the heat resistance stability is higher than 300 ℃.
The thermal properties of the microcapsules were tested using a differential scanning calorimeter (Q200, TA USA) (see Table 1 for specific data). The obtained difunctional microcapsules are applied to the all-cotton knitted fabric (the gram weight is 150 g/m) by adopting a padding method2) The amount of the microcapsule suspension was 200g/L, and the UV resistance of the fabric before and after finishing was measured using a UV transmittance analyzer (UV-2000F, Labsphere, USA) (see Table 2 for specific data).
Example 4
Firstly, 50g of octadecane, 11.7g of methyl methacrylate, 2g of methacrylic acid, 5g of 2-hydroxy-4- [2 '-hydroxy-3' - (acryloyloxypropyl) ] benzophenone, 6.3g of pentaerythritol tetraacrylate and 0.5g of azobisisobutyronitrile are uniformly mixed to form an oil phase, 20g of 10% of polyvinyl alcohol aqueous solution is added into 70g of deionized water to form an aqueous phase, the oil phase is added into the aqueous phase, and a high-speed shearing emulsifying machine is utilized to emulsify for 20min at the speed of 3000r/min to obtain uniform oil/water emulsion.
And then transferring the emulsion into a 500ml four-neck flask, heating to 80-85 ℃, and carrying out polymerization reaction for 5h under the protection of nitrogen to obtain the uvioresistant phase change microcapsule suspension. The solid content of the obtained microcapsule suspension is 47%, the particle size of the microcapsule is 5-10um, and the heat resistance stability is higher than 300 ℃.
The thermal properties of the microcapsules were tested using a differential scanning calorimeter (Q200, TA USA) (see Table 1 for specific data). The obtained difunctional microcapsules are applied to the all-cotton knitted fabric (the gram weight is 150 g/m) by adopting a padding method2) The amount of the microcapsule suspension was 200g/L, and the UV resistance of the fabric before and after finishing was measured using a UV transmittance analyzer (UV-2000F, Labsphere, USA) (see Table 2 for specific data).
Example 5
Firstly, 50g of octadecane, 7g of methyl methacrylate, 1.5g of methacrylic acid, 3g of 2-hydroxy-4-acryloyloxybenzophenone, 4g of dipropylene glycol diacrylate, 1g of trimethylolpropane triacrylate and 0.17g of azobisisobutyronitrile are uniformly mixed to form an oil phase, 20g of 10% of polyvinyl alcohol aqueous solution is added into 60g of deionized water to form an aqueous phase, the oil phase is added into the aqueous phase, and a high-speed shearing emulsifying machine is utilized to emulsify for 20min at the speed of 3000r/min to obtain uniform oil/water emulsion.
And then transferring the emulsion into a 500ml four-neck flask, heating to 80-85 ℃, and carrying out polymerization reaction for 5h under the protection of nitrogen to obtain the uvioresistant phase change microcapsule suspension. The solid content of the obtained microcapsule suspension is 47%, the particle size of the microcapsule is 5-10um, and the heat resistance stability is higher than 300 ℃.
The thermal properties of the microcapsules were tested using a differential scanning calorimeter (Q200, TA USA) (see Table 1 for specific data). The obtained difunctional microcapsules are applied to the all-cotton knitted fabric (the gram weight is 150 g/m) by adopting a padding method2) The amount of the microcapsule suspension was 200g/L, and the UV resistance of the fabric before and after finishing was measured using a UV transmittance analyzer (UV-2000F, Labsphere, USA) (see Table 2 for specific data).
Example 6
Firstly, 50g of butyl stearate, 5g of methyl methacrylate, 1.5g of methacrylic acid, 2.5g of 2-hydroxy-4-acryloyloxyethoxy benzophenone, 2.5g of dipropylene glycol diacrylate, 1g of trimethylolpropane triacrylate and 0.25g of azobisisobutyronitrile are uniformly mixed to form an oil phase, 15.7g of 10% of polyvinyl alcohol aqueous solution is added into 60g of deionized water to form an aqueous phase, the oil phase is added into the aqueous phase, and a high-speed shearing emulsifying machine is used for emulsifying for 20min at the speed of 3000r/min to obtain uniform oil/water emulsion.
And then transferring the emulsion into a 500ml four-neck flask, heating to 80-85 ℃, and carrying out polymerization reaction for 5h under the protection of nitrogen to obtain the uvioresistant phase change microcapsule suspension. The solid content of the obtained microcapsule suspension is 46%, the particle size of the microcapsule is 5-10um, and the heat resistance stability is higher than 250 ℃.
The thermal properties of the microcapsules were tested using a differential scanning calorimeter (Q200, TA USA) (see Table 1 for specific data). The obtained difunctional microcapsules are applied to the all-cotton knitted fabric (the gram weight is 150 g/m) by adopting a padding method2) The amount of the microcapsule suspension was 200g/L, and the UV resistance of the fabric before and after finishing was measured using a UV transmittance analyzer (UV-2000F, Labsphere, USA) (see Table for specific data)2)。
TABLE 1 thermal Performance data for the bifunctional phase-change microcapsules of the different examples
| Numbering | Enthalpy (J/g) | Melting Point (. degree.C.) |
| Example 1 | 109.2 | 35.0 |
| Example 2 | 144.7 | 31.1 |
| Example 3 | 143.5 | 32.7 |
| Example 4 | 144.2 | 28.8 |
| Example 5 | 160.3 | 30.9 |
| Example 6 | 176.1 | 31.7 |
As can be seen from Table 1, the phase-change micro-gels prepared in examples 1-6 all have higher enthalpy values, which indicates that they have better heat storage performance, and the enthalpy values of the microcapsules are obviously increased along with the increase of the core-wall ratio.
TABLE 2 ultraviolet resistance of cotton knitted fabrics finished with the bifunctional phase-change microcapsule emulsion in different examples
| Numbering | UPF | T(UVA)AV(％) | T(UVB)AV(％) |
| All-cotton knitted fabric | 29.30 | 14.21 | 12.4 |
| Example 1 | 44.72 | 4.89 | 1.2 |
| Example 2 | 56.86 | 4.05 | 0.4 |
| Example 3 | 54.93 | 4.12 | 1.0 |
| Example 4 | 57.28 | 4.11 | 0.3 |
| Example 5 | 47.65 | 4.56 | 0.9 |
| Example 6 | 47.40 | 4.62 | 1.1 |
According to GB/T18830-2009 evaluation of ultraviolet resistance of textiles, UPF of a sample>30, and T (UVA)AV<At 5%, it can be called "UV-resistant product". As can be seen from Table 2, the untreated all-cotton knitted fabric does not meet the performance requirements of the UV resistant product. The all-cotton knitted fabric finished by the microcapsules in the embodiments 1 to 6 can meet the performance requirements of the ultraviolet-resistant product, and the ultraviolet resistance of the finished all-cotton knitted fabric is enhanced along with the increase of the dosage of the ultraviolet-resistant absorbent in the system.
Claims (10)
1. A preparation method of polyacrylate phase change microcapsules is characterized by comprising the following steps:
step 1), uniformly mixing a phase-change material with a melting point of 18-40 ℃, a polymerized monomer of methyl methacrylate, methacrylic acid, an organic anti-ultraviolet absorbent containing unsaturated double bonds, a cross-linking agent and a proper amount of initiator of azobisisobutyronitrile to form an oil phase, adding the oil phase into a water phase containing an emulsifier, and emulsifying to obtain an oil/water emulsion;
and 2), heating the oil/water emulsion to 80-85 ℃, and carrying out polymerization reaction for 4-6h under the protection of nitrogen to obtain the polyacrylate phase change microcapsule suspension.
2. The preparation method according to claim 1, wherein in the step 1), the emulsifier is 5-15 wt% of polyvinyl alcohol aqueous solution, and the amount of the emulsifier is 25-35% of the total mass of the oil phase.
3. The preparation method according to claim 1, wherein in the step 1), the phase change material is any one or a mixture of n-hexadecane, n-octadecane, n-eicosane, n-dodecanol, n-tetradecanol, methyl palmitate, ethyl palmitate, butyl stearate and methyl myristate.
4. The method of claim 1, wherein the organic anti-uv absorber containing unsaturated double bond in step 1) is any one or more selected from 2-hydroxy-4-acryloxy benzophenone, 2-hydroxy-4- (methacryloxy) benzophenone, 2-hydroxy-4-acryloxy ethoxy benzophenone, 2-hydroxy-4- [2 '-hydroxy-3' - (methacryloxypropyl) ] benzophenone, and 2-hydroxy-4- [2 '-hydroxy-3' - (acryloxypropyl) ] benzophenone.
5. The method for preparing the polyurethane foam according to claim 1, wherein in the step 1), the crosslinking agent is any one or a mixture of dipropylene glycol diacrylate, trimethylolpropane triacrylate and pentaerythritol tetraacrylate.
6. The preparation method according to claim 1, wherein in the step 1), the mass of the azobisisobutyronitrile accounts for 1-3% of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the crosslinking agent.
7. The preparation method according to claim 1, wherein in the step 1), the mass of the crosslinking agent accounts for 25-35% of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the crosslinking agent.
8. The preparation method according to claim 1, wherein in the step 1), the ratio of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the crosslinking agent to the total mass of the phase-change material is 1:1 to 1: 4.
9. The preparation method according to claim 1, wherein in the step 1), the mass of the organic anti-ultraviolet absorbent accounts for 10-20% of the total mass of the methyl methacrylate, the methacrylic acid, the organic anti-ultraviolet absorbent and the crosslinking agent.
10. The polyacrylate phase-change microcapsule prepared by the preparation method of any one of claims 1-9, which takes the phase-change material as a capsule core and takes polyacrylate modified by an organic ultraviolet-resistant absorbent as a capsule wall, wherein the capsule wall has an ultraviolet-resistant function, and the capsule core has an intelligent temperature control function.
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