CN109913178A - A kind of preparation method of the modified phase-change microcapsule material of graphene - Google Patents
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Abstract
This application discloses a kind of preparation methods of the modified phase-change microcapsule of graphene, belong to phase-change material technical field.The preparation method of the application is the following steps are included: prepare graphene modified melamine resin prepolymer for melamine, formaldehyde, graphene hybrid reaction；It is emulsified after graphene and emulsifier is added into phase-change material, obtains homogeneous latex emulsion；The homogeneous latex emulsion is mixed with the graphene modified melamine resin prepolymer and carries out home position polymerization reaction, obtains microencapsulation material.Compared with the prior art, wall material of the application using graphene modified melamine resin as microencapsulation material, as core material, the heating conduction for the microencapsulation material being prepared is been significantly enhanced the mixture of phase-change material and graphene, and overall structure and thermal stability are significantly improved.
Description
Technical field
The application belongs to phase-change material technical field, more specifically to a kind of modified phase-change microcapsule of graphene
Preparation method.
Background technique
Phase-change material (PCM-Phase Change Material) refer to it is temperature-resistant in the case where and change state of matter
And the substance of latent heat can be provided, the process for changing physical property is known as phase transition process, and phase-change material can be inhaled in phase transition process
A large amount of heat is received and discharged, temperature control and energy storage can be played the role of.
Phase-change material is in use, it may appear that volume change, it is perishable and leakage the problem of, it is therefore necessary to phase
Become material to be coated.Microcapsule coated is a kind of solid or liquid to be overmolding to core-shell structure particle using film technique
Method, to phase-change material carry out microcapsule coated can play a protective role.
It has been always the heat of research due to its excellent mechanical property, hot property and electric property since graphene self-discovery
Point material.Currently, photoelectric material, biologic medical and in terms of have certain application.The thermal conductivity of grapheme material
Rate can reach 5000W/mK, therefore, can use grapheme material enhance the overall structural strength of phase transformation microencapsulation material and
Heating conduction improves application range and the field of microcapsules of storing energy through phase change.
Publication date is that the Chinese patent 201410006689.9 on April 30th, 2014 discloses a kind of graphene oxide phase transformation
The preparation method of microcapsules, comprising the following steps: graphite oxide is soluble in water, stirring, ultrasound, configuration graphene oxide are molten
Liquid；Phase-change material is added in graphene oxide solution, be higher than phase-change material fusing point at a temperature of heat, make phase-change material
Fusing, stirs to get the stabilization Pickering lotion of graphene oxide coating phase-change materials；It is added into Pickering lotion
Acid, the pH value of regulation system are 2~3, and active force envelopes phase-change material emulsion droplet, shape completely between graphene oxide passes through functional group
At graphene oxide cyst wall；Cooling encystation is precipitated, and obtains graphene oxide phase-change microcapsule.The invention using graphene oxide as
A kind of emulsifier and enhanced thermal conduction wall material, no additional other emulsifiers have obtained the microcapsule phase-change with Thermal conductivity
Material.
For the thermal conductivity for further increasing microcapsules, percolation ratio is reduced, publication date is the Chinese patent on the 26th of August in 2015
201510274641.0 disclose a kind of preparation method of the phase-change microcapsule of the modified wall material of graphene, including graphene oxide is molten
The preparation of liquid, the preparation of the modified wall material performed polymer of graphene, the emulsification of phase-change material and the modified wall material phase-change microcapsule of graphene
Preparation, wherein wall material includes melamine formaldehyde resin, urea-melamine-formaldehyde resin etc., so that phase-change microcapsule
Thermal conductivity and percolation ratio obtain the space for improving to a certain extent, but still having promotion.
Summary of the invention
Aiming at the problem that phase-change material heating conduction declines after microcapsules of the existing technology, the application provides one kind can
The preparation method of the modified phase-change microcapsule of graphene to be used to effectively improve microcapsules heating conduction and overall structural strength.
To solve the above-mentioned problems, technical solution used by the application is as follows:
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
Melamine, formaldehyde, graphene hybrid reaction are prepared graphene modified melamine resin prepolymer by S1；
S2 is emulsified after graphene and emulsifier is added into phase-change material, obtains homogeneous latex emulsion；
The homogeneous latex emulsion is mixed with the graphene modified melamine resin prepolymer and carries out home position polymerization reaction by S3,
Obtain microencapsulation material.
Further, the home position polymerization reaction is by the way of sectional-regulated pH.
Further, the reaction condition of home position polymerization reaction is first to adjust pH to 6~8, is stirred to react 1 at 50~70 DEG C
Then~2h adjusts pH to 4~6,1~2h is stirred to react at 60~80 DEG C, adjust pH after reaction to neutrality.
Further, step S1 specifically: weigh mass ratio be 1:(1~2) melamine and formalin, and add
Enter to account for the graphene and appropriate amount of deionized water of prepolymer gross mass 0.5~2 ‰, pH to 8~9 is adjusted, in 60~90 DEG C of conditions
Under be stirred to react 0.5~1h to get to mass concentration be 20%~40% modified melamine resin prepolymer.
Further, step S2 specifically: the graphene that mass fraction is 0.1~2% is added into phase-change material, obtains
Then mixture is added the emulsifier and suitable quantity of water for accounting for mixture quality score 7~10%, is carried out using high-speed shearing emulsion machine
Emulsification treatment obtains homogeneous latex emulsion.
Further, the graphene is pure graphene, graphene oxide or amino graphene.
Further, the phase-change material is paraffin or butyl stearate.
Further, the emulsifier is cationic emulsifier.
Further, the emulsifier is selected from lauryl ammonium chloride, cetyl trimethylammonium bromide, cetyl
One or more of the pyridinium bromide nymph of a locust, neopelex, polyoxethylene octylphenyl phenol ether -10.
Further, adjust pH using sodium hydroxide solution, potassium hydroxide solution, ammonium hydroxide, triethanolamine, hydrochloric acid, phosphoric acid,
One or more of citric acid, acetic acid.
Compared with the prior art, wall material of the application using graphene modified melamine resin as microencapsulation material, phase transformation material
As core material, the heating conduction for the microencapsulation material being prepared is been significantly enhanced the mixture of material and graphene, whole to tie
Structure and thermal stability are significantly improved, and have broad application prospects in fabric and specific occasion.
Positively charged emulsifier is added in the application in core material, is emulsified using high-speed shearing emulsion machine, so that lotion liquid
It is positively charged to drip surface, graphene dispersing solution is added dropwise, using electrostatic interaction graphene dispersing solution is formed certainly in droplet surface
Package assembly, and then the core material as microencapsulation material make graphene arrange in core material more neat in this way,
It is partial to form planar structure, is conducive to the heating conduction for improving material.
The application when preparing microencapsulation material by the way of sectional-regulated pH, the pH of reaction system to wall material synthesis and
Shaping influence is larger, reacts it has been found that system pH is first adjusted to neutrality left and right, then adjusting pH to acidity, into
The preparation of row microencapsulation material, not only wall material is easily molded, but also the area requirement that pH is adjusted is wide, and zmodem is suitable for industrialization
Using.
Specific embodiment
The application is further described below combined with specific embodiments below.
Embodiment 1
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
1, melamine and the mass fraction that quality is respectively 10g and 10g are weighed as 37% formalin, and is added
The graphene oxide and 50mL deionized water for accounting for prepolymer gross mass 0.5 ‰ adjust pH to 8~9 using sodium hydroxide solution,
At 80 DEG C and have and react 0.5h under magnetic agitation, the modified melamine resin prepolymer that mass concentration is 24.3% is obtained, as wall
Material.
2, phase-change material paraffin is weighed according to the ratio that core wall mass ratio is 1:1.5, and mass fraction is added wherein and is
The emulsifier dodecyl chloride for accounting for core material mass fraction 7% is added as microcapsules core material in 0.1 ‰ graphene in core material
Change ammonium and 300mL deionized water, emulsification treatment is carried out using high-speed shearing emulsion machine, in the emulsified 10min of 10000rpm revolving speed
Obtain homogeneous latex emulsion.
3, homogeneous latex emulsion is added dropwise into modified melamine resin prepolymer, adjusts pH to 8, is stirred to react 2h at 70 DEG C,
Then pH to 5 is adjusted, 1h is stirred to react at 60 DEG C, reaction later-stage utilization triethylamine adjusts pH to neutrality, and reaction was completed, obtains
Microencapsulation material.
4, step 3 gained microencapsulation material is obtained to the modified phase-change microcapsule powder of graphene after washing, drying.
Embodiment 2
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
1, melamine and the mass fraction that quality is respectively 10g and 20g are weighed as 37% formalin, and is added
The graphene oxide and 50mL deionized water for accounting for prepolymer gross mass 1 ‰ adjust pH to 8~9 using sodium hydroxide solution,
60 DEG C and have and react 1h under magnetic agitation, the modified melamine resin prepolymer that mass concentration is 33.1% is obtained, as wall material.
2, phase-change material paraffin is weighed according to the ratio that core wall mass ratio is 1:2, and it is 2 ‰ that mass fraction is added wherein
Graphene as microcapsules core material, be added in core material the neopelex for accounting for core material mass fraction 10% and
300mL deionized water carries out emulsification treatment using high-speed shearing emulsion machine, obtains in the emulsified 15min of 8000rpm revolving speed
Even lotion.
3, emulsion droplets are added in modified melamine resin prepolymer, adjusts pH to 7,1h is stirred to react at 60 DEG C, then
PH to 4 is adjusted, 1h is stirred to react at 60 DEG C, reaction later-stage utilization sodium hydroxide solution adjusts pH to neutrality, and reaction was completed, obtains
To microencapsulation material.
4, step 3 gained microencapsulation material is obtained to the modified phase-change microcapsule powder of graphene after washing, drying.
Embodiment 3
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
1, melamine and the mass fraction that quality is respectively 10g and 14g are weighed as 37% formalin, and is added
The graphene and 50mL deionized water for accounting for prepolymer gross mass 2 ‰ adjust pH to 8~9 using triethylamine, at 80 DEG C and have magnetic
Power stirring is lower to react 0.5h, the modified melamine resin prepolymer that mass concentration is 25.8% is obtained, as wall material.
2, phase-change material butyl stearate is weighed according to the ratio that core wall mass ratio is 1:1, and quality point is added wherein
The cetyl trimethyl for accounting for core material mass fraction 10% is added as microcapsules core material in the graphene that number is 2 ‰ in core material
Ammonium bromide and 300mL deionized water carry out emulsification treatment using high-speed shearing emulsion machine, emulsified in 10000rpm revolving speed
15min obtains homogeneous latex emulsion.
3, emulsion droplets are added in modified melamine resin prepolymer, adjusts pH to 6,2h is stirred to react at 60 DEG C, then
PH to 4 is adjusted, 2h is stirred to react at 70 DEG C, reaction later-stage utilization ammonia spirit adjusts pH to neutrality, and reaction was completed, obtains micro-
Capsule material.
4, step 3 gained microencapsulation material is obtained to the modified phase-change microcapsule powder of graphene after washing, drying.
Embodiment 4
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
1, melamine and the mass fraction that quality is respectively 10g and 12g are weighed as 37% formalin, and is added
The graphene and 50mL deionized water for accounting for prepolymer gross mass 2 ‰ adjust pH to 8~9 using triethylamine, at 80 DEG C and have magnetic
Power stirring is lower to react 0.5h, the modified melamine resin prepolymer that mass concentration is 25.9% is obtained, as wall material.
2, phase-change material butyl stearate is weighed according to the ratio that core wall mass ratio is 1:1, and quality point is added wherein
The neopelex for accounting for core material mass fraction 7% is added as microcapsules core material in the graphene that number is 2 ‰ in core material
With 300mL deionized water, emulsification treatment is carried out using high-speed shearing emulsion machine, is obtained in the emulsified 20min of 8000rpm revolving speed
Even lotion.
3, emulsion droplets are added in modified melamine resin prepolymer, adjust pH to 8, is stirred to react 2h at 50~70 DEG C,
Then pH to 4 is adjusted, 1h is stirred to react at 60 DEG C, reaction later-stage utilization ammonia spirit adjusts pH to neutrality, and reaction was completed, obtains
To microencapsulation material.
4, step 3 gained microencapsulation material is obtained to the modified phase-change microcapsule powder of graphene after washing, drying.
Embodiment 5
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
1, melamine and the mass fraction that quality is respectively 10g and 18g are weighed as 37% formalin, and is added
The graphene and 50mL deionized water for accounting for prepolymer gross mass 0.5 ‰ adjust pH to 8~9 using triethylamine, at 80 DEG C and have
0.5h is reacted under magnetic agitation, the modified melamine resin prepolymer that mass concentration is 31.2% is obtained, as wall material.
2, phase-change material paraffin is weighed according to the ratio that core wall mass ratio is 1:1.5, and mass fraction is added wherein and is
The cetyl pyridinium bromide nymph of a locust for accounting for core material mass fraction 10% is added as microcapsules core material in 1 ‰ graphene in core material
With 300 mL deionized waters, emulsification treatment is carried out using high-speed shearing emulsion machine, is obtained in the emulsified 10min of 10000rpm revolving speed
Homogeneous latex emulsion.
3, emulsion droplets are added in modified melamine resin prepolymer, adjust pH to 7, is stirred to react 2h at 50~70 DEG C,
Then pH to 5 is adjusted, 2h is stirred to react at 80 DEG C, reaction later-stage utilization sodium hydroxide solution adjusts pH to neutrality, terminates anti-
It answers, obtains microencapsulation material.
4, step 3 gained microencapsulation material is obtained to the modified phase-change microcapsule powder of graphene after washing, drying.
Embodiment 6
A kind of preparation method of the modified phase-change microcapsule material of graphene, comprising the following steps:
1, melamine and the mass fraction that quality is respectively 10g and 20g are weighed as 37% formalin, and is added
The graphene and 50mL deionized water for accounting for prepolymer gross mass 2 ‰ adjust pH to 8~9 using triethylamine, at 80 DEG C and have magnetic
Power stirring is lower to react 0.5h, the modified melamine resin prepolymer that mass concentration is 33.1% is obtained, as wall material.
2, phase-change material paraffin is weighed according to the ratio that core wall mass ratio is 1:1.5, and mass fraction is added wherein and is
The neopelex for accounting for core material mass fraction 9% is added as microcapsules core material in 0.5 ‰ graphene in core material
With 300 mL deionized waters, emulsification treatment is carried out using high-speed shearing emulsion machine, is obtained in the emulsified 10min of 10000rpm revolving speed
Homogeneous latex emulsion.
3, emulsion droplets are added in modified melamine resin prepolymer, adjusts pH to 8,1h is stirred to react at 70 DEG C, then
PH to 5 is adjusted, 2h is stirred to react at 80 DEG C, reaction later-stage utilization sodium hydroxide solution adjusts pH to neutrality, and reaction was completed, obtains
To microencapsulation material.
4, step 3 gained microencapsulation material is obtained to the modified phase-change microcapsule powder of graphene after washing, drying.
The preparation-obtained microencapsulation material powder of the above various embodiments and waterborne polyurethane adhesive are mixed, are configured to
Simple microcapsules finishing fluid, is coated uniformly on nylon nonwoven fabrics cloth specimen, 65 DEG C of preliminary dryings, 150 DEG C bake using directly painting method
4min is most washed afterwards, is dried, and is obtained microcapsules and is arranged temperature induced color changing fabric.
Passed through with Japanese KATO company KES-F7-II contact changes in temperature sense tester (THERMOLABO TESTER) test 1h
The heat flow of fabric sample, then with compact tester by sample constant speed pressurize, obtain the thickness of sample, with following formula into
Row calculates, and show that the thermal coefficient of surveyed fabric sample, acquired results are shown in Table 1.
In formula: k-thermal coefficient (W/m DEG C)；
W-heat flow (W)；
D-fabric sample thickness (m)；
A-hot plate area (m2)；
The temperature difference (DEG C) between △ T-upper and lower hot plate.
As shown in Table 1, it compares with the fabric for being not added with the modified phase-change microcapsule of graphene, is arranged by phase-change microcapsule
Its thermal coefficient of fabric becomes larger, and when the concentration of phase-change microcapsule increases to 10% from 0, thermal coefficient k is increased with it, it is seen then that
The addition of phase-change microcapsule can increase the thermal coefficient of fabric, and when dosage reaches 15%, thermal coefficient increases, but improve
Amplitude is little.Fabric containing phase-change microcapsule can play its effect in summer, this is because when ambient temperature increases, phase transformation material
Material can absorb heat, and from it is solid state transformed be liquid, so that fabric is generated the cooling effect of certain time.After tested it is found that containing phase
The Heat Transfer Coefficient of Fabric for becoming microcapsules becomes larger, and illustrates in temperature change, and fabric is easier to absorb heat, i.e. adjusting microenvironment temperature
The ability of degree improves.
The modified phase-change microcapsule material phase transformation situation of the graphene of each embodiment of table 1
Claims (10)
1. a kind of preparation method of the modified phase-change microcapsule material of graphene, which comprises the following steps:
Melamine, formaldehyde, graphene hybrid reaction are prepared graphene modified melamine resin prepolymer by S1；
S2 is emulsified after graphene and emulsifier is added into phase-change material, obtains homogeneous latex emulsion；
The homogeneous latex emulsion is mixed with the graphene modified melamine resin prepolymer and carries out home position polymerization reaction, obtained by S3
Microencapsulation material.
2. preparation method according to claim 1, which is characterized in that the home position polymerization reaction is using sectional-regulated pH's
Mode.
3. preparation method according to claim 1 or 2, which is characterized in that the reaction condition of home position polymerization reaction is first to adjust
PH to 6~8 is saved, 1~2h is stirred to react at 50~70 DEG C, then adjusts pH to 4~6, it is stirred to react 1 at 60~80 DEG C~
2h adjusts pH to neutrality after reaction.
4. preparation method according to claim 1, which is characterized in that step S1 specifically: weigh mass ratio be 1:(1~
2) melamine and formalin, and the graphene and appropriate deionization for accounting for prepolymer gross mass 0.5~2 ‰ is added
Water adjusts pH to 8~9, is stirred to react 0.5~1h under the conditions of 60~90 DEG C to get being 20%~40% to mass concentration
Modified melamine resin prepolymer.
5. preparation method according to claim 1, which is characterized in that step S2 specifically: matter is added into phase-change material
Measure score be 0.1~2% graphene, obtain mixture, then be added account for mixture quality score 7~10% emulsifier and
Suitable quantity of water carries out emulsification treatment using high-speed shearing emulsion machine and obtains homogeneous latex emulsion.
6. preparation method according to claim 1, which is characterized in that the graphene is pure graphene, graphene oxide
Or amino graphene.
7. preparation method according to claim 1, which is characterized in that the phase-change material is paraffin or butyl stearate.
8. preparation method according to claim 1, which is characterized in that the emulsifier is cationic emulsifier.
9. preparation method according to claim 8, which is characterized in that the emulsifier is selected from lauryl ammonium chloride, ten
Six alkyl trimethyl ammonium bromides, the cetyl pyridinium bromide nymph of a locust, neopelex, polyoxethylene octylphenyl phenol ether -10
One or more of.
10. preparation method according to claim 1, which is characterized in that adjust pH and use sodium hydroxide solution, potassium hydroxide
One or more of solution, ammonium hydroxide, triethanolamine, hydrochloric acid, phosphoric acid, citric acid, acetic acid.
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| CN111518522A (en) * | 2020-06-09 | 2020-08-11 | 长沙理工大学 | Preparation method of graphite modified phase-change microcapsule |
| CN111534285A (en) * | 2020-06-01 | 2020-08-14 | 长沙理工大学 | SiO (silicon dioxide)2Preparation method of modified phase-change microcapsule |
| CN112121738A (en) * | 2020-09-28 | 2020-12-25 | 杭州应星新材料有限公司 | Preparation method of functionalized microcapsule and functionalized microcapsule prepared by preparation method |
| CN115536304A (en) * | 2022-09-26 | 2022-12-30 | 浙江智峰科技有限公司 | Preparation process of compound concrete water reducer and concrete water reducer |
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| CN110479194B (en) * | 2019-07-31 | 2021-12-14 | 天津城建大学 | Phase change microcapsule with high mechanical property and high thermal conductivity and preparation method thereof |
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| CN115536304A (en) * | 2022-09-26 | 2022-12-30 | 浙江智峰科技有限公司 | Preparation process of compound concrete water reducer and concrete water reducer |
| CN116004012A (en) * | 2022-12-24 | 2023-04-25 | 北京创盈光电医疗科技有限公司 | Flexible heat storage phase change composite material and preparation method thereof |
| CN116004012B (en) * | 2022-12-24 | 2024-03-22 | 北京创盈光电医疗科技有限公司 | Flexible heat storage phase change composite material and preparation method thereof |
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Application publication date: 20190621 |