CN111518518A - Multi-wall graphene oxide phase-change microcapsule material and preparation method thereof - Google Patents
Multi-wall graphene oxide phase-change microcapsule material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a multi-wall graphene oxide phase-change microcapsule material and a preparation method thereof, and the multi-wall graphene oxide phase-change microcapsule material comprises 8-15 parts of long-chain n-alkane, 5-12 parts of ethyl orthosilicate, 3-6 parts of methacryloxypropyl tris (trimethylsiloxy) silane, 2-5 parts of hexadecyl trimethylamine bromide, 130 parts of anhydrous ethanol 110-. The invention has the beneficial effects that: the yield is up to over 86 percent; the phase change latent heat is high, the thermal stability is high, and the phase change latent heat is almost unchanged after high-temperature circulation at 500 ℃; the superheat temperature range is small, only 1.1 ℃. The phase change microcapsule prepared by the invention can be widely applied to the fields of fibers, cloth and clothes, fine chemical industry with strong heat exchange requirements and the like.
Description
Technical Field
The invention relates to a multi-wall graphene oxide phase-change microcapsule material and a preparation method thereof, belonging to the field of functional materials.
Background
Since the middle of the twentieth century, the demand and consumption of energy in countries around the world have increased year by year, and therefore, how to fully utilize energy has become an important factor for the development of national economy.
In the last 80 th century, a new technology based on Phase Change Materials (PCM) is provided for protecting astronauts and equipment from being influenced by changes of outer space temperature environment. The research opens a new idea of applying phase-change materials as representative heat storage and temperature regulation materials. A phase change material is a substance that can absorb or release heat from the environment by virtue of its self-reversible phase change properties over a range of temperatures. The phase change process of the phase change material is a reversible reaction and can be repeatedly used, so that the waste of resources can not be caused. The phase-change material is combined with the textile by a certain method, so that the protective material with the functions of heat storage and temperature regulation can be prepared. The material can automatically adjust the internal temperature according to the change of the external environment temperature, reduce the discomfort caused by the change of the environment temperature, and when the external environment temperature is reduced, the phase-change material can release the heat stored before, thereby realizing the function of keeping warm. When the temperature of the external environment rises, the phase-change material can absorb and store heat, and the function of heat storage is realized. The phase-change material is used as a new-generation environment-friendly energy-saving material, can absorb or release heat from the environment through phase change, meets the requirements of energy storage and temperature regulation, and has important research significance for reasonable utilization of energy. The phase-change material is applied to building materials to be made into energy-saving wallboards, floors, doors and windows, glass and the like, can effectively utilize solar energy and waste heat in buildings, and has wide application prospect. However, the phase-change material has disadvantages, such as leakage of liquid phase-change material during phase change, waste of resources and environmental pollution.
In order to overcome the defects of the existing phase change material, the invention discloses a multi-wall graphene oxide phase change microcapsule taking n-alkane as a phase change material (core), rGO as an inner core and silicon dioxide as an outer shell and a formula thereof. The yield of the phase change microcapsule prepared by the method is up to more than 81 percent; the phase change latent heat is high, the phase change temperature range is 16-32 ℃ according to the type of the selected long-chain n-alkane, and the phase change latent heat reaches 234.3-250.7Jg-1(ii) a The heat conductivity and the sealing performance are good, the heat conductivity coefficient is 0.1521W/mK-0.1739W/mK, the melting permeability after being processed by a pressure sheet is only 0.3% -1.0%, compared with a pure alkane phase change microcapsule, the heat conductivity coefficient is improved by 57.33% -62.83%, the permeability is reduced by 14.2% -19.8%, the thermal stability is high, and the latent heat of phase change is almost unchanged after high-temperature circulation at 400 ℃; the superheat temperature range is small, only 1.1 ℃. The phase-change microcapsule prepared by the invention can be widely applied to fibers, cloth and clothes and fine chemical industry with strong heat exchange requirementsAnd the like.
Disclosure of Invention
Based on the problems, the invention provides a multi-wall graphene oxide phase-change microcapsule and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the raw material composition of the multi-wall graphene oxide phase-change microcapsule comprises the following raw materials in parts by weight: 8-15 parts of long-chain n-alkane, 5-12 parts of ethyl orthosilicate, 3-6 parts of methacryloxypropyl tri (trimethylsiloxy) silane, 2-5 parts of cetyltrimethylammonium bromide (CTAB), 130 parts of anhydrous ethanol, 300 parts of deionized water 250-containing organic silicon, 8-12 parts of ammonia water, 0.03-0.1 part of reduced graphene oxide (rGO), 0.3-1 part of surfactant and 0.3-1 part of emulsifier.
Further, the long-chain n-alkanes include n-hexadecane, n-octadecane, n-eicosane and the like.
Further, the concentration of ammonia water was 25 wt%.
Further, the emulsifier is one or more of ethoxylated propoxylated fatty alcohol, monoglyceride and lauric acid monoglyceride, or can be selected according to actual requirements, and is not particularly required.
Further, the surfactant is polyvinylpyrrolidone.
A multi-wall graphene oxide phase-change microcapsule material is prepared by the following steps:
(1) firstly, adding rGO powder, a surfactant and deionized water into a container, mixing, oscillating for 12 hours by an ultrasonic oscillation instrument (40kHz), then magnetically stirring for 80 minutes (600 revolutions per minute), adding long-chain n-alkane into the container, continuously magnetically stirring for 80 minutes (600 revolutions per minute), and carrying out water bath emulsification reaction for 40 minutes at normal temperature;
(2) adding tetraethoxysilane and methacryloxypropyl tris (trimethylsiloxy) silane into the container in the step (1), and magnetically stirring (300 revolutions per minute) for 60 minutes until the materials are uniformly mixed to obtain a dispersion solution. Adding hexadecyl trimethylamine bromide and absolute ethyl alcohol into the dispersion solution, keeping stirring for 10 minutes, adding an emulsifying agent, increasing the stirring speed to 800 rpm, and keeping for 5 minutes;
(3) then keeping the temperature of the mixed solution at 35 ℃, adding ammonia water to initiate interfacial cohydrolysis and co-condensation reaction, keeping the stirring speed at 300 r/min for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the multi-wall phase change microcapsule;
the multi-wall phase change microcapsule obtained by the invention has the structure that the phase change microcapsule with inner and outer walls sequentially comprises the following components from inside to outside: the organic phase-change core material is provided with graphene oxide on the inner wall and silicon dioxide on the outer wall. In the double-layer wall structure, the graphene oxide is used as the inner wall and is closer to the phase change core material, so that the graphene oxide can exert the effect for a long time, and the graphene oxide is not compounded with the outer wall, so that the original performance of the outer wall is not influenced, and the graphene oxide has better compatibility and cyclability.
The invention has the beneficial effects that: (1) the yield is up to over 86 percent; (2) the phase change latent heat is high, the phase change temperature range is 16-32 ℃ according to the type of the selected long-chain n-alkane, and the phase change latent heat reaches 234.3-250.7Jg-1(ii) a (3) The heat conductivity and the sealing performance are good, the heat conductivity coefficient is 0.1784W/mK-0.1997W/mK, and the melt permeability is only 0.3% -1.0% after the pressure sheet treatment; (4) the overheating temperature range is small and is only 1.1 ℃; (5) the phase change microcapsule system with the double-wall structure has excellent design and better optimizes the overall thermodynamic performance. The fabric has wide application prospect, is particularly suitable for fibers, cloth, clothes and the like, and solves the problems of the reduction of the comfortable sensation of a human body caused by temperature changes in winter and summer.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic representation of a preparation scheme of the present invention;
FIG. 2 is a scanning electron micrograph of phase change microcapsules prepared according to example 2 of the present invention.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
Example 1
(1) Adding 0.05g of reduced graphene oxide, 0.3g of polyvinylpyrrolidone and 250g of deionized water into a container, mixing, oscillating for 12 hours by an ultrasonic oscillator, stirring to realize uniform mixing (600 revolutions per minute), stirring for 80 minutes, adding 10g of n-hexadecane into the container, magnetically stirring (600 revolutions per minute) for 80 minutes, and carrying out water bath emulsification reaction for 40 minutes at normal temperature to obtain a uniform dispersion liquid
(2) 12g of ethyl orthosilicate and 6g of methacryloxypropyl tris (trimethylsiloxy) silane were added to the vessel from step (1) and mixed, stirred uniformly (300 revolutions per minute) and stirred for 60 minutes. Then, 3g of cetyltrimethylammonium bromide and 110g of anhydrous ethanol were added, stirring was maintained for 10 minutes, 0.3g of an emulsifier (ethoxylated propoxylated-C8-10-fatty alcohol) was added and the stirring rate was increased to 800 rpm for 5 minutes, to give a mixed solution.
(3) And then keeping the temperature of the mixed solution at 35 ℃, adding 8g of ammonia water to initiate interfacial cohydrolysis and cocondensation reaction, keeping the stirring speed at 300 revolutions per minute for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the phase-change microcapsule.
Example 2
(1) Adding 0.05g of reduced graphene oxide, 0.3g of polyvinylpyrrolidone and 280g of deionized water into a container, mixing, oscillating for 12 hours by an ultrasonic oscillator, stirring to realize uniform mixing (600 revolutions per minute), stirring for 80 minutes, adding 10g of n-hexadecane into the container, magnetically stirring (600 revolutions per minute) for 80 minutes, and carrying out water bath emulsification reaction for 40 minutes at normal temperature to obtain a uniform dispersion liquid.
(2) Then 10g of n-octadecane, 10g of ethyl orthosilicate and 5g of methacryloxypropyl tris (trimethylsiloxy) silane are added into the container in the step (1) and mixed, and the mixture is uniformly mixed (300 revolutions per minute) by stirring and stirred for 60 minutes. Then, 3.5g of cetyltrimethylammonium bromide and 120g of anhydrous ethanol were added, stirring was maintained for 10 minutes, 0.8g of an emulsifier (ethoxylated propoxylated-C8-10-fatty alcohol) was added and the stirring rate was increased to 800 rpm for 5 minutes, to obtain a mixed solution.
(3) And then keeping the temperature of the mixed solution at 35 ℃, adding 10g of ammonia water to initiate interfacial cohydrolysis and cocondensation reaction, keeping the stirring speed at 300 revolutions per minute for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the phase-change microcapsule.
Example 3
(1) Adding 0.05g of reduced graphene oxide, 0.3g of polyvinylpyrrolidone and 280g of deionized water into a container, mixing, oscillating for 12 hours by an ultrasonic oscillator, stirring to realize uniform mixing (600 revolutions per minute), stirring for 80 minutes, adding 10g of n-hexadecane into the container, magnetically stirring (600 revolutions per minute) for 80 minutes, and carrying out water bath emulsification reaction for 40 minutes at normal temperature to obtain a uniform dispersion liquid.
(2) Then 8g of n-octadecane, 12g of ethyl orthosilicate and 3g of methacryloxypropyl tris (trimethylsiloxy) silane are added into the container in the step (1) and mixed, and the mixture is uniformly mixed (300 revolutions per minute) by stirring and stirred for 60 minutes. Then 5g of cetyltrimethylammonium bromide and 110g of anhydrous ethanol were added, stirring was maintained for 10 minutes, 0.3g of an emulsifier (ethoxylated propoxylated-C8-10-fatty alcohol) was added and the stirring rate was increased to 800 rpm for 5 minutes, to obtain a mixed solution.
(3) And then keeping the temperature of the mixed solution at 35 ℃, adding 12g of ammonia water to initiate interfacial cohydrolysis and cocondensation reaction, keeping the stirring speed at 300 revolutions per minute for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the phase-change microcapsule.
Example 4
(1) Adding 0.05g of reduced graphene oxide, 0.3g of polyvinylpyrrolidone and 270g of deionized water into a container, mixing, oscillating for 12 hours by an ultrasonic oscillator, stirring to achieve uniform mixing (600 revolutions per minute), stirring for 80 minutes, adding 10g of n-hexadecane into the container, magnetically stirring (600 revolutions per minute) for 80 minutes, and carrying out water bath emulsification reaction for 40 minutes at normal temperature to obtain a uniform dispersion liquid.
(2) Then 15g of n-hexadecane, 5g of ethyl orthosilicate and 6g of methacryloxypropyl tris (trimethylsiloxy) silane are added into the container in the step (1) and mixed, and the mixture is uniformly mixed (300 revolutions per minute) by stirring and stirred for 60 minutes. Then 6g of cetyltrimethylammonium bromide and 130g of anhydrous ethanol were added, stirring was maintained for 10 minutes, 1g of an emulsifier (ethoxylated propoxylated-C8-10-fatty alcohol) was added and the stirring rate was increased to 800 rpm for 5 minutes, to obtain a mixed solution.
(3) And then keeping the temperature of the mixed solution at 35 ℃, adding 10g of ammonia water to initiate interfacial cohydrolysis and cocondensation reaction, keeping the stirring speed at 300 revolutions per minute for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the phase-change microcapsule.
Comparative example 1
Comparative example 1 is different from example 1 in that: and (3) not adding graphene oxide to obtain the phase change microcapsule only taking silicon dioxide as a shell.
10g of n-hexadecane, 12g of ethyl orthosilicate and 6g of methacryloxypropyltris (trimethylsiloxyalkyl) silane were added to a vessel and mixed, and the mixture was stirred uniformly (300 revolutions per minute) for 60 minutes. Then 3g of cetyltrimethylammonium bromide and 110g of absolute ethanol are added, stirring is maintained for 10 minutes, 0.3g of emulsifier (ethoxylated propoxylated fatty alcohol) is added and the stirring rate is increased to 800 revolutions per minute for 5 minutes. And then keeping the temperature of the mixed solution at 35 ℃, adding 8g of ammonia water to initiate interfacial cohydrolysis and cocondensation reaction, keeping the stirring speed at 300 revolutions per minute for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the phase-change microcapsule.
Comparative example 2
Compared with the organic phase change microcapsule coated by the graphene oxide doped silica inorganic wall material prepared by CN 201710613151.8.
In the method of comparative example 2, the obtained single-layer phase-change microcapsule structure achieves improvement of the overall thermal performance by doping modification of graphene oxide to the wall material, but with the increase of the number of use times, due to the influence of the working environment, a certain loss is generated on the wall shell structure, the effect of graphene oxide in the wall material is further influenced, and the modified silicon dioxide wall material is weakened in the original strength and original performance, so that the economical efficiency is poor.
The results of the performance test of the phase-change microcapsules prepared in the above examples are shown in the following table:
TABLE 1
The yield, namely the encapsulation rate of the phase change microcapsule in table 1 is calculated by calculating the contents of the surface phase change core material and the total phase change core material in the microcapsule, and the encapsulation rate is finally obtained;
the detection of the high temperature resistance stability is to judge the highest temperature resistance by calculating the weight loss rate through gradient heating of a TG thermogravimetric analyzer.
In Table 1, the measurement was carried out by a known method.
The overheating phenomenon is the condition that the microcapsule is unevenly heated and the phase change of the core material does not occur or only partially occurs when the phase change temperature is reached due to the influence of the internal heat conduction speed in the rapid heating process of the microcapsule working environment. The difference value of the actual delayed phase-change temperature and the theoretical phase-change temperature is the overheat temperature of the phase-change microcapsule, and the difference value is obtained by one-step difference calculation. The smaller the overheating temperature is, the better the manufacturing process of the microcapsule is, and the uniform heating is, and if the overheating temperature is too high, the nonuniform preparation of the microcapsule component is indicated, so that the accurate working temperature cannot be obtained, and the micro control effect is not favorably exerted.
The table shows that the phase change microcapsule has excellent performances, completely meets the relevant national standards, and is energy-saving and environment-friendly.
In light of the foregoing description of the preferred embodiments of the present invention, it is to be understood that various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (5)
1. A multi-wall graphene oxide phase-change microcapsule material is characterized in that: the composite material comprises the following raw materials in parts by weight: 8-15 parts of long-chain n-alkane, 5-12 parts of ethyl orthosilicate, 3-6 parts of methacryloxypropyl tris (trimethylsiloxy) silane, 2-5 parts of hexadecyl trimethylamine bromide, 130 parts of anhydrous ethanol, 300 parts of deionized water, 8-12 parts of ammonia water, 0.03-0.1 part of reduced graphene oxide (rGO), 0.3-1 part of surfactant and 0.3-1 part of emulsifier.
2. The multi-walled graphene oxide phase change microcapsule material according to claim 1, wherein the long-chain n-alkane comprises one or more of n-hexadecane, n-octadecane or n-eicosane.
3. The multi-walled graphene oxide phase change microcapsule material according to claim 1, wherein the emulsifier is one or more of ethoxylated propoxylated fatty alcohol, monoglyceride and monoglyceride laurate.
4. The multi-walled graphene oxide phase change microcapsule material according to claim 1, wherein: the surfactant is polyvinylpyrrolidone.
5. The preparation method of the multi-walled graphene oxide phase-change microcapsule material according to any one of claims 1 to 4, which comprises the following steps:
(1) adding reduced graphene oxide powder, a surfactant and deionized water into a container, mixing, vibrating by an ultrasonic oscillator, magnetically stirring, adding long-chain n-alkane into the container, continuously magnetically stirring, and carrying out water bath emulsification reaction for 40 minutes at normal temperature after stirring;
(2) adding tetraethoxysilane and methacryloxypropyl tris (trimethylsiloxy) silane into the container in the step (1), and magnetically stirring until the materials are uniformly mixed to obtain a dispersion solution;
(3) and (3) adding hexadecyl trimethylamine bromide and absolute ethyl alcohol into the dispersion solution obtained in the step (2), adding an emulsifier after stirring, increasing the stirring speed to 800 r/min, stirring, keeping the temperature of the mixed solution at 35 ℃, adding ammonia water to initiate interfacial cohydrolysis and cocondensation reaction, keeping the stirring speed at 300 r/min for 16 hours, and filtering, cleaning and drying the obtained white powder to obtain the phase-change microcapsule.
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