聚乙二醇类高分子型固—固相变储能材料的研究
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摘要
随着人类对能源的需求日益增加,相变储能材料(PCM)近年来已成为研究的热点。尤其是固-固相转变储能材料由于具有固-液相变材料所不具备的独特优点,已成为最具实际发展潜力的储热材料。然而,现有的固-固相变贮能材料也有其不足,例如多元醇类固-固相变贮能材料因存在塑晶而限制了它的使用;在低温范围内可供选择的无机盐类相变材料较少;高分子类相变材料品种少、相变焓较小、导热性能差等。因此急需研究和开发新型的固-固相变储能材料。
在本课题中,我们选用具有优异的相变特性和良好储能效果的聚乙二醇类相变单元作为研究对象,从分子设计出发,打破传统的通过接枝来实现PEG从固-液相变到固-固相变的方法,制备了四种高性能、多功能的聚乙二醇类固-固相转变材料。其分析结果表明制得的新型相变材料拥有较高的相变焓值和热性能稳,具有广阔的应用前景。
本课题的具体研究内容主要包括以下几个方面:
1.选择与聚乙二醇具有相同的羟基反应活性的MPEG作为相变单元,通过引入含有双键的N-羟甲基丙烯酰胺(NMA)合成了含有双键的MPEG大分子相变单体MPEG-TDI-NMA(PD)。然后采用PD与醋酸乙烯酯(VAc)共聚,形成侧链含有MPEG的新型固-固的相变储能材料(MGVM)。利用傅立叶变换红外光谱(FT-IR)和核磁共振氢谱(~1H-NMR)对MGVM组成、结构进行表征,通过差热扫描分析(DSC)、热失重分析(TG)、偏光显微镜(POM)对MGVM的相转变性能和热性能进行了测试。
结果表明成功制备了MGVM。同时当PD与VAc的比小于1∶50时,MGVM没有结晶峰。当PD与VAc的比等于1∶2时,其熔融焓值为80.66J/g,相变转变温度为72℃。当PD与VAc的比大于1∶50时,MGVM出现了结晶峰,结晶特性较好,但结晶焓值较低,其热分解温度可达到415℃。通过MGVM在一年使用中的储能特性的分析发现:MGVM的储能强度仅下降了10%,能够满足相变材料在储能使用寿命上的要求。
2.为了改善聚合物的结晶性能和热稳定性,进一步提高聚合物的相变焓值,我们采用含有刚性苯环的苯乙烯(St)作为聚合单元来代替VAc,合成了侧链含有MPEG相变单元的新型固-固相变材料(MGPM)。运用FT-IR和~1H-NMR表征了MGPM的组成与结构;利用DSC对MGPM的相转变性能进行了分析。利用TG和DTG对其热稳定性进行了分析;利用POM、广角X射线衍射(WAXD)对其储能、结晶性能进行分析。
结果表明,随着MPEG添加量的减少,聚合物的热稳定性逐渐提高。同时通过对MGPM进行了储能及结晶行为的分析,研究了MGPM和MGPM/蛋白石(Opal)复合材料的非等温结晶动力学,揭示了其结晶特点、实质及影响结晶的主要因素。其相变类型为有固-固相转变,相变的实质是侧链MPEG的软段部分可以通过发生晶态到无定形态的可逆固-固相变而储能。MGPM相变焓值随着PD和St的共聚比例的增大而增大,可以根据需要,通过改变投料比得到不同相变焓和不同相变温度的一系列固-固PCM。当PD和St投料摩尔比为1∶2时,MPEG的质量百分数可以达到71%,此时MGPM的相变熔融焓值达到最大;其熔融焓值为98.5 J/g,结晶焓值为71.6J/g。与PD和VAc的投料摩尔比为1∶2时的MGVM相比较,MGPM不仅出现了结晶焓值,而且焓值还很高。同时,引入支链带有刚性苯环基团的St作为聚合单体的MGPM的热分解温度要比同比例添加脂肪族的醋酸乙烯酯作为聚合单体的MGVM的热稳定性明显提高,所以通过引入苯乙烯单体代替醋酸乙烯酯得到了具有较好相变行为的固-固相变材料。
为了提高MGPM的结晶和相变性能,在MGPM中引入了具有天然纳米孔径结构的蛋白石制备了MGPM/Opal复合材料。对添加Opal前后的相变材料的晶体结构进行了表征,研究了MGPM和MGPM/Opal的结晶性能、成核机理。结果表明,适量添加蛋白石后晶区的晶形没有改变,但可以在一定程度上细化晶粒和提高结晶度。添加质量分数为0.7%蛋白石后的MGPM结晶度提高了3.12%。MGPM/Opal的相变焓值最高,达到109.07J/g。结晶速率比MGPM结晶速率明显提高,提高了99s。同时Opal的加入提高了共聚物的热稳定性,MGPM/Opal的在420℃以下不会发生热分解,所以通过引入Opal,MGPM/Opal的结晶性能和热稳定性得到了提高。
通过MGPM的非等温动力学研究表明:随着降温速率变大,结晶峰逐渐向低温区移动,结晶放热逐渐升高。这是由于分子运动的时间依赖性所致,聚合物从一种平衡态通过分子运动过渡到另一种与外界条件相适应的新的平衡态是需要时间的。所以降温速率越小,结晶开始越早,结晶峰峰值温度较高。整个分子链、链段、链节等运动单元的运动需要克服内摩擦力阻力,是不可能瞬时完成的,所以降温速率越快,结晶开始越晚,结晶峰向低温运动。降温速率大的时候,分子链运动需要在短时间达到新的平衡态,克服的内摩擦阻力做功越大,放热越多,因此结晶峰越大。
不同模型模拟的分析结果表明:MGPM的非等温动力学过程不符合Jeziprny模型,但是和Ozawa模型有较好的近似。MGPM的Avrami指数n的值介于3和4之间。这个结果表明:MGPM在结晶初期成核类型为散现成核,随着结晶时间的延续,MGPM成核类型从散现成核转变成以预先成核为主。MGPM/Opal的Avrami指数n的值接近于3,这说明加入蛋白石之后,MGPM/Opal成核类型发生了改变,其主要以预先成核为主。换句话说,Opal的引入,提高了MGPM/Opal的成核速率,赋予了MGPM/Opal优异的相转变特性。
3.为了研究合成优异的相转变材料的新型聚合方法,我们合成了含有双羟基并带有MPEG相变单元的新型单体,然后通过逐步聚合的方法合成了一种新型的相变储能材料(MGEM)。通过FT-IR和~1H-NMR等测试手段,对MGEM的组成和结构进行了表征。通过DSC、TGA等分析方法对其相变性能和热性能进行测试。结果表明得到了预期的产物,共聚物具有良好的相变性能和热稳定性,相变焓值为75.6J/g。
4.在课题的最后一部分中,我们合成了一种超支化固-固相转变材料PUPCM。在PUPCM中,其支化度越高,则PUPCM的相转变单元的含有越高,故而其相变焓值越高,最高可达到105.35J/g。通过选用不同分子量的PEG,我们合成了不同的PUPCM,并以此研究了它们的相变类形、结晶度和相变焓值的变化规律。结果表明,PUPCM的相变焓值随着PEG分子量的增大而逐渐增大。聚合物结构规整,结晶类型为完整的球晶状态并具有良好的热稳定性。
同时,以天然无机纳米材料-蛋白石(Opal)微粉作为无机异相成核剂,我们制备了PUPCM/Opal固-固相转变材料;通过DSC和POM分析表明:制备的PUPCM/Opal具有更高的相变焓值和适宜的相变温度。
As demand for energy resources increasing, the researches of energy storage phase changed materials (PCM) has become a hotspot in recent years, especially the solid-solid phase changed energy storage materials with some unique advantages has now become the most potential application materials. However, some defects do exist in the solid-solid phase changed energy storage materials. For example, the applications of the polyhydric alcohols solid-solid phase changed energy storage materials have their limitations with plastic crystals existing; inorganic salt phase changed materials in low temperatures are not enough; the varieties of macromolecules is limited. Their phase change enthalpy and thermal conductivity properties are small and poor. So, researches on development of some new solid-solid phase changed materials are urgent -needed.
In this paper, the researches were made on polyethylene glycol phase changed materials with outstanding phase change characteristics and heat storage properties. We started our work from molecule design, used untraditional grafting methods, made achievements on solid-solid phase change from traditional PEG solid-liquid phase change, and prepared high-performance, multi-functional solid - solid phase changed materials. Four kinds of Polyethylene glycol phase changed materials were prepared in this work. The analysis results show that the novel polymers prepared possess of higher phase transition enthalpy value and stable thermal performance with excellent prospect of application.
The main results of this study are as follow:
1. The MPEG with same hydroxyl reactive activity of the PEG was used as the basic phase change unit. MPEG macromolecule phase changed monomer MPEG-TDI-NMA (PD) containing double bonds was synthesized by introducing NMA with double bonds, and the PD was copolymerized with Vinyl acetate (VAc). In that way, a new solid-solid phase changed heat storage material (MGVM) with side chains containing MPEG was prepared. The composition and structure of the MGVG were characterized with Fourier transform infrared spectroscopy (FT-IR) and hydrogen-nuclear magnetic resonance spectrum (~1H-NMR). Properties of the MGVM were tested through differential scanning calorimetry (DSC), thermal gravimetric analysis (TG), and partial Optical microscopy (POM).
The results show that the MGVG has been successfully prepared. Furthermore, MGVM has no crystal peak until the ratio of PD: VAc was more than 1:50. When the ratio of PD: VAc is 1:2, its melting enthalpy value reaches 80.66 J/g and melting phase change temperature is 72℃. When the ratio was more than 1:50, crystal peak appeared and the crystal properties were better, but the crystallization enthalpy value became lower, and the decomposition temperature was 415℃. By analyzing the heat storage behavior of the MGVM after 12 months and its recyclable property, we found that the ultimate heat storage intensity only decreased 10%, whose durability satisfied the demand of the heat storage materials.
2. In order to improve the crystal properties and thermal stability of the MGVG, and enhance its phase transition enthalpy value, we used styrene (St) containing rigid benzene ring as the polymerization unit instead of the VAc, synthesized the novel solid-solid phase change materials (MGPM) which had side chains containing MPEG. The composition and structure of the MGPM were characterized by FT-IR and ~1H-NMR; DSC was used to analyze the transformation properties of the MGPM; its thermal properties were analyzed via TG and DTG; heat storage and crystal properties of the MGPM were analyzed via polarizing optical microscopy (POM) and wide-angle X-ray diffraction (WAXD).
The results showed that thermal stability of the MGPM gradually improved with the MPEG decreasing, and its effects on the behavior of heat storage and crystallization of the MGPM were also analysis. Researches on their non-isothermal crystallization kinetics of the MGPM and MGPM/Opal were made; the characteristics, essence and main factors of the crystallization were reveals. The transformation of the MGPM was a kind of solid - solid phase change, and the heat storage happened when the soft part of the side chain MPEG transformed from crystal phase to amorphous phase. The phase change enthalpy value of the MGPM enhanced with the copolymerization proportion of PD and St increasing. If necessary, we can produce a series of solid-solid PCM with different phase change enthalpy value and different phase change temperature by changing the copolymerization proportion. When the ratio of PD to St was 1:2, and the percentage of the MPEG was 71%, the phase change enthalpy value of the MGPM reached the highest, with the melting enthalpy value of 98.5 J/g and the crystallization enthalpy value of 71.6 J/g. Compared with the enthalpy value of the MGPM synthesized with the ratio of PD to VAc of 1:2, high crystallization enthalpy value of the MGPM appeared. The decomposition temperature of the MGPM with St as the polymerization unit was apparently higher than the MGVM's with aliphatic vinyl acetate as the polymerization unit with the same ratio. In that way, a excellent solid-solid changed material was produced by introducing the styrene monomer instead of the vinyl acetate monomer for polymerization.
By adding Opal to MGPM materials to produce a kind of MGPM/opal composite material, its properties of crystallization and transformation was improved. Both the crystal structures of the MGPM and MGPM/Opal were characterized with WAXD diffraction, and their crystal properties and nucleation mechanisms were also analyzed. The results showed that the crystal type has been not changed after adding Opal with proper quantity, but the crystal grain was smaller and the crystallinity was increased. The crystallinity of the MGPM/opal increased 3.12% by adding 0.7% opal, with higher transitional enthalpy value of 109.07J/g, and crystallization rate is apparently increased. Comparing the MGPM with the MGVM, the time shortened is 99-second. Generally speaking, the thermal stability of the MGPM/Opal was improved, which would not decompose below 420°C, and also the crystallization properties.
The non-isothermal kinetics of the MGPM showed that: crystal peaks of the MGPM moved to lower temperature zone with the rate of temperature decreasing, and the exothermal crystallization increased, for a new balance of the MGPM formed by molecular movement after some time. With lower rate of temperature decreasing, crystallization happened earlier, and the temperature of the crystal peak was higher. When the whole molecular chain, chain segment and chain element moved, internal friction should be overcome, which made instant movement impossible. So the higher rate of temperature decreasing, the later the crystallization happened, and the crystallization peak are moved to low temperature district. Otherwise, the higher rate of temperature decreasing, the shorter the time of the movement of molecular chain arrives at the new equilibrium state, the bigger the energy of overcoming internal friction, and the more the heat produced, so the crystallization peak is stronger.
The results of the analysis of the different models show that the non-isothermal dynamics process of MGPM don't match Jeziprny model, but the Ozawa model is suitable to describe its non-isothermal crystallization behaviors. For the MGPM, the Avrami exponent obtained based on the Ozawa model lies in the range of 3 to 4. The results show that the nucleating type of MGPM is sporadic nucleation during the crystallization initial stage. As the crystalline time increasing, the nucleating type of MGPM is changed into instantaneous nucleation. The Avrami exponent of MGPM / Opal based on the Ozawa model is closer to 3. This showed that after the accession of opal, there is influence to the nucleating type of MGPM/Opal. The nucleating type of MGPM / Opal mainly is instantaneous nucleation. In other words, the introducing Opal increases the nucleating rate of MGPM/Opal, and endows with the excellent phase change properties for the MGPM/Opal.
3. In order to research novel polymeric ways for synthesizing unique phase change materials, we synthesized a new phase change monomer with double-hydroxyl and PEG unit. The new phase change material (MGEM) was prepared with the monomer via step copolymerization. The composition and structure of MGEM were characterized by FTIR and 1 H-NMR. The phase change performance and thermal properties were analyzed by DSC and TG. The results show that the composition and structure of MGEM is the same as that of the anticipated polymer. At same time, the copolymer possesses of excellent phase transition behaviors and thermal stability, and the phase transition enthalpy value of MGEM is 75.6 J / g.
4. In the last section of the paper, we synthesized a hyperbranched solid - solid phase change materials (PUPCM). In the PUPCM, the higher of the degree of branching, the higher the phase change unit. So the PUPCM has higher phase change behaviors, and the highest phase change enthalpy value could reach 105.35 J/g. By using the PEG with different molecular weigh, different PUPCM were synthesized. Furthermore, the crystalline type, crystallization, and the phase change enthalpy value of different PUPCM were researched. The results showed that the crystallization and the phase change enthalpy value of PUPCM were enhanced with the increase of molecular weight of PEG. The structure of PUPCM is regular, the crystalline type is perfect ball-crystal, and thermal stability is good.
By adding inorganic nanomaterial-Opal to PUPCM materials to produce a kind of PUPCM/Opal composite material, its properties of crystallization and phase change behaviors was further improved. The analysis of DSC and POM of PUPCM/Opal show that the PUPCM/Opal has higher phase change enthalpy value and appropriate phase change temperature.
在本课题中,我们选用具有优异的相变特性和良好储能效果的聚乙二醇类相变单元作为研究对象,从分子设计出发,打破传统的通过接枝来实现PEG从固-液相变到固-固相变的方法,制备了四种高性能、多功能的聚乙二醇类固-固相转变材料。其分析结果表明制得的新型相变材料拥有较高的相变焓值和热性能稳,具有广阔的应用前景。
本课题的具体研究内容主要包括以下几个方面:
1.选择与聚乙二醇具有相同的羟基反应活性的MPEG作为相变单元,通过引入含有双键的N-羟甲基丙烯酰胺(NMA)合成了含有双键的MPEG大分子相变单体MPEG-TDI-NMA(PD)。然后采用PD与醋酸乙烯酯(VAc)共聚,形成侧链含有MPEG的新型固-固的相变储能材料(MGVM)。利用傅立叶变换红外光谱(FT-IR)和核磁共振氢谱(~1H-NMR)对MGVM组成、结构进行表征,通过差热扫描分析(DSC)、热失重分析(TG)、偏光显微镜(POM)对MGVM的相转变性能和热性能进行了测试。
结果表明成功制备了MGVM。同时当PD与VAc的比小于1∶50时,MGVM没有结晶峰。当PD与VAc的比等于1∶2时,其熔融焓值为80.66J/g,相变转变温度为72℃。当PD与VAc的比大于1∶50时,MGVM出现了结晶峰,结晶特性较好,但结晶焓值较低,其热分解温度可达到415℃。通过MGVM在一年使用中的储能特性的分析发现:MGVM的储能强度仅下降了10%,能够满足相变材料在储能使用寿命上的要求。
2.为了改善聚合物的结晶性能和热稳定性,进一步提高聚合物的相变焓值,我们采用含有刚性苯环的苯乙烯(St)作为聚合单元来代替VAc,合成了侧链含有MPEG相变单元的新型固-固相变材料(MGPM)。运用FT-IR和~1H-NMR表征了MGPM的组成与结构;利用DSC对MGPM的相转变性能进行了分析。利用TG和DTG对其热稳定性进行了分析;利用POM、广角X射线衍射(WAXD)对其储能、结晶性能进行分析。
结果表明,随着MPEG添加量的减少,聚合物的热稳定性逐渐提高。同时通过对MGPM进行了储能及结晶行为的分析,研究了MGPM和MGPM/蛋白石(Opal)复合材料的非等温结晶动力学,揭示了其结晶特点、实质及影响结晶的主要因素。其相变类型为有固-固相转变,相变的实质是侧链MPEG的软段部分可以通过发生晶态到无定形态的可逆固-固相变而储能。MGPM相变焓值随着PD和St的共聚比例的增大而增大,可以根据需要,通过改变投料比得到不同相变焓和不同相变温度的一系列固-固PCM。当PD和St投料摩尔比为1∶2时,MPEG的质量百分数可以达到71%,此时MGPM的相变熔融焓值达到最大;其熔融焓值为98.5 J/g,结晶焓值为71.6J/g。与PD和VAc的投料摩尔比为1∶2时的MGVM相比较,MGPM不仅出现了结晶焓值,而且焓值还很高。同时,引入支链带有刚性苯环基团的St作为聚合单体的MGPM的热分解温度要比同比例添加脂肪族的醋酸乙烯酯作为聚合单体的MGVM的热稳定性明显提高,所以通过引入苯乙烯单体代替醋酸乙烯酯得到了具有较好相变行为的固-固相变材料。
为了提高MGPM的结晶和相变性能,在MGPM中引入了具有天然纳米孔径结构的蛋白石制备了MGPM/Opal复合材料。对添加Opal前后的相变材料的晶体结构进行了表征,研究了MGPM和MGPM/Opal的结晶性能、成核机理。结果表明,适量添加蛋白石后晶区的晶形没有改变,但可以在一定程度上细化晶粒和提高结晶度。添加质量分数为0.7%蛋白石后的MGPM结晶度提高了3.12%。MGPM/Opal的相变焓值最高,达到109.07J/g。结晶速率比MGPM结晶速率明显提高,提高了99s。同时Opal的加入提高了共聚物的热稳定性,MGPM/Opal的在420℃以下不会发生热分解,所以通过引入Opal,MGPM/Opal的结晶性能和热稳定性得到了提高。
通过MGPM的非等温动力学研究表明:随着降温速率变大,结晶峰逐渐向低温区移动,结晶放热逐渐升高。这是由于分子运动的时间依赖性所致,聚合物从一种平衡态通过分子运动过渡到另一种与外界条件相适应的新的平衡态是需要时间的。所以降温速率越小,结晶开始越早,结晶峰峰值温度较高。整个分子链、链段、链节等运动单元的运动需要克服内摩擦力阻力,是不可能瞬时完成的,所以降温速率越快,结晶开始越晚,结晶峰向低温运动。降温速率大的时候,分子链运动需要在短时间达到新的平衡态,克服的内摩擦阻力做功越大,放热越多,因此结晶峰越大。
不同模型模拟的分析结果表明:MGPM的非等温动力学过程不符合Jeziprny模型,但是和Ozawa模型有较好的近似。MGPM的Avrami指数n的值介于3和4之间。这个结果表明:MGPM在结晶初期成核类型为散现成核,随着结晶时间的延续,MGPM成核类型从散现成核转变成以预先成核为主。MGPM/Opal的Avrami指数n的值接近于3,这说明加入蛋白石之后,MGPM/Opal成核类型发生了改变,其主要以预先成核为主。换句话说,Opal的引入,提高了MGPM/Opal的成核速率,赋予了MGPM/Opal优异的相转变特性。
3.为了研究合成优异的相转变材料的新型聚合方法,我们合成了含有双羟基并带有MPEG相变单元的新型单体,然后通过逐步聚合的方法合成了一种新型的相变储能材料(MGEM)。通过FT-IR和~1H-NMR等测试手段,对MGEM的组成和结构进行了表征。通过DSC、TGA等分析方法对其相变性能和热性能进行测试。结果表明得到了预期的产物,共聚物具有良好的相变性能和热稳定性,相变焓值为75.6J/g。
4.在课题的最后一部分中,我们合成了一种超支化固-固相转变材料PUPCM。在PUPCM中,其支化度越高,则PUPCM的相转变单元的含有越高,故而其相变焓值越高,最高可达到105.35J/g。通过选用不同分子量的PEG,我们合成了不同的PUPCM,并以此研究了它们的相变类形、结晶度和相变焓值的变化规律。结果表明,PUPCM的相变焓值随着PEG分子量的增大而逐渐增大。聚合物结构规整,结晶类型为完整的球晶状态并具有良好的热稳定性。
同时,以天然无机纳米材料-蛋白石(Opal)微粉作为无机异相成核剂,我们制备了PUPCM/Opal固-固相转变材料;通过DSC和POM分析表明:制备的PUPCM/Opal具有更高的相变焓值和适宜的相变温度。
As demand for energy resources increasing, the researches of energy storage phase changed materials (PCM) has become a hotspot in recent years, especially the solid-solid phase changed energy storage materials with some unique advantages has now become the most potential application materials. However, some defects do exist in the solid-solid phase changed energy storage materials. For example, the applications of the polyhydric alcohols solid-solid phase changed energy storage materials have their limitations with plastic crystals existing; inorganic salt phase changed materials in low temperatures are not enough; the varieties of macromolecules is limited. Their phase change enthalpy and thermal conductivity properties are small and poor. So, researches on development of some new solid-solid phase changed materials are urgent -needed.
In this paper, the researches were made on polyethylene glycol phase changed materials with outstanding phase change characteristics and heat storage properties. We started our work from molecule design, used untraditional grafting methods, made achievements on solid-solid phase change from traditional PEG solid-liquid phase change, and prepared high-performance, multi-functional solid - solid phase changed materials. Four kinds of Polyethylene glycol phase changed materials were prepared in this work. The analysis results show that the novel polymers prepared possess of higher phase transition enthalpy value and stable thermal performance with excellent prospect of application.
The main results of this study are as follow:
1. The MPEG with same hydroxyl reactive activity of the PEG was used as the basic phase change unit. MPEG macromolecule phase changed monomer MPEG-TDI-NMA (PD) containing double bonds was synthesized by introducing NMA with double bonds, and the PD was copolymerized with Vinyl acetate (VAc). In that way, a new solid-solid phase changed heat storage material (MGVM) with side chains containing MPEG was prepared. The composition and structure of the MGVG were characterized with Fourier transform infrared spectroscopy (FT-IR) and hydrogen-nuclear magnetic resonance spectrum (~1H-NMR). Properties of the MGVM were tested through differential scanning calorimetry (DSC), thermal gravimetric analysis (TG), and partial Optical microscopy (POM).
The results show that the MGVG has been successfully prepared. Furthermore, MGVM has no crystal peak until the ratio of PD: VAc was more than 1:50. When the ratio of PD: VAc is 1:2, its melting enthalpy value reaches 80.66 J/g and melting phase change temperature is 72℃. When the ratio was more than 1:50, crystal peak appeared and the crystal properties were better, but the crystallization enthalpy value became lower, and the decomposition temperature was 415℃. By analyzing the heat storage behavior of the MGVM after 12 months and its recyclable property, we found that the ultimate heat storage intensity only decreased 10%, whose durability satisfied the demand of the heat storage materials.
2. In order to improve the crystal properties and thermal stability of the MGVG, and enhance its phase transition enthalpy value, we used styrene (St) containing rigid benzene ring as the polymerization unit instead of the VAc, synthesized the novel solid-solid phase change materials (MGPM) which had side chains containing MPEG. The composition and structure of the MGPM were characterized by FT-IR and ~1H-NMR; DSC was used to analyze the transformation properties of the MGPM; its thermal properties were analyzed via TG and DTG; heat storage and crystal properties of the MGPM were analyzed via polarizing optical microscopy (POM) and wide-angle X-ray diffraction (WAXD).
The results showed that thermal stability of the MGPM gradually improved with the MPEG decreasing, and its effects on the behavior of heat storage and crystallization of the MGPM were also analysis. Researches on their non-isothermal crystallization kinetics of the MGPM and MGPM/Opal were made; the characteristics, essence and main factors of the crystallization were reveals. The transformation of the MGPM was a kind of solid - solid phase change, and the heat storage happened when the soft part of the side chain MPEG transformed from crystal phase to amorphous phase. The phase change enthalpy value of the MGPM enhanced with the copolymerization proportion of PD and St increasing. If necessary, we can produce a series of solid-solid PCM with different phase change enthalpy value and different phase change temperature by changing the copolymerization proportion. When the ratio of PD to St was 1:2, and the percentage of the MPEG was 71%, the phase change enthalpy value of the MGPM reached the highest, with the melting enthalpy value of 98.5 J/g and the crystallization enthalpy value of 71.6 J/g. Compared with the enthalpy value of the MGPM synthesized with the ratio of PD to VAc of 1:2, high crystallization enthalpy value of the MGPM appeared. The decomposition temperature of the MGPM with St as the polymerization unit was apparently higher than the MGVM's with aliphatic vinyl acetate as the polymerization unit with the same ratio. In that way, a excellent solid-solid changed material was produced by introducing the styrene monomer instead of the vinyl acetate monomer for polymerization.
By adding Opal to MGPM materials to produce a kind of MGPM/opal composite material, its properties of crystallization and transformation was improved. Both the crystal structures of the MGPM and MGPM/Opal were characterized with WAXD diffraction, and their crystal properties and nucleation mechanisms were also analyzed. The results showed that the crystal type has been not changed after adding Opal with proper quantity, but the crystal grain was smaller and the crystallinity was increased. The crystallinity of the MGPM/opal increased 3.12% by adding 0.7% opal, with higher transitional enthalpy value of 109.07J/g, and crystallization rate is apparently increased. Comparing the MGPM with the MGVM, the time shortened is 99-second. Generally speaking, the thermal stability of the MGPM/Opal was improved, which would not decompose below 420°C, and also the crystallization properties.
The non-isothermal kinetics of the MGPM showed that: crystal peaks of the MGPM moved to lower temperature zone with the rate of temperature decreasing, and the exothermal crystallization increased, for a new balance of the MGPM formed by molecular movement after some time. With lower rate of temperature decreasing, crystallization happened earlier, and the temperature of the crystal peak was higher. When the whole molecular chain, chain segment and chain element moved, internal friction should be overcome, which made instant movement impossible. So the higher rate of temperature decreasing, the later the crystallization happened, and the crystallization peak are moved to low temperature district. Otherwise, the higher rate of temperature decreasing, the shorter the time of the movement of molecular chain arrives at the new equilibrium state, the bigger the energy of overcoming internal friction, and the more the heat produced, so the crystallization peak is stronger.
The results of the analysis of the different models show that the non-isothermal dynamics process of MGPM don't match Jeziprny model, but the Ozawa model is suitable to describe its non-isothermal crystallization behaviors. For the MGPM, the Avrami exponent obtained based on the Ozawa model lies in the range of 3 to 4. The results show that the nucleating type of MGPM is sporadic nucleation during the crystallization initial stage. As the crystalline time increasing, the nucleating type of MGPM is changed into instantaneous nucleation. The Avrami exponent of MGPM / Opal based on the Ozawa model is closer to 3. This showed that after the accession of opal, there is influence to the nucleating type of MGPM/Opal. The nucleating type of MGPM / Opal mainly is instantaneous nucleation. In other words, the introducing Opal increases the nucleating rate of MGPM/Opal, and endows with the excellent phase change properties for the MGPM/Opal.
3. In order to research novel polymeric ways for synthesizing unique phase change materials, we synthesized a new phase change monomer with double-hydroxyl and PEG unit. The new phase change material (MGEM) was prepared with the monomer via step copolymerization. The composition and structure of MGEM were characterized by FTIR and 1 H-NMR. The phase change performance and thermal properties were analyzed by DSC and TG. The results show that the composition and structure of MGEM is the same as that of the anticipated polymer. At same time, the copolymer possesses of excellent phase transition behaviors and thermal stability, and the phase transition enthalpy value of MGEM is 75.6 J / g.
4. In the last section of the paper, we synthesized a hyperbranched solid - solid phase change materials (PUPCM). In the PUPCM, the higher of the degree of branching, the higher the phase change unit. So the PUPCM has higher phase change behaviors, and the highest phase change enthalpy value could reach 105.35 J/g. By using the PEG with different molecular weigh, different PUPCM were synthesized. Furthermore, the crystalline type, crystallization, and the phase change enthalpy value of different PUPCM were researched. The results showed that the crystallization and the phase change enthalpy value of PUPCM were enhanced with the increase of molecular weight of PEG. The structure of PUPCM is regular, the crystalline type is perfect ball-crystal, and thermal stability is good.
By adding inorganic nanomaterial-Opal to PUPCM materials to produce a kind of PUPCM/Opal composite material, its properties of crystallization and phase change behaviors was further improved. The analysis of DSC and POM of PUPCM/Opal show that the PUPCM/Opal has higher phase change enthalpy value and appropriate phase change temperature.
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