CN1474180A - Method and device for continuously measuring lifetime of phase change material - Google Patents
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Abstract
本发明涉及一种连续测定相变材料寿命的方法：将待测相变材料放入熔冻实验池中，利用冷液和热液两组自动循环熔冻系统对其进行连续多次熔冻实验；在实验过程中，温度测量装置连续检测其温度变化数据，并将其同时分别送给数据采集装置和温控开关装置，由后者对冷液和热液两组自动循环熔冻系统进行自动切换，而由前者记录并计算出相变材料温度随时间的变化数值和绘制出该变化曲线，进而依此确定相变材料的相变点及相变热的相对大小，测定出相变材料的寿命。本发明连续测定相变材料寿命的装置按本发明方法设计。本发明方法取样多，可自动连续测量，测定准确，费用较低；本发明装置结构简单，制造成本低，操作简便，使用费用少。
The invention relates to a method for continuously measuring the service life of a phase change material: put the phase change material to be tested into a thawing test pool, and use two sets of automatic circulation thawing systems of cold liquid and hot liquid to conduct continuous multiple thawing experiments ;During the experiment, the temperature measurement device continuously detects the temperature change data, and sends it to the data acquisition device and the temperature control switch device at the same time, and the latter automatically controls the two sets of automatic circulation freezing systems of cold liquid and hot liquid. switch, and the former records and calculates the change value of the temperature of the phase change material with time and draws the change curve, and then determines the phase change point of the phase change material and the relative size of the phase change heat, and determines the temperature of the phase change material. life. The device for continuously measuring the lifetime of phase change materials of the present invention is designed according to the method of the present invention. The method of the invention has many samples, can be automatically and continuously measured, is accurate in measurement, and has low cost; the device of the invention has simple structure, low manufacturing cost, convenient operation and low use cost.
Description
技术领域technical field
本发明涉及相变材料寿命的测量技术，尤其涉及一种经历多次熔冻实验后，根据相变材料在冷凝过程中温度随时间的变化曲线来测定相变材料寿命的方法及装置，国际专利主分类号拟为Int.C17.G01N 25/06。The present invention relates to the measurement technology of the life of phase change materials, in particular to a method and device for measuring the life of phase change materials according to the curve of temperature change with time during the condensation process of the phase change materials after multiple thawing experiments, international patent The main classification number is proposed to be Int.C17.G01N 25/06.
背景技术Background technique
相变材料在使用过程中，由于经历反复相变过程，其结构及功能可能产生改变，例如有机相变材料，因老化，材料会改变原有的性质；又例如无机水合盐相变材料，由于不可避免的相分离趋势，材料的相变热将会逐渐减小。因此，在反复使用后，将由于环境及自身因素的影响，相变材料的功能会产生改变或丧失，这种相变材料的相变点漂移及相变热发生一定衰变的使用次数称为其寿命。During the use of phase change materials, due to repeated phase change processes, their structure and function may change. For example, organic phase change materials will change their original properties due to aging; another example is inorganic hydrated salt phase change materials. Due to With the inevitable phase separation tendency, the phase change heat of the material will gradually decrease. Therefore, after repeated use, the function of the phase change material will be changed or lost due to the influence of the environment and its own factors. life.
对于相变材料寿命的测量，目前还没有统一的标准。通常的方法是考察多次熔冻实验后，相变材料熔点变化大小和相变潜热衰变多少来判断其寿命。熔点的测量方法通常有两种：步冷曲线法和熔点测定仪测定法。相变热的测定方法一般有三种：常规卡计法、差热分析法(DTA)和差示扫描量热法(DSC)。There is no uniform standard for the measurement of the lifetime of phase change materials. The usual method is to judge the lifetime of the phase change material by examining the change in the melting point of the phase change material and the decay of the latent heat of phase change after multiple thawing experiments. There are usually two methods for measuring melting point: step cooling curve method and melting point determination method. There are generally three methods for the determination of phase change heat: conventional calorimeter method, differential thermal analysis (DTA) and differential scanning calorimetry (DSC).
这些常规测定相变材料寿命的方法，必须人工经过多次熔冻实验，每次熔冻实验后都要测定相变材料的相变点和相变热，然后再按下式算出相变材料的衰变率：η＝Hmi/Hm0，式中，Hm0、Hmi分别为相变材料初始及经过i次熔冻实验后的相变潜热。These conventional methods of measuring the life of phase change materials must manually go through multiple thawing experiments. Decay rate: η=H mi /H m0 , where H m0 and H mi are the phase change latent heat of the phase change material at the initial stage and after i times of thawing experiments respectively.
这些测量方法的优点是测量精度较高，但缺点也是显而易见的：首先，由于相变材料寿命的测量判断要经过几百次，甚至上千次熔冻实验，才能获得；而且必须进行DSC测试与冻融实验配套，而DSC测定所取试样每次仅为2.0-10.0毫克，实验结果不能真正反映所测材料(特别是大块材料)的热物性；同时受测定方法所限，测量也不能自动进行，费时费力；特别是不能系统和连续地观测相变材料的衰变过程；此外，上述测量方法测试费用较高，不利于实际应用和推广。The advantage of these measurement methods is that the measurement accuracy is high, but the disadvantages are also obvious: first, because the measurement and judgment of the phase change material life can only be obtained after hundreds or even thousands of thawing experiments; Freezing and thawing experiments are matched, and the samples taken by DSC are only 2.0-10.0 mg each time. The experimental results cannot truly reflect the thermal properties of the measured materials (especially bulk materials); at the same time, due to the limitation of the measurement method, the measurement cannot Automatically, time-consuming and labor-intensive; especially, the decay process of phase-change materials cannot be observed systematically and continuously; in addition, the above-mentioned measurement methods are expensive to test, which is not conducive to practical application and promotion.
发明内容 Contents of the invention
针对现有测定方法的不足，本发明主要解决所述的技术问题是提供一种连续测定相变材料寿命的方法，它具有取样多，可自动连续测量，测定结果准确，且费用较低等优点；同时也设计一种实施本发明方法的连续测定相变材料寿命的装置，该装置具有结构简单，制造成本低，操作简便，使用费用少等优点。Aiming at the deficiencies of the existing measuring methods, the main solution of the present invention is to provide a method for continuously measuring the life of phase change materials, which has the advantages of many samples, automatic and continuous measurement, accurate measurement results, and low cost. Simultaneously also design a kind of device that implements the continuous measurement phase change material life of the inventive method, this device has advantages such as simple in structure, manufacturing cost is low, easy and simple to operate, use cost is few.
本发明解决所述方法技术问题的技术方案是：设计一种连续测定相变材料寿命的方法：将待测相变材料放入熔冻实验池中，利用与之相连的冷液和热液两组液流循环装置对其进行连续多次熔冻实验；冷液和热液两组液流循环装置分别由各自的液流输送设备及流量计量设备构成；冷液和热液两组液流循环装置和与其相连的低、高温恒温浴槽共同构成了自动循环熔冻系统；在实验过程中，利用温度测量装置从与之相连接的实验池中连续检测其温度变化数据，并将该采集数据同时分别送给与之相连的数据采集装置和温控开关装置，由后者对冷液和热液两组液流循环装置进行自动切换，而由前者记录并计算出相变材料温度随时间的变化数值和绘制出该变化曲线，进而依此确定相变材料的相变点及相变热的相对大小，测定出相变材料的寿命。The technical scheme of the present invention to solve the technical problems of the method is: to design a method for continuously measuring the life of the phase change material: put the phase change material to be tested into the freezing test pool, and use the two cold liquid and hot liquid connected to it A group of liquid flow circulation devices are used for multiple consecutive thawing experiments; the two sets of liquid flow circulation devices for cold liquid and hot liquid are respectively composed of their own liquid flow conveying equipment and flow metering equipment; the two sets of liquid flow circulation for cold liquid and hot liquid The device and the low and high temperature constant temperature baths connected to it together constitute an automatic circulation thawing system; They are respectively sent to the connected data acquisition device and temperature control switch device, the latter automatically switches the two groups of liquid flow circulation devices for cold liquid and hot liquid, while the former records and calculates the temperature change of the phase change material with time Numerical and draw the change curve, and then determine the phase change point of the phase change material and the relative size of the phase change heat, and measure the life of the phase change material.
本发明解决所述装置技术问题的技术方案是，按照本发明方法设计的一种连续测定相变材料寿命的装置，其特征在于它包含承载被测相变材料的熔冻实验池装置，与之相连可连续多次对相变材料进行熔冻实验的独立的两组液流循环装置；两组液流循环装置中的一组是低温液流循环装置，其与低温恒温浴槽相连接；另一组是高温液流循环装置，其与高温恒温浴槽相连接，并且所述的低温液流循环装置和高温液流循环装置分别与可切换其输送设备起闭的温控开关装置相连接；温控开关装置还与温度测量装置相连接；温度测量装置分别与所述的熔冻实验池装置和数据采集装置相连接。The technical solution of the present invention to solve the technical problems of the device is that a device for continuously measuring the life of a phase change material designed according to the method of the present invention is characterized in that it includes a thawing test pool device carrying the measured phase change material, and Two sets of independent liquid flow circulation devices that can be connected to conduct thawing experiments on phase change materials for multiple times in a row; The first group is a high-temperature liquid flow circulation device, which is connected with a high-temperature constant temperature bath, and the low-temperature liquid flow circulation device and the high-temperature liquid flow circulation device are respectively connected with a temperature control switch device that can switch the on and off of the conveying equipment; The switch device is also connected with the temperature measuring device; the temperature measuring device is respectively connected with the freezing experiment pool device and the data acquisition device.
本发明方法独特设计了自动循环熔冻系统，可根据相变材料在冷凝过程中温度随时间变化的曲线规律来测定相变材料寿命的方法，与传统测定方法相比，具有以下优点：无需进行DSC测试与冻融实验配套；测试采样数量多，一般可取30g左右，因此可以更准确地反映大块物料的热物性等，使所得数据更接近工程应用的实际情况；本发明设计的连续测定相变材料寿命的装置结构简单，无需成套的精密仪器，成本低，进而使用本装置测试的费用也大幅降低，测试费用比目前通用的方法低50％以上；同时相变潜热的测定方法也简捷，并可实现连续的寿命测定；另外，本发明所述的对相变材料寿命的连续测定，无论对无机相变材料还是对有机相变材料均可适用，大大有利于相变材料寿命的筛选。The method of the present invention has a unique design of an automatic cycle thawing system, which can measure the life of the phase change material according to the curve of the temperature of the phase change material during the condensation process with time. Compared with the traditional measurement method, it has the following advantages: no need to carry out The DSC test is matched with the freeze-thaw experiment; the number of test samples is large, generally about 30g, so it can more accurately reflect the thermal properties of bulk materials, etc., making the obtained data closer to the actual situation of engineering applications; the continuous measurement phase designed by the present invention The life-changing device has a simple structure, does not require a complete set of precision instruments, and is low in cost. The cost of testing with this device is also greatly reduced, and the test cost is more than 50% lower than the current general method; at the same time, the method for measuring the latent heat of phase change is also simple and convenient. And it can realize continuous life measurement; in addition, the continuous measurement of phase change material life according to the present invention is applicable to both inorganic phase change materials and organic phase change materials, which greatly facilitates the screening of phase change material life.
附图说明：Description of drawings:
下面结合实施例及其附图详细描述本发明。The present invention will be described in detail below in conjunction with the embodiments and accompanying drawings.
图1-1是相变材料不出现过冷现象时，确定相变温度随时间变化的步冷曲线图。由于物质发生相变时，具有一定的热效应，因此出现第一个转折点处所对应的温度被定义为相变温度。如图1-1中的Tm；Figure 1-1 is a step-cooling curve for determining the change of the phase transition temperature with time when the phase change material does not appear to be overcooled. Since there is a certain thermal effect when a substance undergoes a phase transition, the temperature corresponding to the first turning point is defined as the phase transition temperature. T m in Figure 1-1;
图1-2是相变材料出现过冷现象时，确定相变温度随时间变化的步冷曲线图。由图1-2可以看出，当步冷曲线出现第一转折点后，温度会有一定的回升(即过冷现象)，通常将相变材料出现过冷而回升的最高温度定义为相变温度。如图1-2中的Tm。Figure 1-2 is a step cooling curve for determining the change of phase transition temperature with time when supercooling occurs in the phase change material. It can be seen from Figure 1-2 that when the first turning point of the step cooling curve appears, the temperature will rise to a certain extent (that is, the phenomenon of supercooling). Usually, the highest temperature at which the phase change material is supercooled and rises is defined as the phase change temperature. . T m in Figure 1-2.
图2是本发明测定相变材料寿命方法的原理示意图；其中，Fig. 2 is a schematic diagram of the principle of the method for measuring the lifetime of phase change materials in the present invention; wherein,
图2-1是相变材料在第一次冷凝过程中，利用数据采集系统记录并处理的相变温度与时间的关系图；Figure 2-1 is a graph of the relationship between phase change temperature and time recorded and processed by the data acquisition system during the first condensation process of the phase change material;
图2-2是相变材料在第i次冷凝过程中，利用数据采集系统记录并处理的相变温度与时间关系图。Figure 2-2 is a diagram of the relationship between phase change temperature and time recorded and processed by the data acquisition system during the ith condensation process of the phase change material.
图3是本发明连续测定相变材料寿命的装置的一种实施例结构原理框图；Fig. 3 is a block diagram of an embodiment of the device for continuously measuring the lifetime of a phase change material in the present invention;
图4是本发明测定相变材料寿命的装置与图3所述的方法结构原理对应的一种实施例结构示意图；Fig. 4 is a schematic diagram of an embodiment corresponding to the device for measuring the life of a phase change material according to the present invention and the method structure principle described in Fig. 3;
图5是本发明实施例1相变材料相变点随熔冻次数的变化曲线图；Fig. 5 is a graph showing the variation of the phase transition point of the phase change material according to the number of times of thawing in Example 1 of the present invention;
图6-1是实施例1相变材料第一次冷凝过程中利用数据采集系统记录并处理的温度与时间关系曲线图；Fig. 6-1 is the temperature-time relation graph recorded and processed by the data acquisition system during the first condensation process of the phase change material in Example 1;
图6-2是实施例1相变材料在第50次冷凝过程中得到的温度与时间关系曲线图。Fig. 6-2 is a graph showing the relationship between temperature and time obtained during the 50th condensation of the phase change material in Example 1.
具体实施方式Detailed ways
本发明设计的连续测定相变材料寿命的方法(参见图3和4)是：将待测相变材料放入熔冻实验池1中，利用与之相连的冷液和热液两组液流循环装置21和22对其进行连续多次熔冻实验；冷液和热液两组液流循环装置21、22分别由各自公知的液流输送设备及流量计量设备构成；冷液和热液两组液流循环装置21、22和与其相连的低、高温恒温浴槽51、52共同构成了熔冻实验自动循环熔冻系统；在实验过程中，利用温度测量装置3从与之相连接的熔冻实验池1中连续检测相变材料温度变化数据，并将该采集数据同时分别送给与之相连的数据采集装置4和温控开关装置6，由后者对冷液和热液两组液流循环装置51、52根据设定工艺条件进行自动切换，而由前者记录并计算出相变材料温度随时间的变化数值和绘制出该全程的变化曲线，包括进而依此确定相变材料的相变点及相变热的相对大小的冷凝过程的曲线，即测定出相变材料的寿命。The method (referring to Fig. 3 and 4) of the continuous measurement life-span of the phase-change material designed by the present invention is: put the phase-change material to be measured in the thawing test pool 1, utilize the two groups of liquid flows of cold liquid and hot liquid connected with it The circulators 21 and 22 carry out multiple continuous thawing experiments; the two groups of liquid flow circulation devices 21 and 22 for cold liquid and hot liquid are respectively composed of known liquid flow conveying equipment and flow metering equipment; the two groups of cold liquid and hot liquid A group of liquid flow circulation devices 21, 22 and the low and high temperature constant temperature baths 51, 52 connected thereto constitute the automatic circulation thawing system of the thawing experiment; The temperature change data of the phase change material is continuously detected in the experimental pool 1, and the collected data are sent to the data acquisition device 4 and the temperature control switch device 6 connected to it at the same time, and the latter controls the flow of the two groups of cold liquid and hot liquid. The circulators 51 and 52 automatically switch according to the set process conditions, and the former records and calculates the change value of the temperature of the phase change material with time and draws the change curve of the whole process, including determining the phase change of the phase change material accordingly. The curve of the condensation process of the point and the relative size of the phase change heat can determine the life of the phase change material.
本发明的连续测定原理(参见图1-1、1-2、2-1和2-2)是基于发明人以下研究成果：相变材料的熔点及相变潜热变化的相对大小，是由相变材料在冷凝过程中温度随时间变化曲线(参见图2-1)确定的。在恒定冷源下，液态相变材料从时间t1进行降温处理；在相变发生前，降温曲线可看作一直线；当有相变发生时，降温曲线出现转折点(即图2-1上的t2，Tm点)；当完全实现相转换时，降温曲线出现第二个转折点(t3，T3点)。假设材料没有相变发生，那么在t2-t3时间内，其降温曲线应当沿t1-t2时间内降温曲线的延长线(图2-1中虚线部分)发展，仍呈线性变化，但在实际过程中，由于相变的发生，降温曲线发生了转折。设在时间t2-t3相变期间内，相变材料实际降温与假想无相变降温的温差为ΔT，根据热力学状态函数与过程无关的原则，可以得到：Hm0＝mcpΔT0，Hmi＝mcpΔTi；所以η＝Hmi/Hm0＝ΔTi/ΔT0，其中，m为熔冻实验池中相变材料的质量；Hm0、Hmi分别为相变材料初始及经过i次熔冻实验后的相变潜热；cp为相变材料液态时的恒压热容。当保持多次冷凝环境温度相同时，则可将所述的相变时间内的降温曲线直线化(参见图2-1，2-2)，其表达式为η＝Hmi/Hm0＝Δti/Δt0＝(t3i-t2i)/(t30-t20)。因此，本发明方法可以根据相变材料在冷凝过程中温度随时间变化的曲线来连续测定其寿命。The continuous measurement principle of the present invention (referring to Fig. 1-1, 1-2, 2-1 and 2-2) is based on the inventor's following research results: the melting point of the phase change material and the relative size of the phase change latent heat change are determined by the phase It is determined by the temperature change curve (see Figure 2-1) of the variable material during the condensation process. Under a constant cold source, the liquid phase change material is cooled from time t 1 ; before the phase change occurs, the cooling curve can be regarded as a straight line; t 2 , T m point); when the phase transition is fully realized, the cooling curve appears a second turning point (t 3 , T 3 point). Assuming that there is no phase change in the material, then during the time t 2 -t 3 , its cooling curve should develop along the extension line of the cooling curve during the time t 1 -t 2 (the dotted line in Figure 2-1), and it still changes linearly. But in the actual process, due to the occurrence of phase transition, the cooling curve has a turning point. Assuming that during the time t 2 -t 3 phase change period, the temperature difference between the actual cooling of the phase change material and the hypothetical cooling without phase change is ΔT, according to the principle that the thermodynamic state function has nothing to do with the process, it can be obtained: H m0 = mc p ΔT 0 , H mi ＝mc p ΔT i ; so η＝H mi /H m0 ＝ΔT i /ΔT 0 , where m is the mass of the phase change material in the freezing test pool; H m0 and H mi are the initial and The latent heat of phase change after i times of thawing experiments; c p is the constant pressure heat capacity of the phase change material in liquid state. When the ambient temperature of multiple condensations is kept the same, the cooling curve within the phase transition time can be linearized (see Figure 2-1, 2-2), and its expression is η=H mi /H m0 =Δt i /Δt 0 =(t 3i -t 2i )/(t 30 -t 20 ). Therefore, the method of the present invention can continuously measure the lifetime of the phase change material according to the curve of the temperature changing with time during the condensation process.
本发明测定相变材料寿命方法的原理如图2所示(参见图2-1、2-2)。其中图2-1是相变材料在第一次冷凝过程中利用数据采集系统记录并处理的温度与时间关系曲线图；图2-2是相变材料在第i次冷凝过程中得到的温度与时间关系图。根据两曲线图中ΔT的不同数值，便可得到相变材料相变热的衰变率。The principle of the method for measuring the lifetime of phase change materials in the present invention is shown in Figure 2 (see Figures 2-1 and 2-2). Among them, Fig. 2-1 is the curve diagram of the temperature and time relationship recorded and processed by the data acquisition system in the first condensation process of the phase change material; Fig. 2-2 is the temperature and the Time graph. According to the different values of ΔT in the two graphs, the decay rate of the phase change heat of the phase change material can be obtained.
本发明连续测定相变材料寿命的测量装置(参见图3和4)主要包含承载被测相变材料的熔冻实验池装置1，与之相连可连续多次对相变材料进行熔冻实验的两组液流循环装置2；两组液流循环装置2中，一组是低温液流循环装置21，其与低温恒温浴槽51相连接；另一组是高温液流循环装置22，其与高温恒温浴槽52相连接，并且所述的低温液流循环装置21和高温液流循环装置22分别与可切换其输送设备起闭的温控开关装置6(以下简称温控开关6)相连接，温控开关6还与温度测量装置3相连接；所述的温控开关6可以进行温度设定，当输入温度信号高于温度的设定上限，温控开关6呈长闭状态；当输入温度信号低于温度的设定下限，温控开关6呈长开状态；所述的温度测量装置3分别与所述的熔冻实验池装置1和数据采集装置4相连接。所述的低温及高温恒温浴槽装置51、52用于储存加热或冷却相变材料的液流介质以进行熔冻实验；所述的低温及高温液流循环装置21、22用于进行相变材料加热或冷冻测定实验的液流循环流动；所述的温度测量装置3用于测定相变材料在整个测定期间温度变化的即时检测；所述的数据采集装置4用于采集并记录相变材料在整个连续熔冻测定实验期间内温度随时间的变化；所述的温控开关6用于控制对相变材料熔化或者冷冻测定实验的转换，即进行所述的低温及高温液流循环装置21、22的自动切换。The measuring device (see Figures 3 and 4) of the present invention for continuously measuring the life of a phase change material mainly includes a thawing test pool device 1 carrying the phase change material to be measured, which is connected to it and can carry out thawing experiments on the phase change material for multiple times continuously. Two groups of liquid flow circulation devices 2; in the two groups of liquid flow circulation devices 2, one group is a low temperature liquid flow circulation device 21, which is connected with a low temperature constant temperature bath 51; the other group is a high temperature liquid flow circulation device 22, which is connected to a high temperature The constant temperature bath 52 is connected, and the low-temperature liquid flow circulation device 21 and the high-temperature liquid flow circulation device 22 are respectively connected with the temperature control switch device 6 (hereinafter referred to as the temperature control switch 6 ) which can switch the on and off of the conveying equipment. The control switch 6 is also connected with the temperature measuring device 3; the temperature control switch 6 can be used for temperature setting, and when the input temperature signal is higher than the set upper limit of the temperature, the temperature control switch 6 is in a long-closed state; when the input temperature signal Below the set lower limit of the temperature, the temperature control switch 6 is in a long-open state; the temperature measuring device 3 is respectively connected with the thawing experimental pool device 1 and the data acquisition device 4 . The low-temperature and high-temperature constant temperature bath devices 51, 52 are used to store the liquid flow medium for heating or cooling the phase-change material for freezing experiments; the low-temperature and high-temperature liquid flow circulation devices 21, 22 are used to conduct phase change material The liquid flow circulation of the heating or freezing measurement experiment; the temperature measurement device 3 is used to measure the instant detection of the temperature change of the phase change material during the whole measurement period; the data acquisition device 4 is used to collect and record the temperature change of the phase change material The temperature changes with time during the whole continuous thawing test period; the temperature control switch 6 is used to control the conversion of the phase change material melting or freezing test experiment, that is, the low temperature and high temperature liquid flow circulation device 21, 22 automatic switching.
图3是本发明相变材料寿命测量装置一种实施例结构原理框图。其中，熔冻实验池装置1作为承载实验测定相变材料的主体部分，内部插有用于测定温度的感温仪器铂电阻温度计；铂电阻温度计测定的信号通过温度测量装置3，向两个方向传送，一是传到数据采集装置4进行数据储存；二是传到温控开关装置6进行输送设备的自动开启与关闭，达到冷热循环系统的自动切换，当测定温度高于温控开关装置6设定的上限温度(如Tm+10℃)时，将发出电信号给冷循环系统中的输送设备，冷循环系统被开启，相变材料处于降温凝固阶段，同时相变系统温度降低；当测定温度低于温控开关装置6设定的下限温度(如Tm-10℃)时，冷循环系统中的输送设备停止运转，冷循环系统关闭，外套管C(参见图4)中的冷液会自动回流到低温恒温浴槽51，同时，热循环系统中输送设备开始运转，热循环系统被开启，相变系统温度开始增高，相变体系进入熔化阶段；当测定温度再次高于设定温度(Tm+10℃)时，冷循环系统自动开启，热循环系统同时自动关闭，同时，内套管B(参见图4)中的热液会自动回流到高温恒温浴槽52，相变材料又处于降温凝固阶段。感温仪器时时感受温度，并发出信号，相变材料便可实现多次熔冻实验。在实验进行之时，通过事先调节设定高温及低温恒温浴槽52、51中液体的温度值，将相变材料的升、降温速率控制在2-5℃/min。Fig. 3 is a schematic block diagram of an embodiment of the phase change material life measuring device of the present invention. Wherein, the thawing test pool device 1 is used as the main part of carrying experiment to measure the phase change material, and the temperature sensing instrument platinum resistance thermometer for measuring temperature is inserted inside; the signal measured by the platinum resistance thermometer is transmitted to two directions through the temperature measuring device 3 , one is transmitted to the data acquisition device 4 for data storage; the other is transmitted to the temperature control switch device 6 for automatic opening and closing of the conveying equipment, to achieve automatic switching of the cold and heat cycle system, when the measured temperature is higher than the temperature control switch device 6 When the upper limit temperature is set (such as T m +10°C), an electrical signal will be sent to the conveying equipment in the cold cycle system, the cold cycle system will be turned on, the phase change material will be in the cooling and solidification stage, and the temperature of the phase change system will decrease at the same time; When the measured temperature is lower than the lower limit temperature (such as Tm -10°C) set by the temperature control switch device 6, the conveying equipment in the cold circulation system stops running, the cold circulation system is closed, and the cooling in the outer casing C (see Figure 4) The liquid will automatically return to the low-temperature constant temperature bath 51. At the same time, the conveying equipment in the thermal cycle system starts to operate, the thermal cycle system is turned on, the temperature of the phase change system begins to increase, and the phase change system enters the melting stage; when the measured temperature is higher than the set temperature again (T m +10 ℃), the cold circulation system is automatically turned on, and the heat circulation system is automatically closed at the same time. At the same time, the hot liquid in the inner sleeve B (see Figure 4) will automatically return to the high temperature constant temperature bath 52, and the phase change material In the stage of cooling and solidification. The temperature-sensing instrument senses the temperature all the time and sends out a signal, and the phase-change material can realize multiple thawing experiments. During the experiment, the temperature rise and fall rate of the phase change material was controlled at 2-5° C./min by adjusting and setting the temperature values of the liquids in the high temperature and low temperature constant temperature baths 52 and 51 in advance.
图4是本发明连续测定相变材料寿命装置与图3所述的方法结构原理对应的一种实施例结构示意图。其特征是承载被测相变材料的熔冻实验池装置1包含(参见图4)：放置相变材料的结晶玻璃管A及其两个密闭但开有液流进出口的内套管B和外套管C；所述的结晶玻璃管A长度为150-200mm，外径25mm，壁厚2mm；结晶玻璃管A外的对相变材料进行液浴加热的内套管B，同时兼做结晶玻璃管A的保护套管，玻璃制，长度为130-180mm，内径45mm，壁厚2mm，其热液进口位于内套管B(保护套管，下同)的底部a位置，出口位于内套管的顶部b位置；内套管B外的对相变材料进行液浴冷却的外套管C，也是玻璃制，高度为200-250mm，内、外套管B、C之间的夹层厚度30mm，其冷液进口位于外套管C底部的c位置，出口位于外套管C的顶部d位置；所述内套管B的进液口a穿过所述的外套管C。尽管所述的实施例已经给出了具体的数据值，但本发明并不受实施例所给出的数值限定。低温恒温浴槽装置D(图3中的51)及高温恒温浴槽装置E(图3中的52)是一种公知的超级恒温器装置；液流循环装置包含冷液或低温液流循环装置和热液高温液流循环装置。两个液流循环系统的线路相互闭锁，即当一路液流循环系统开启时，另一路液流循环系统则关闭；两路液流循环系统分别包括各自的输送设备K、L和流量计量设备(如旋转流量计)；温度测量装置F(图3中的3)包含公知的铂电阻温度计G，用以测定相变材料在整个实验测定期间温度的变化；数据采集装置H(图3中的4)也是现有技术，它可以自动记录来自测温装置F的数据信号；公知的温控开关I(图3中的6)的作用是当测定温度高于其设定的上限温度(如Tm+10℃)时，将发出电信号给冷循环系统中的输送设备，开启冷循环系统；当测定温度低于其设定的下限温度(如Tm-10℃)时，冷循环系统关闭，热循环系统开启，即自动循环熔冻系统可以接收来自温控开关I的信号，并执行相应的动作；同时，温控开关I也受到温度测量装置F的控制。所述的温度上下限温度值的设定取决于被测定材料的性质。当热液循环系统关闭后，内套管B中的热液将自动回流到高温恒温浴槽E中；同样道理，当冷液循环系统关闭时，外套管C中的冷液将自动回流到低温恒温浴槽D中。J为熔冻实验池装置1的支架，它应当使熔冻实验池装置1的水平高度高于所述的冷、热浴槽D、E的高度，以有利于循环装置关闭后，内、外套管B、C中的液流能够靠重力自动顺利回流到所述的冷、热浴槽D、E内。在实验进行之时，通过事先调节设定的高温及低温恒温浴槽中液体的温度值，将相变材料的升、降温速率控制在2-5℃/min。如果升、降温速率太快，相变材料的相变过程将会过快，使相变不完全；而如果升、降温速率太慢，将会使实验时间过长，不利于实验的连续测定。Fig. 4 is a schematic structural diagram of an embodiment of the device for continuously measuring the life of a phase change material of the present invention corresponding to the structural principle of the method described in Fig. 3 . It is characterized in that the thawing experimental pool device 1 carrying the phase change material to be tested includes (see Figure 4): a crystallized glass tube A for placing the phase change material and two inner sleeves B that are closed but have a liquid flow inlet and outlet and The outer sleeve C; the length of the crystallized glass tube A is 150-200mm, the outer diameter is 25mm, and the wall thickness is 2mm; the inner sleeve B outside the crystallized glass tube A is used for liquid bath heating of the phase change material, and also serves as a crystallized glass The protective sleeve of tube A, made of glass, has a length of 130-180mm, an inner diameter of 45mm, and a wall thickness of 2mm. The inlet of the hot liquid is located at the bottom a of the inner sleeve B (protective sleeve, the same below), and the outlet is located at the inner sleeve. position b at the top of the top; the outer sleeve C outside the inner sleeve B that cools the phase change material in a liquid bath is also made of glass with a height of 200-250mm, and the thickness of the interlayer between the inner and outer sleeves B and C is 30mm. The liquid inlet is located at position c at the bottom of the outer sleeve C, and the outlet is located at position d at the top of the outer sleeve C; the liquid inlet a of the inner sleeve B passes through the outer sleeve C. Although specific data values have been given in the described examples, the present invention is not limited by the numerical values given in the examples. Low temperature constant temperature bath device D (51 among Fig. 3) and high temperature constant temperature bath device E (52 among Fig. 3) are a kind of known super thermostat device; Liquid high temperature liquid circulation device. The lines of the two liquid flow circulation systems are mutually locked, that is, when one liquid flow circulation system is opened, the other liquid flow circulation system is closed; the two liquid flow circulation systems respectively include their own conveying equipment K, L and flow metering equipment ( Such as rotameter); Temperature measuring device F (3 among Fig. 3) comprises known platinum resistance thermometer G, in order to measure the change of temperature of phase change material during whole experimental determination; Data acquisition device H (4 among Fig. 3 ) is also a prior art, it can automatically record the data signal from the temperature measuring device F; the effect of the known temperature control switch 1 (6 among Fig. +10°C), an electric signal will be sent to the conveying equipment in the cold cycle system to start the cold cycle system; when the measured temperature is lower than its set lower limit temperature (such as T m -10°C), the cold cycle system will be closed, The thermal cycle system is turned on, that is, the automatic cycle thawing system can receive the signal from the temperature control switch I and perform corresponding actions; at the same time, the temperature control switch I is also controlled by the temperature measuring device F. The setting of the upper and lower temperature limits depends on the properties of the material to be measured. When the hot liquid circulation system is closed, the hot liquid in the inner sleeve B will automatically return to the high temperature constant temperature bath E; similarly, when the cold liquid circulation system is closed, the cold liquid in the outer sleeve C will automatically return to the low temperature constant temperature in bath D. J is the support of the thawing test tank device 1, which should make the horizontal height of the thawing test tank device 1 higher than the height of the cold and hot baths D and E, so that after the circulation device is closed, the inner and outer casings The liquid flows in B and C can automatically and smoothly flow back into the cold and hot baths D and E by gravity. When the experiment is carried out, the temperature rise and fall rate of the phase change material is controlled at 2-5°C/min by adjusting the temperature values of the liquid in the high temperature and low temperature constant temperature baths set in advance. If the heating and cooling rate is too fast, the phase change process of the phase change material will be too fast, making the phase change incomplete; and if the heating and cooling rate is too slow, the experiment time will be too long, which is not conducive to the continuous measurement of the experiment.
利用本发明方法和装置测定相变材料寿命的过程如下：已知该相变材料的相变点为Tm，首先调节高、低温恒温浴槽E、D的温度分别为Tm+15℃、Tm-15℃，并将温控开关装置I的温度上限设定为Tm+10℃，下限为Tm-10℃，然后将一定量(一般可选30g)的相变材料升温至Tm+15后，置于结晶玻璃管A中，其内的铂电阻温度计G将测量出其温度。由于此时相变材料的温度高于温控开关装置I的设定上限温度，冷液循环系统中的输送设备K被开启，并通过调节流量计大小来控制冷液的流量。此时，外套管C中充满冷流体，相变体系进入凝固阶段；由于冷凝作用，相变体系的温度将逐渐下降，直到相变体系的温度下降到温控开关装置I的设定下限温度，冷、热循环系统自动切换，即冷液循环系统中的输送设备K被关闭，热液循环系统的输送设备L开始运行。此时，外套管C中的冷流体依靠重力回流到低温恒温浴槽D中，而内套管B中逐渐充满热流体，相变体系开始进入熔化阶段。当温度再次上升到Tm+10℃时，输送设备K开启，而L关闭，相变体系开始进入下一个冻、熔过程。在整个实验过程中相变体系的温度变化通过铂电阻温度计G测定并由数据采集装置H进行记录和储存，并且全部测定实验过程是连续进行的。最后，根据相变材料在全部冷凝过程中的温度随时间变化曲线，利用所述的公式可确定出该相变材料的寿命。The process of utilizing the method and device of the present invention to measure the lifetime of phase change materials is as follows: the phase change point of the phase change material is known to be T m , first adjust the temperatures of the high and low temperature constant temperature baths E and D to be T m +15° C., T m respectively. m -15°C, and set the temperature upper limit of the temperature control switch device I as T m +10°C, and the lower limit as T m -10°C, and then raise the temperature of a certain amount (generally 30g) of phase change material to T m After +15, put it in the crystallized glass tube A, and the platinum resistance thermometer G inside it will measure its temperature. Since the temperature of the phase change material is higher than the set upper limit temperature of the temperature control switch device 1, the delivery device K in the cold liquid circulation system is opened, and the flow of the cold liquid is controlled by adjusting the size of the flowmeter. At this time, the outer sleeve C is filled with cold fluid, and the phase change system enters the solidification stage; due to condensation, the temperature of the phase change system will gradually decrease until the temperature of the phase change system drops to the lower limit temperature of the temperature control switch device 1, The cooling and heating circulation systems are automatically switched, that is, the conveying equipment K in the cold liquid circulation system is closed, and the conveying equipment L in the hot liquid circulation system starts to run. At this time, the cold fluid in the outer casing C flows back into the low-temperature constant temperature bath D by gravity, while the inner casing B is gradually filled with hot fluid, and the phase change system begins to enter the melting stage. When the temperature rises to Tm+10℃ again, the conveying device K is turned on and L is turned off, and the phase change system begins to enter the next freezing and melting process. During the whole experiment process, the temperature change of the phase change system is measured by the platinum resistance thermometer G and recorded and stored by the data acquisition device H, and the whole measurement experiment process is carried out continuously. Finally, according to the time-varying curve of the temperature of the phase-change material during the entire condensation process, the lifespan of the phase-change material can be determined by using the formula.
下面给出一个具体的实施例：A specific embodiment is given below:
寿命测定实验的相变材料配方为：相变工质材料芒硝85％，填充物海泡石9％，增稠剂海藻酸钠2％，晶型调节剂六偏磷酸钠1％，成核剂硼砂3％。The phase change material formula for the life measurement experiment is: 85% mirabilite as a phase change working substance, 9% sepiolite as a filler, 2% sodium alginate as a thickener, 1% sodium hexametaphosphate as a crystal form regulator, and 1% as a nucleating agent Borax 3%.
已知该相变材料的初始相变点为32.0℃。首先调节高、低温恒温浴槽E、D(这里选用超级恒温水浴槽)中水溶液的温度分别为47.0℃和17℃，并将温控开关装置I的温度上限设定为42℃，下限为22℃，然后将30g的相变材料升温至47.0℃后，置于玻璃管结晶A中，所述的铂电阻温度计G测量出其温度高于温控开关装置I的设定上限温度，将信号传递给温控开关I，进而指令冷液循环系统中的输送设备离心泵K开启，并通过调节流量计大小来控制水流的流量。此时，外套管C中充满冷液，相变体系进入凝固阶段；由于冷凝作用，相变体系的温度将逐渐下降，直到体系的温度下降到温控开关装置I的设定下限温度22℃，冷、热循环系统自动切换，即离心泵K被关闭，热液循环系统的输送设备离心泵L开始运行。此时，外套管C中的水流依靠重力回流到低温恒温浴槽D内；内套管B中充满热液，相变体系开始进入熔化阶段，当温度再次上升到42℃时，离心泵K开启，而L关闭，相变体系开始进入下一个冻、熔实验测定过程。在实验过程中，相变材料的升、降温速率控制在2℃/min。在实验过程中，相变体系的温度变化通过铂电阻温度计测定并由数据采集装置H进行记录和储存，例如，图6-1就绘出了该相变材料第一次冷凝过程中利用数据采集系统记录并处理的温度与时间关系曲线图；图6-2是该相变材料在第50次冷凝过程中得到的温度与时间关系曲线图，并且全部测定实验过程(即第1次到第50次)是连续进行的，图5则给出了此相变材料的相变点随熔冻次数的变化曲线图。该图说明了经历50次熔冻实验后，此相变体系的相变点没有发生漂移，同时也反应出此相变体系具有较好的抗衰老性。It is known that the initial phase transition point of this phase change material is 32.0°C. First adjust the temperature of the aqueous solution in the high and low temperature constant temperature baths E and D (here the super constant temperature water bath is selected) to 47.0°C and 17°C respectively, and set the temperature upper limit of the temperature control switch device I to 42°C and the lower limit to 22°C , and then 30g of the phase change material is heated to 47.0°C, and placed in the glass tube crystal A, the platinum resistance thermometer G measures its temperature higher than the set upper limit temperature of the temperature control switch device I, and transmits the signal to The temperature control switch I further instructs the delivery equipment centrifugal pump K in the cold liquid circulation system to turn on, and controls the flow of water by adjusting the size of the flow meter. At this time, the outer sleeve C is filled with cold liquid, and the phase change system enters the solidification stage; due to condensation, the temperature of the phase change system will gradually decrease until the temperature of the system drops to 22° C., the lower limit temperature of the temperature control switch device 1. The cooling and heating circulation systems are switched automatically, that is, the centrifugal pump K is turned off, and the centrifugal pump L, the conveying equipment of the thermal liquid circulation system, starts to run. At this time, the water flow in the outer sleeve C flows back into the low-temperature constant temperature bath D by gravity; the inner sleeve B is filled with hot liquid, and the phase change system begins to enter the melting stage. When the temperature rises to 42°C again, the centrifugal pump K is turned on. When L is closed, the phase change system begins to enter the next freezing and melting experiment measurement process. During the experiment, the heating and cooling rate of the phase change material was controlled at 2°C/min. During the experiment, the temperature change of the phase change system is measured by the platinum resistance thermometer and recorded and stored by the data acquisition device H. The temperature and time curve graph recorded and processed by the system; Figure 6-2 is the temperature and time curve graph obtained during the 50th condensation process of the phase change material, and the entire measurement experiment process (that is, the 1st to the 50th times) is carried out continuously, and Figure 5 shows the change curve of the phase change point of the phase change material with the number of times of thawing. This figure shows that after 50 times of freezing experiments, the phase change point of this phase change system has not drifted, and it also reflects that this phase change system has good anti-aging properties.
最后，根据相变材料在50次冷凝过程中的温度随时间变化曲线，利用所述的公式可确定出该相变材料的寿命：即根据图6-1，6-2两个曲线图中的关键值ΔT的不同数值，便可计算得到该相变材料相变热的衰变率为，η＝Hmi/Hm0＝ΔTi/ΔT0＝[29.0-(-14.4)]/[29.3-(-31.3)]＝71.6％。这种计算可以通过计算机或计算器简单完成。Finally, according to the temperature change curve of the phase change material with time during the 50 times of condensation, the life of the phase change material can be determined by using the formula: With different values of the key value ΔT, the decay rate of the phase change heat of the phase change material can be calculated, η=H mi /H m0 =ΔT i /ΔT 0 =[29.0-(-14.4)]/[29.3-( -31.3)] = 71.6%. This calculation can be done simply by computer or calculator.
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