CN1462876A - Method for testing stability of tempering composite material by phase change - Google Patents

Method for testing stability of tempering composite material by phase change Download PDF

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Publication number
CN1462876A
CN1462876A CN 03129762 CN03129762A CN1462876A CN 1462876 A CN1462876 A CN 1462876A CN 03129762 CN03129762 CN 03129762 CN 03129762 A CN03129762 A CN 03129762A CN 1462876 A CN1462876 A CN 1462876A
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temperature
changing
phase
compound substance
regulating
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CN1203309C (en
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梁金生
梁广川
梁秀红
吴子钊
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Hebei University of Technology
Hebei Polytechnic University
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Hebei University of Technology
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Abstract

A method for testing the stability of temp-regulating composite phase-change material includes uniformly spreading the composite material with standard weight in a central test area on standard filter paper, baking at 40-50 deg.C for 5-12 hrs, measuring the maximal and minimal diameters of diffused circles, calculating average diameter, comparing it with standard setting to judge its stability. Its advantages are easy operation etc.

Description

The detection method of phase-changing and temperature-regulating compound substance stability
Technical field
The present invention relates to building materials and additives for building materials detection technique, be specially a kind ofly, judge the detection method technology of phase-changing and temperature-regulating compound substance stability by test to phase-changing and temperature-regulating working medium component stripping situation in its product material (being temperature regulation building material).
Background technology
Temperature regulation building material is a kind of New Building Materials.It has according to variation of ambient temperature regulates indoor temperature automatically, saves the energy, improves the characteristics of indoor comfort.Therefore, temperature regulation building material in use can reduce air-conditioning, heating installation service time and air-conditioning and open number of times, and they also help to avoid peak of power consumption work and the translation electricity consumption time, thereby reach energy saving purposes.
The phase-changing and temperature-regulating working material is the main material of temperature regulation building material, comprises inorganics and organism two big classes.Wherein inorganic-phase variable temperature adjustment working material phase transition temperature is suitable, and latent heat of phase change is big, and cost is also lower, and the problem but the general existence of inorganic-phase variable temperature adjustment working material is exosmosed easily, is corrosive etc. is used and is subjected to bigger restriction.Organic phase-change temperature adjustment working material has and did not have cold, steady performance, so the temperature regulation building material of exploitation mainly uses organic phase-change temperature adjustment working material at present, as paraffin alkane, organic alcohol, butyl stearate etc.The preparation temperature regulation building material mainly contains three kinds of methods (referring to document " civil engineering material magazine " (Journal of materials in civil engineering) at present, 1998,5:98-105): (1) directly mixes method, promptly in the building materials preparation process, the phase-change working substance material directly mixed wherein make building materials with phase-changing and temperature-regulating function; (2) infusion process is about to make the building materials with phase-changing and temperature-regulating function in the building materials after the phase-change working substance material infiltrates moulding; (3) microcapsule method, promptly make the microcapsules that contain phase-change material earlier, or the compound composition large capsule of the microcapsules that will contain phase-change material earlier, in the building materials preparation process, mix these microcapsules or large capsule then, make building materials with temperature adjustment function (referring to the method for among the preparation method of microcapsules among the U.S. Pat P4708812 and the USP20020061954 microcapsules being formed large capsule).
All there is to a certain degree the phase-changing and temperature-regulating working material problem of exosmosing with the temperature regulation building material of above three kinds of methods preparation, especially described (1), (2) two kinds of methods, the phase-change working substance material mechanically combines with building materials, it oozes out, the frosting problem is particularly evident, influence the realization of temperature adjustment function, also hinder normal the use; (3) kind method has solved seepage, the frosting problem of phase-changing and temperature-regulating working material to a certain extent, but because frequent solid-liquid phase change of phase-change material causes breathing in the microcapsules, the microcapsules cyst wall will be tired gradually, and the problem of oozing out of phase-change working substance material also can display.At present, many patents are devoted to solve the problem of exosmosing of phase-change working substance material, as: patent documentation CN1327024A has reported the preparation method of a kind of organic phase change material/bentonite nano composite phase change heat-storing building material.It is bumped into organic phase change materials such as erucic acid, certain herbaceous plants with big flowers acid, stearic acid, palmitic acid between bentonitic nanometer layer, thereby reduces the problem of exosmosing of organic phase change material.But the technology of these bibliographical informations all is conceived to the prescription of thermal control material and preparation method to solve the problem of exosmosing of phase-change working substance material, and for the detection of temperature regulation building material product temperature adjusting performance, the exosmose problem of temperature adjustment working material in phase-changing and temperature-regulating compound substance or temperature regulation building material particularly, the detection method technology of phase-changing and temperature-regulating compound substance stability is not seen bibliographical information both at home and abroad as yet in other words conj.or perhaps.The importance of this problem is: the temperature adjusting performance of phase-changing and temperature-regulating compound substance or temperature regulation building material not only depends on the kind and the content of temperature adjustment working material in its prescription, and depends on the stability of temperature adjustment working material in its product.Therefore, the detection method of the suitable phase-changing and temperature-regulating compound substance stability of design is very necessary and important.
Summary of the invention
At the deficiencies in the prior art, the technical matters that the present invention mainly solves just provides a kind of detection method of phase-changing and temperature-regulating compound substance stability.It is simple that it has method, and available conventional equipment detects, and visual result is judged and detected low cost and other advantages easily.
The technical scheme that the present invention solves described detection method technical matters is: the detection method that designs a kind of phase-changing and temperature-regulating compound substance stability, comprise following program: (1) produces sample: the phase-changing and temperature-regulating compound substance of standard weights is dispersed in the phase-changing and temperature-regulating composite material test zone of standard filter paper central authorities, makes sample to be detected; (2) baking sample: sample to be detected is moved on in the baking oven, after 5~12 hours, take out test samples 40~50 ℃ of following constant temperature bakings; (3) observation sample: observe the modify tone situation of oozing out of warm working medium component of phase-changing and temperature-regulating composite material test zone foreign minister on the filter paper, and measure it and ooze out outer formed maximum gauge and the minimum diameter that oozes out circle of test zone, calculate the mean diameter of oozing out circle by maximum gauge and the minimum diameter that oozes out circle again; (4) judge stability:, judge the stability of the phase-changing and temperature-regulating compound substance that detects according to result of calculation and established standards.
Detection method of the present invention has only designed to be produced sample, baking sample, observation sample and judges four programs of stability or step, thus method simple, practical, promote the use of easily; In detection method of the present invention, the baking oven that only needs the use common laboratory all to have, promptly available conventional equipment detects, and not needing increases any equipment and instrument, and the also familiar baking oven that uses of experimenter, and it is very low therefore to detect cost; Because the testing result of described stability is to ooze out the outer formed diameter of oozing out circle of test zone as basic judgment basis by described phase-changing and temperature-regulating working medium component, so visual result, judges easily, also helps popularizing and uses.The positive effect of detection method of the present invention also is; It is not only applicable to the detection of described phase-changing and temperature-regulating compound substance stability, and be applicable to the accumulation of heat of temperature regulation building material heat storage performance and building materials temperature adjustment adjuvant or the detection of temperature adjustment stability, for the quality of judging their service qualities provides technical basis, also the formulation for its standard provides technical support.
Description of drawings
Fig. 1 makes the synoptic diagram of sample to be detected for detection method of the present invention; The phase-changing and temperature-regulating composite material test zone and the interior homodisperse phase-changing and temperature-regulating compound substance thereof of wherein, 1---standard filter paper, 2---standard filter paper central authorities;
Fig. 2 is the synoptic diagram of detection method observation sample of the present invention; Wherein, 3---phase-changing and temperature-regulating working medium component is oozed out the outer formed circle that oozes out of described test zone.
Embodiment
Below in conjunction with embodiment and accompanying drawing thereof detection method of the present invention is done further narration:
The phase-changing and temperature-regulating working medium component of a kind of phase-changing and temperature-regulating compound substance of the present invention's design is oozed out the detection method of stability, comprise four step programs: the first step is to produce sample: the phase-changing and temperature-regulating compound substance that is about to standard weights is dispersed in the phase-changing and temperature-regulating composite material test zone (hereinafter to be referred as the test section) of standard filter paper central authorities, makes sample to be detected.In this step program, the standard weights of described phase-changing and temperature-regulating compound substance is meant needed weight when doing this type of material experiment usually.The phase-changing and temperature-regulating compound substance standard weights of detection method special recommendation of the present invention is meant 0.2g, 0.5g, 1.0g.The size of described standard weights is relevant with the size of the diameter of described test section, also is size and described phase-changing and temperature-regulating compound substance standard weights big or small corresponding of described filter paper central authorities test section diameter.So-called correspondence is meant that both are proportional, promptly when the test section diameter design of filter paper central authorities is big, then needs described phase-changing and temperature-regulating compound substance standard weights bigger.Embodiment described test section diameter and described phase-changing and temperature-regulating compound substance standard weights correspond to 10mm, 20mm or 30mm.When placing the phase-changing and temperature-regulating compound substance of described standard weights in described filter paper central authorities test section, should all cover described test section with the phase-changing and temperature-regulating compound substance, what do not leak filter paper and consistency of thickness evenly is separated into principle.For this reason, the phase-changing and temperature-regulating compound substance particle diameter of embodiment of the invention design is 0.01~100 micron, is preferably 0.1~45 micron.Standard filter paper of the present invention is meant the filter paper of regular size, and the filter paper diameter that embodiment selects for use is φ 70mm, φ 90mm or φ 115mm.It is also corresponding with described phase-changing and temperature-regulating compound substance standard weights.Phase-changing and temperature-regulating compound substance standard weights of the present invention and particle size thereof, the size of filter paper specification and its central test section are not subjected to the restriction of embodiment.
Second step of detection method of the present invention is the baking sample: be about to sample to be detected and move on in the baking oven, after 5~12 hours, take out sample 40~50 ℃ of following constant temperature bakings.In this step program, why setting the constant temperature baking temperature is 40~50 ℃, is because temperature when too high, and the volatility of the phase-changing and temperature-regulating working medium component of phase-changing and temperature-regulating compound substance strengthens, and the quantitative change that causes volatilizing is big, and testing result is on the low side, and it is too little promptly to ooze out circle; Temperature is crossed when hanging down, and phase-changing and temperature-regulating working medium component temperature can not reach fusing fully in the phase-changing and temperature-regulating compound substance, viscosity is low, and testing result is also on the low side.No matter the testing result that the sort of situation causes is on the low side, promptly ooze out circle too hour, bring difficulty all can for next step " observation sample ", also be not easy to measurements and calculations.Why setting constant temperature stoving time scope is 5~12 hours, is for phase-changing and temperature-regulating working medium component fully being undergone phase transition, becoming liquid on the one hand; Be to form the circle that exosmoses on the other hand for unnecessary phase-changing and temperature-regulating working medium component is fully exosmosed.The size of concrete constant temperature stoving time is relevant with the kind and the content of phase-changing and temperature-regulating working medium component.It should also be noted that simultaneously under the prerequisite that guarantees aforementioned two conditions,, should choose the constant temperature stoving time of trying one's best little in order to shorten the time of whole testing process.
The 3rd step of detection method of the present invention is the observation sample: promptly observe the modify tone situation of oozing out of warm working medium component of thermal control material test zone foreign minister on the filter paper, and measure it and ooze out outer formed maximum gauge and the minimum diameter that oozes out circle of test zone, calculate the mean diameter of oozing out circle by maximum gauge and the minimum diameter that oozes out circle again.This coupon results has good intuitive.Measurement phase-changing and temperature-regulating working medium component is oozed out the outer formed diameter of oozing out circle of test zone can adopt multiple instrument, for example ruler, set square, vernier caliper or projector etc.In order to reach relatively accurate measurement result, the instrument that detection method of the present invention recommends to use is vernier caliper.
The 4th step of detection method of the present invention is a stability of judging test material: promptly according to result of calculation and established standards, judge the phase-changing and temperature-regulating working medium component stability of the phase-changing and temperature-regulating compound substance that detects.So-called result of calculation is meant that calculating described the oozing out of sample encloses the percent value that mean diameter exceeds described test zone diameter.So-called established standards is meant described percent value of regulation as boundary value, and stipulates that a series of described percent value are as standard value.The phase-changing and temperature-regulating working medium component stability of the so-called judgement phase-changing and temperature-regulating compound substance that detects is meant with described result of calculation and described established standards and compares that all then thinking of described boundary value that be not higher than do not ooze out or function-stable; Thinking of described boundary value oozes out or instability and be higher than.All stability of then thinking that is not higher than described standard value has reached respective standard, and the stability of thinking that is higher than described standard value has exceeded respective standard.Described established standards is as shown in table 1: (table 1)
Established standards Stable or ooze out boundary value
Do not ooze out Trace oozes out Ooze out on a small quantity Middle amount is oozed out Ooze out in a large number
Number percent (%) ??≤10 ??>10-≤15 >15-≤30 >30-≤50 ??>50
Judge stability Highly stable Stable Basicly stable Unstable Very unstable
Provide specific embodiment below:
Embodiment 1
(1) produces sample: the phase-changing and temperature-regulating compound substance (self-control: the microcapsules that contain the phase-changing and temperature-regulating working material) be dispersed in the diameter 10mm test zone of diameter 70mm filter paper central authorities, make sample to be detected that with the 0.2g mean grain size is 0.1 micron; (2) baking sample: sample to be detected is moved on in the baking oven,, take out sample 40 ℃ of following constant temperature bakings 5 hours; (3) observation sample: observe on the filter paper thermal control material test zone foreign minister situation of oozing out of warm working medium component that modifies tone, and to measure its maximum gauge that oozes out circle be 11.0mm, minimum diameter is 10.6mm, is 10.8mm thereby calculate the mean diameter of oozing out circle; (4) judge stability: calculate that to ooze out the percent value that the circle mean diameter exceeds the test section diameter be 8%.That sets phase-changing and temperature-regulating compound substance stability does not ooze out judgment criteria for not being higher than 10% (referring to table 1, down together), therefore judges this thermal control material for not exosmosing, and promptly the phase-changing and temperature-regulating compound substance is highly stable.
Embodiment 2
(1) produce sample: with the 0.5g mean grain size is the (self-controls: lauryl alcohol-bentonitic clay organic/inorganic phase-changing and temperature-regulating compound substance) be dispersed in the diameter 20mm test zone of diameter 90mm filter paper central authorities, make sample to be detected of 30 microns phase-changing and temperature-regulating compound substances; (2) baking sample: sample to be detected is moved on in the baking oven,, take out sample 45 ℃ of following constant temperature bakings 8 hours; (3) observation sample: observe on the filter paper thermal control material test zone foreign minister situation of oozing out of warm working medium component that modifies tone, and to measure its maximum gauge that oozes out circle be 24.0mm, minimum diameter is 22.0mm, is 23.0mm thereby calculate the mean diameter of oozing out circle; (4) judge stability: calculate that to ooze out the percent value that the circle mean diameter exceeds the test zone diameter be 15%.As set judgment criteria that the phase-changing and temperature-regulating compound substance oozes out for not being higher than 10%, then judge this thermal control material for exosmosing, i.e. phase-changing and temperature-regulating compound substance instability; And as set judgment criteria that temperature adjustment working material trace oozes out for not being higher than 15%, then this thermal control material of decidable is that trace oozes out, promptly the phase-changing and temperature-regulating compound substance is stablized.
Embodiment 3.
(1) produce sample: with the 1.0g mean grain size is the (self-controls: tetradecyl alchohol-bentonitic clay organic/inorganic phase-changing and temperature-regulating compound substance) be dispersed in the diameter 30mm test zone of diameter 115mm filter paper central authorities, make sample to be detected of 40 microns phase-changing and temperature-regulating compound substances; (2) baking sample: sample to be detected is moved on in the baking oven,, take out sample 50 ℃ of following constant temperature bakings 12 hours; (3) observation sample: observe on the filter paper thermal control material test zone foreign minister situation of oozing out of warm working medium component that modifies tone, and to measure its maximum gauge that oozes out circle be 59.0mm, minimum diameter is 47.0mm, is 53.0mm thereby calculate the mean diameter of oozing out circle; (4) judge stability: calculate that to ooze out the percent value that the circle mean diameter exceeds the test section diameter be 76.7%.What kind of no matter takes set phase-changing and temperature-regulating compound substance stability judgment criteria, and this thermal control material all should be judged to be and exosmose, and promptly the phase-changing and temperature-regulating compound substance is very unstable.
Embodiment 4
(1) produces sample: the phase-changing and temperature-regulating compound substance (self-control: lauryl alcohol-sepiolite organic/inorganic phase-transition self-temperature-regulating unit combination thing) be dispersed in the diameter 10mm test zone of diameter 70mm filter paper central authorities, make sample to be detected that with the 0.5g mean grain size is 10 microns; (2) baking sample: sample to be detected is moved on in the baking oven,, take out sample 45 ℃ of following constant temperature bakings 7 hours; (3) observation sample: observe on the filter paper thermal control material test zone foreign minister situation of oozing out of warm working medium component that modifies tone, and to measure its maximum gauge that oozes out circle be 10.5mm, minimum diameter is 10.7mm, is 10.6mm thereby calculate the mean diameter of oozing out circle; (4) judge stability: calculate that to ooze out the percent value that the circle mean diameter exceeds the test zone diameter be 6%.Therefore the judgment criteria of setting phase-changing and temperature-regulating compound substance stability judges this thermal control material for not oozing out for not being higher than 10%, and promptly the phase-changing and temperature-regulating compound substance is highly stable.

Claims (6)

1. the detection method of a phase-changing and temperature-regulating compound substance stability, comprise following program: (1) produces sample: the phase-changing and temperature-regulating compound substance of standard weights is dispersed in the phase-changing and temperature-regulating composite material test zone of standard filter paper central authorities, makes sample to be detected; (2) baking sample: sample to be detected is moved on in the baking oven, after 5~12 hours, take out test samples 40~50 ℃ of following constant temperature bakings; (3) observation sample: observe the modify tone situation of oozing out of warm working medium component of phase-changing and temperature-regulating composite material test zone foreign minister on the filter paper, and measure it and ooze out outer formed maximum gauge and the minimum diameter that oozes out circle of test zone, calculate the mean diameter of oozing out circle by maximum gauge and the minimum diameter that oozes out circle again; (4) judge stability:, judge the stability of the phase-changing and temperature-regulating compound substance that detects according to result of calculation and established standards.
2. the detection method of phase-changing and temperature-regulating compound substance stability according to claim 1, it is characterized in that described phase-changing and temperature-regulating compound substance standard weights is meant 0.2g, 0.5g or 1.0g, described standard filter paper diameter and described phase-changing and temperature-regulating compound substance standard weights correspond to φ 70mm, φ 90mm or φ 115mm, the phase-changing and temperature-regulating composite material test regional diameter and the described phase-changing and temperature-regulating compound substance standard weights of described filter paper central authorities correspond to 10mm, 20mm or 30mm, and the mean grain size of described phase-changing and temperature-regulating compound substance is 0.01~100 micron.
3. the detection method of phase-changing and temperature-regulating compound substance stability according to claim 2, the mean grain size that it is characterized in that described phase-changing and temperature-regulating compound substance is 0.1~45 micron.
4. according to the detection method of claim 1,2 or 3 described phase-changing and temperature-regulating compound substance stability, it is characterized in that described is 5~8 hours at 40~50 ℃ of following constant temperature stoving times.
5. according to the detection method of claim 1,2 or 3 described phase-changing and temperature-regulating compound substance stability, it is characterized in that described established standards is: do not ooze out≤10%, trace oozes out>10%-≤15%, ooze out on a small quantity>15%-≤30%, middle amount oozes out>30%-≤50%, ooze out in a large number>50%.
6. the detection method of phase-changing and temperature-regulating compound substance stability according to claim 4 is characterized in that described established standards is: do not ooze out≤10%, trace oozes out>10%-≤15%, ooze out on a small quantity>15%-≤30%, middle amount oozes out>30%-≤50%, ooze out in a large number>50%.
CN 03129762 2003-05-16 2003-05-16 Method for testing stability of tempering composite material by phase change Expired - Fee Related CN1203309C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101975792A (en) * 2010-09-14 2011-02-16 中国科学技术大学 System for testing stability of solid-liquid phase change materials
CN104964998A (en) * 2015-07-08 2015-10-07 山东祥通橡塑集团有限公司 Burning-resisting experimental method of burning-resisting conveyor belt
CN114062204A (en) * 2021-10-26 2022-02-18 浙江理工大学 Method for detecting migration of phase-change material in heat-storage and temperature-adjustment textile product

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101975792A (en) * 2010-09-14 2011-02-16 中国科学技术大学 System for testing stability of solid-liquid phase change materials
CN101975792B (en) * 2010-09-14 2013-06-26 中国科学技术大学 System for testing stability of solid-liquid phase change materials
CN104964998A (en) * 2015-07-08 2015-10-07 山东祥通橡塑集团有限公司 Burning-resisting experimental method of burning-resisting conveyor belt
CN104964998B (en) * 2015-07-08 2017-07-18 山东祥通橡塑集团有限公司 Burning-resistant conveyor belt is resistance to burn experimental method
CN114062204A (en) * 2021-10-26 2022-02-18 浙江理工大学 Method for detecting migration of phase-change material in heat-storage and temperature-adjustment textile product
CN114062204B (en) * 2021-10-26 2024-03-01 浙江理工大学 Method for detecting migration of phase change material in heat-accumulating temperature-regulating textile product

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