Summary of the invention
The thermal performance test Apparatus and method for that the purpose of this invention is to provide a kind of phase-change temperature regulation building material, latent heat of phase change and the phase transition temperature that can test the large scale phase-change temperature regulation building material simultaneously.
The thermal performance of phase-change temperature regulation building material testing apparatus that the present invention proposes, comprise test subject, the heating arrangement and the electronic balance that are used with test subject, described test subject is made up of insulation can, sample receiver, a plurality of thermopair, recording instrument without paper and computer etc., water is housed in the insulation can, sample receiver is immersed in the water, and a plurality of thermopairs are loaded on respectively in sample receiver and the water, and the lead of thermopair is connected with computer with insulation can recording instrument without paper outward respectively.
Wherein, described insulation can is that a sealing that has loam cake is incubated casing, and the casing of insulation can comprises three parts: cladding material is that high density polyethylene, intermediate layer material are that the one-body molded foaming of polyurethane, inner layer material are impact resistant polystyrene; The bottom of insulation can is provided with the dewatering outlet.
Wherein, fill testing sample and sealing in the described sample receiver, its volume 〉=0.03m
3Container is made by the material that readily conducts heat.
Wherein, in the described thermopair three layout be located at the testing sample in the sample receiver the outside to the centre position, be located in the water for two; Thermopair adopts Pt100, and precision is 0.1 ℃.
Wherein, described recording instrument without paper has at least 16 tunnel input/output port, and has logging interval from 10 seconds to 1 hour selection shelves.
Wherein, heating arrangement is used to finish the heating of experiment water and the heating of sample receiver, can be the water bath with thermostatic control heating arrangement of adjustable temperature; Electronic balance is used for weighing and is loaded on the quality of testing sample of sample receiver or the quality of water, and the precision of electronic balance is more than 0.1g
Another purpose of the present invention provides a kind of thermal performance test method at phase-change temperature regulation building material.
Thermal performance of phase-change temperature regulation building material method of testing of the present invention is to utilize aforesaid testing apparatus to finish.Concrete, phase transition temperature scope T in the thermal behavior
1~T
2Mensuration may further comprise the steps:
1) sample is prepared: (sample of granularity≤3mm) is packed in the sample receiver and is filled, and thermopair is installed, the seal sample container with liquid or graininess; At laboratory temperature T
0Under kept 24 hours, take by weighing the quality m of sample;
2) hot water is prepared: get pure water 10L, with heating arrangement water is heated to more than 80 ℃, be poured into then in the insulation can, cover the insulation can case lid;
3) adding of sample: hot water added after 3 hours, opened the insulation can case lid, rapidly ready sample receiver was put into the water of insulation can, covered case lid, and the water temperature that obtains by thermopair in the water is recorded as T
h
4) record of finishing temperature:, after the temperature of the temperature of sample in the insulation can and hot water is consistent, be recorded as T by thermopair record temperature variation
4
Boiler through after the same time, writes down the temperature T that hot water drops under no sample receiver adding situation
5
5) calculating of phase transition temperature: computer changes according to the water and the sample temperature of recording instrument without paper record, draws water and sample temperature change curve; The phase transition temperature T of sample
1, T
2The position determine by the tangent line joining of the heating curve temperature flex point both sides curve of sample, determine the phase transition temperature scope T of sample thus
1~T
2
Further, the mensuration of sample specific heat capacity c further may further comprise the steps:
6) set a temperature value T
3, T
3Be greater than T
2But be less than 50 ℃, preferably near T
2And carry out following operation:
(1) sample receiver is put into water bath with thermostatic control and be heated to T
3To temperature constant;
(2) constant temperature is to T
3Sample receiver be reentered into set by step 2) and 3) in the insulation can prepared;
(3) after the temperature of the temperature of sample in the insulation can and hot water is consistent, be recorded as T
4'; Kept again 3 hours, and took out subsequently under the sample receiver room temperature and lower the temperature; Take by weighing the quality of hot water in the insulation can in addition with electronic balance, be recorded as m
1
(4) boiler of step (3) through after the same time, writes down the temperature T that hot water drops under no sample receiver adding situation
5';
7) calculate the sample specific heat capacity by following formula
(formula 2).
By above test and calculating, sample latent heat of phase change H
mMensuration further comprise following calculating:
Q=4.2 * m
1(T
5-T
4) (formula 1)
(formula 3).
The present invention compares with traditional phase-change material method of testing has following advantage:
1) can be simultaneously qualitative and test out the latent heat of phase change and the phase transition temperature scope of phase transformation building materials quantitatively.
2) but the bigger phase-change material of test size and can be tested the process that the inner phase transformation of phase transformation building materials takes place, help to study the phase-change mechanism of phase transformation building materials.
3) the testing apparatus manufacturing cost is well below DSC equipment.
4) method of testing is simple, need not the complicated operations process.
Embodiment:
The thermal performance of phase-change temperature regulation building material test macro that the present invention proposes, comprise testing apparatus and method of testing, the latent heat of phase change that the principle of utilizing the thermal discharge of hot water in the heat-insulation system to equal the caloric receptivity of phase transformation building materials and heat-insulation system heat dissipation capacity summation is calculated the phase transformation building materials utilizes phase-change material can remain on the phase transition temperature of testing the phase transformation building materials in certain temperature range in phase transition process.This test macro can carry out the test of latent heat of phase change and phase transition temperature simultaneously at large scale phase-change temperature regulation building material sample.Below described in detail.
Testing apparatus constitutes:
Described testing apparatus includes the test subject of being made up of insulation can 4, sample receiver 3, thermopair 1, recording instrument without paper and computer 5 etc. as shown in Figure 1, also has the heating arrangement and the electronic balance that are used with test subject.
In the test subject, insulation can 4 is that a sealing that has loam cake is incubated casing, and water 6 wherein is housed, and the bottom of insulation can 4 also is provided with the dewatering outlet; The casing of insulation can comprises three parts: cladding material is that high density polyethylene, intermediate layer material are that the one-body molded foaming of polyurethane, inner layer material are impact resistant polystyrene;
After filling the testing sample sealing in the sample receiver 3, soak in the water 6 in insulation can 4, for guaranteeing the accuracy of test, sample receiver volume 〉=0.03m
3Container is made by the material that readily conducts heat;
Thermopair 1 is provided with many, wherein three layout be located at the testing sample in the sample receiver 3 the outside to the centre position, be used to obtain the temperature of diverse location sample, lay the temperature that two thermopairs 1 are used to obtain water in the water 6 in addition, thermal resistance adopts Pt100, and precision is 0.1 ℃; All thermopairs 1 and recording instrument without paper and computer 5 are connected by data line, the Temperature numerical that each thermopair 1 is obtained is finished by the recording instrument without paper record and by computer and is analyzed and the experimental data computing, recording instrument without paper requires at least 16 tunnel input/output port, show measurement data in real time, logging interval can many grades of selections from 10 seconds to 1 hour.
External heating arrangement is used to finish the heating of experiment water and the heating of sample receiver in the testing apparatus, can be the water bath with thermostatic control heating arrangement of adjustable temperature; Electronic balance is used for weighing and is loaded on the quality of testing sample of sample receiver or the quality of water, and the precision of electronic balance is more than 0.1g.
Method of testing:
1) environment control
Environment temperature keeps 10~18 ℃ of certain steady state values, is designated as T
0(as Fig. 2), relative humidity≤50%.
2) preparation of sample
Testing sample in the present invention's test should be finished product state, the cumulative volume 〉=0.03m of sample
3If sample is liquid or graininess (granularity≤3mm), test in the sample receiver of can directly packing into; If sample is a shaping thing such as block, tabular, (granularity≤3mm), reinstall in the sample receiver takes by weighing the quality (being designated as m) of sample can be ground into graininess.Sample has been adorned the back and has been loaded 3 thermopairs (as shown in Figure 1) respectively to the middle part in the outside of sample.Covered container covers then, at laboratory temperature (T
0) kept 24 hours down.
3) preparation of hot water
Get pure water 10L, water is heated to more than 80 ℃, be poured into then in the insulation can, cover the insulation can case lid with heating arrangement.
4) adding of sample
Hot water added after 3 hours, opened the insulation can case lid, rapidly ready sample receiver was put into the water of insulation can, covered case lid.The water temperature that obtain by thermopair in the water this moment is recorded as T
h(as Fig. 2), simultaneously, each electric thermo-couple temperature of recording instrument without paper real-time automatic recording changes.
5) record of finishing temperature
After the temperature of the temperature of sample in the insulation can and hot water is consistent, be recorded as T
4(as shown in Figure 2), boiler through after the same time, writes down the temperature T that hot water drops under no sample receiver adding situation
5(drawing practice with Fig. 2 also can obtain similar theoretical temperatures T
5).Kept again 3 hours, and took out sample receiver subsequently and under room temperature, lower the temperature.
6) calculating of phase transition temperature
Computer changes according to the water and the sample temperature of recording instrument without paper record, draws water and sample temperature change curve (referring to Fig. 2),
The phase transition temperature T of sample
1, T
2The position determine the phase transition temperature scope T of sample thus by the tangent line joining of the heating curve temperature flex point both sides curve of sample
1~T
2Can from the heating curve (with reference to Fig. 2) of sample, directly draw.
7) mensuration of sample specific heat capacity
T
2After determining, set a temperature value T
3, T
3Be greater than T
2But be less than 50 ℃, preferably near T
2(as Fig. 2).
(1) sample receiver is put into water bath with thermostatic control and be heated to T
3To temperature constant;
(2) constant temperature is to T
3Sample receiver be reentered into set by step 3) and 4) in the insulation can prepared and carry out the same operation of step 4).
(3) after the temperature of the temperature of sample in the insulation can and hot water is consistent, be recorded as T
4'; Kept again 3 hours, and took out subsequently under the sample receiver room temperature and lower the temperature; Take by weighing the quality of hot water in the insulation can in addition with electronic balance, be recorded as m
1
(4) boiler of step 3) through after the same time, writes down the temperature T that hot water drops under no sample receiver adding situation
5' (drawing practice with Fig. 2 also can obtain similar theoretical temperatures T
5'.
8) calculate the sample latent heat of phase change:
Q=4.2 * m
1(T
5-T
4) (formula 1)
(formula 2)
(formula 3)
In the formula, Q is the caloric receptivity of sample, and unit is kJ/kg.C is the specific heat of sample, H
mLatent heat of phase change for sample.M is the quality of sample.m
1Be the quality of hot water, T
3The initial temperature of sample, T
4The common temperature that test water and sample reach, T
5Add the temperature that fashionable test water drops at the no sample of hypothesis.
Below further specify test process of the present invention with test case.
Example 1: the sample that uses in this example carries out test operation as the compound phase transformation particle of expanded perlite-paraffin organic-inorganic by above-mentioned testing procedure, and concrete numerical value is in the operation:
Environment temperature T in the step 1)
0It is 18 ℃; Step 2) sample particle 0.5-2.0mm in, sample receiver size 0.3m * 0.3m * 0.3m, population of samples is long-pending to be 0.027m
3, quality m is 7.56kg; Step 4) uses the insulation can volume to be 0.53m * 0.32m * 0.32m, the hot water temperature T of record
hBe 65 ℃, the balance finishing temperature T of step 5) record
4Be 43.8 ℃, T
5Be 60.1 ℃, the sample heating curve that step 6) is drawn as shown in Figure 2.Can see that by sample heating curve among Fig. 2 sample has first place's temperature flex point 35 minutes the time after thermometric is approximately put into sample, second place's temperature flex point was arranged in the time of 130 minutes, tangent line joining by every place flex point both sides curve is determined the temperature value that it is corresponding, obtain the phase transition temperature scope of this sample, the phase transition temperature of the compound phase transformation particle of promptly tested organic-inorganic is 26~30 ℃.
The T that step 7) is determined according to Fig. 2
3Be 35 ℃ of temperature, sample receiver is stabilized in again after 35 ℃, substep 3) and 4) definite respectively T
4' be 56.5 ℃, hot water quality m
1Be 10kg, T
5' be 60 ℃.Calculate the latent heat of phase change H of the compound phase transformation particle of sample organic-inorganic by calculating formula (formula 2) and (formula 3)
mBe 67.3kJ/kg.
The compound phase transformation particle of this organic-inorganic is through DSC test (sampling amount 10mg), and drawing its phase transition temperature is 25 ℃, and latent heat of phase change is 64.2kJ/kg.Contrast draws the method for testing error of the present invention's proposition in 5%.Illustrate that the inventive method is feasible.
Example 2: the sample that uses in this example wherein is mixed with 50% the compound phase transformation particle of expanded perlite-paraffin organic-inorganic as the phase-changing and temperature-regulating mortar.Carry out test operation by above-mentioned testing procedure, concrete numerical value is in the operation:
Environment temperature T in the step 1)
0It is 18 ℃; Step 2) sample particle 0.5~2mm in, sample receiver size 0.3m * 0.3m * 0.3m, population of samples is long-pending to be 0.027m
3, quality m is 10.8kg; Step 4) uses the insulation can volume to be 0.53m * 0.32m * 0.32m, the hot water temperature T of record
hBe 65 ℃, the balance finishing temperature T of step 5) record
4Be 45.6 ℃, T
5Be 60.2 ℃, the sample heating curve that step 6) is drawn as shown in Figure 3.Can see that by sample heating curve among Fig. 3 sample has first place's temperature flex point at thermometric in the time of about 43 minutes, second place's temperature flex point was arranged in the time of 98 minutes, tangent line joining by every place flex point both sides curve is determined the temperature value that it is corresponding, obtain the phase transition temperature scope of this sample, the phase transition temperature of promptly tested phase-changing and temperature-regulating mortar material is 26~30 ℃.It is close with example 1 testing result that this detects numerical value.
The T that step 7) is determined according to Fig. 3
3Be 35 ℃ of temperature, after sample receiver is stabilized in 35 ℃ again, by substep 3) and 4) definite respectively T
4' be 53.6 ℃, hot water quality m
1Be 10kg, T
5' be 58 ℃.Calculate the latent heat of phase change H of sample phase-changing and temperature-regulating mortar material thus
mBe 31.6kJ/kg.This theoretical latent heat of phase change 33.65kJ/kg of mortar numerical value that detects numerical value and the reckoning of example 1 testing result is approaching, illustrates that the present invention is suitable for being applied to the phase-changing and temperature-regulating building materials is carried out thermal performance test.
With DSC same phase-transition heat-preserving mortar is tested, pressed the maximum sampling amount 10mg sampling of DSC instrument, do not obtain testing result, illustrate that the DSC detection is unsuitable for testing at phase-changing and temperature-regulating building materials thermal behavior.