CN107271313A - A kind of method of testing of inorganic phase-changing material modified effect - Google Patents
A kind of method of testing of inorganic phase-changing material modified effect Download PDFInfo
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Abstract
The invention provides a kind of method of testing of inorganic phase-changing material modified effect.The present invention carries out differential thermal analysis and thermogravimetric analysis by the levels solution to inorganic phase-changing material after before modified, according to differential thermal analysis result and thermal gravimetric analysis results calculate respectively inorganic phase-changing material before and after addition thickener be completely melt the corresponding hot-fluid difference of temperature than A, start the corresponding hot-fluid difference of dehydration temperaturre and compare C than B and thermogravimetric analysis point quality difference value；The value that the value of the A is more than 85%, B is more than 70%, and C value be more than 95% when, the thickener of the volume can be effectively improved the lamination of inorganic phase-changing material.The present invention utilizes the uniformity for testing modified inorganic phase-changing material levels material, by the change of the thermodynamic behaviour of inorganic phase-changing material after test before modified, realize to Different adding amount, different types of thickener to the Accurate Determining of inorganic phase-changing material modified effect.
Description
Technical field
The present invention relates to phase change material modified technical field, more particularly to a kind of test of inorganic phase-changing material modified effect
Method.
Background technology
Phase-change material is a kind of material for completing to discharge and absorb hot-cast socket by itself phase transition process, is that one kind has
The material of very strong energy-saving temperature-regulating potentiality.Phase-change material has thousands of kinds, is generally divided into inorganic phase-changing material and organic phase change material, but
Be really be able to apply to building field less than hundred kinds, it is organic phase change material to have quite a few among these.
Organic phase change material in general stablize relatively by performance, there is relatively-stationary freezing point and fusing point, this also means that
Organic phase change material has fixed transformation temperature, but organic phase change material has certain volatility, to the living environment of the mankind
Have a certain impact and endanger, while the fire resistance of organic phase change material is poor, do not possess fire protecting performance, this is mainly and organic
The chemical characteristic of phase-change material is relevant.
Inorganic phase-changing material has preferable fire protecting performance, either metal oxide or crystalline hydrate salt class phase transformation material
Material can resist naked light and high temperature, be a kind of foolproof phase-change material.But compared to the stabilization of organic phase change material
Property, inorganic phase-changing material typically has supercooling and is mutually layered the two problems.By taking crystalline hydrate salt phase-change material as an example, work as phase
When change material is cooled near phase transformation temperature pointses, its phase transition process will not typically start at once, only when temperature is progressively decreased to
When to a certain degree, the phenomenon that phase transition process is just abruptly started to is exactly the surfusion of inorganic hydrated salt class phase transformation material；And be layered
Phenomenon be exactly inorganic hydrated salt class phase transformation material metal salt of itself in melting process can not be dissolved in fusing crystallization it is water-soluble
Phenomenon in liquid.If can effectively eliminate supercooling and phase lamination if can large-scale use inorganic phase-changing material, and
And the fire performance of inorganic phase-changing material can be fully played out.
It is general using nucleator method that supercooling is solved at present, typically by adding some nucleators, so that in temperature-fall period, it is auxiliary
Help inorganic phase-changing material to form nucleus in time, facilitate crystallization；And solve the method that is mutually layered, it is general use add variety classes with
And the method for different amounts of thickener improves.The eradicating efficacy of nucleator improvement supercooling utilizes temperature sensor to remember in general
Recording temperature change and drawing cooling curve intuitively to characterize, but variety classes improves what is be mutually layered with the thickener of volume
The judgement of effect is identified by naked eyes, subjective, the drawbacks of having very big and getting sth into one's head property, without one kind
Objective characterizing method evaluates its improvement.
The content of the invention
It is an object of the invention to provide a kind of method of testing of inorganic phase-changing material modified effect.The survey that the present invention is provided
Method for testing can carry out accurate objectively analysis to inorganic phase-changing material modified effect.
The invention provides a kind of method of testing of inorganic phase-changing material modified effect, comprise the following steps：
(1) inorganic phase-changing material is heated to fusing, obtains stratified liquid；It is each in the upper and lower of the stratified liquid
Partially liq is extracted, and marks sample position；
(2) liquid for extracting the step (1) with lower floor at the middle and upper levels distinguishes decrease temperature crystalline, obtains upper strata sample and lower floor
Sample；
(3) remaining liq after extracting in the step (1) is mixed with the thickener of certain volume, obtains being modified molten
Liquid；
(4) after the mark in the modified solution correspondence step (1) that the step (3) is obtained extracts partially liq respectively
Decrease temperature crystalline, obtains being modified upper strata sample and modified lower floor sample；
(5) the modification upper strata that the upper strata sample and lower floor's sample and the step (4) obtained to the step (2) is obtained
Sample and modified lower floor sample carry out differential thermal analysis and thermogravimetric analysis respectively, obtain differential thermal analysis result and thermal gravimetric analysis results；
(6) temperature correspondence is completely melt before and after addition thickener according to differential thermal analysis result calculating inorganic phase-changing material
Hot-fluid difference compare B with the corresponding hot-fluid difference of dehydration temperaturre is started than A；
The of poor quality of thermogravimetric analysis point of the inorganic phase-changing material before and after addition thickener is calculated according to thermal gravimetric analysis results
Value compares C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1To be completely melt the difference of the heat flow value of the corresponding upper strata sample of temperature and the heat flow value of lower floor's sample；
D2To be completely melt the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of temperature with being modified lower floor's sample
Value；
D3For the difference of the heat flow value and the heat flow value of lower floor's sample that start the corresponding upper strata sample of dehydration temperaturre；
D4To start the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of dehydration temperaturre with being modified lower floor's sample
Value；
M1For the difference of the quality and the quality of lower floor's sample of the corresponding upper strata sample of thermogravimetric analysis point；
M2The difference of the quality of quality and modified lower floor sample for the corresponding modified upper strata sample of thermogravimetric analysis point；
The value that the value of the A is more than 85%, B is more than 70%, and C value be more than 95% when, the volume
Thickener can be effectively improved the lamination of inorganic phase-changing material.
It is preferred that, the inorganic phase-changing material includes crystalline hydrate salt phase-change material.
It is preferred that, the crystalline hydrate salt phase-change material includes Na2SO4·10H2O、CaCl2·6H2O or Na2HPO4·
12H2O。
It is preferred that, the thickener is not expanded at 200~250 DEG C and physical and chemical character is constant.
It is preferred that, the thickener includes super absorbent resin and/or sodium carboxymethylcellulose.
It is preferred that, the volume that the step (1) extracts liquid with lower floor at the middle and upper levels independently is 0.3~0.6mL.
It is preferred that, the speed for the liquid cooling that the step (2) is extracted with lower floor at the middle and upper levels independently is 1~3 DEG C/min.
It is preferred that, the mixing in the step (3) is carried out under agitation；The speed of the stirring is 400~600r/
min；The time of the stirring is 15~25min.
It is preferred that, the volume that the step (4) extracts liquid with lower floor at the middle and upper levels independently is 0.3~0.6mL.
It is preferred that, the speed for the liquid cooling that the step (4) is extracted with lower floor at the middle and upper levels independently is 1~3 DEG C/min.
The invention provides a kind of method of testing of inorganic phase-changing material modified effect, comprise the following steps：By inorganic phase
Become material and be heated to fusing, obtain stratified liquid；Partially liq is respectively extracted in the upper and lower of the stratified liquid, is dropped respectively
Temperature crystallization, obtains upper strata sample and lower floor's sample；Remaining liq after extraction is mixed with the thickener of certain volume, changed
Property solution；Extract decrease temperature crystalline after partially liq respectively in the same position of above-mentioned sample position, obtain being modified upper strata sample and
Modified lower floor sample；Upper strata sample, lower floor's sample, modified upper strata sample and modified lower floor sample are carried out respectively differential thermal analysis and
Thermogravimetric analysis, obtains differential thermal analysis result and thermal gravimetric analysis results；Counted respectively according to differential thermal analysis result and thermal gravimetric analysis results
Calculate inorganic phase-changing material is completely melt the corresponding hot-fluid difference of temperature than A, beginning dehydration temperaturre pair before and after addition thickener
The hot-fluid difference answered compares C than B and thermogravimetric analysis point quality difference value；The value that the value of the A is more than 85%, B is more than 70%,
And when C value is more than 95%, the thickener of the volume can be effectively improved the lamination of inorganic phase-changing material.
The present invention passes through nothing after test before modified using the uniformity for testing modified inorganic phase-changing material levels material
The change of the thermodynamic behaviour of machine phase-change material, is realized to Different adding amount, different types of thickener to inorganic-phase variable material
Expect the Accurate Determining of modified effect.Test result indicates that, the method for testing that the present invention is provided is objective, can be to inorganic phase-changing material
Modified effect carry out Accurate Determining.
Brief description of the drawings
Fig. 1 be in the embodiment of the present invention 1 before modified after inorganic phase-changing material outward appearance comparison diagram；
Fig. 2 is the TA test curves of the embodiment of the present invention 1 sample and lower floor's sample at the middle and upper levels；
Fig. 3 is the DTA test curves of the embodiment of the present invention 1 sample and lower floor's sample at the middle and upper levels；
Fig. 4 is the TA test curves of modified upper strata sample and modified lower floor sample in the embodiment of the present invention 1；
Fig. 5 is the DTA test curves of modified upper strata sample and modified lower floor sample in the embodiment of the present invention 1；
Fig. 6 is the TA test curves and DTA test curves of the embodiment of the present invention 2 sample and lower floor's sample at the middle and upper levels；
Fig. 7 is that the TA test curves and DTA tests of modified upper strata sample and modified lower floor sample in the embodiment of the present invention 2 are bent
Line；
Fig. 8 is the TA test curves and DTA test curves of the embodiment of the present invention 3 sample and lower floor's sample at the middle and upper levels；
Fig. 9 is that the TA test curves and DTA tests of modified upper strata sample and modified lower floor sample in the embodiment of the present invention 3 are bent
Line.
Embodiment
The invention provides a kind of method of testing of inorganic phase-changing material modified effect, comprise the following steps：
(1) inorganic phase-changing material is heated to fusing, obtains stratified liquid；It is each in the upper and lower of the stratified liquid
Partially liq is extracted, and marks sample position；
(2) liquid for extracting the step (1) with lower floor at the middle and upper levels distinguishes decrease temperature crystalline, obtains upper strata sample and lower floor
Sample；
(3) remaining liq after extracting in the step (1) is mixed with the thickener of certain volume, obtains being modified molten
Liquid；
(4) after the mark in the modified solution correspondence step (1) that the step (3) is obtained extracts partially liq respectively
Decrease temperature crystalline, obtains being modified upper strata sample and modified lower floor sample；
(5) the modification upper strata that the upper strata sample and lower floor's sample and the step (4) obtained to the step (2) is obtained
Sample and modified lower floor sample carry out differential thermal analysis and thermogravimetric analysis respectively, obtain differential thermal analysis result and thermal gravimetric analysis results；
(6) temperature correspondence is completely melt before and after addition thickener according to differential thermal analysis result calculating inorganic phase-changing material
Hot-fluid difference compare B with the corresponding hot-fluid difference of dehydration temperaturre is started than A；
The of poor quality of thermogravimetric analysis point of the inorganic phase-changing material before and after addition thickener is calculated according to thermal gravimetric analysis results
Value compares C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1To be completely melt the difference of the heat flow value of the corresponding upper strata sample of temperature and the heat flow value of lower floor's sample；
D2To be completely melt the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of temperature with being modified lower floor's sample
Value；
D3For the difference of the heat flow value and the heat flow value of lower floor's sample that start the corresponding upper strata sample of dehydration temperaturre；
D4To start the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of dehydration temperaturre with being modified lower floor's sample
Value；
M1For the difference of the quality and the quality of lower floor's sample of the corresponding upper strata sample of thermogravimetric analysis point；
M2The difference of the quality of quality and modified lower floor sample for the corresponding modified upper strata sample of thermogravimetric analysis point；
The value that the value of the A is more than 85%, B is more than 70%, and C value be more than 95% when, the volume
Thickener can be effectively improved the lamination of inorganic phase-changing material.
Inorganic phase-changing material is heated to fusing by the present invention, obtains stratified liquid；On the upper strata of the stratified liquid with
Layer is each to extract partially liq, and marks sample position.In the present invention, the inorganic phase-changing material preferably includes crystalline hydrate salt
Class phase transformation material.In the present invention, the crystalline hydrate salt phase-change material preferably includes Na2SO4·10H2O、CaCl2·6H2O
Or Na2HPO4·12H2O。
Inorganic phase-changing material is heated to fusing by the present invention, obtains stratified liquid.Operation of the present invention to the heating does not have
There is special restriction, using the technical scheme of heating well known to those skilled in the art.In the present invention, the heating is excellent
Elect heating water bath as.In the present invention, the speed of the heating is preferably 4~6 DEG C/min, more preferably 5 DEG C/min.The present invention
There is no special restriction to the outlet temperature of the heating, make inorganic phase-changing material fusing layering.In the present invention, institute is worked as
Inorganic phase-changing material is stated for CaCl2·6H2During O, the outlet temperature of the heating is preferably 40~60 DEG C, more preferably 45~55
℃。
In the present invention, the insulation of end-point temperature is preferably included in after the fusing；The time of the insulation is preferred
For 50~70min, more preferably 55~65min.In the present invention, it is described to be heated to nodeless mesh water steaming in fusing and insulating process
Hair.
Obtain after stratified liquid, the present invention respectively extracts partially liq in the upper and lower of the stratified liquid, and marks
Sample position.In the present invention, the volume that liquid is extracted in the upper and lower is preferably independently 0.3~0.6mL, more preferably
For 0.4~0.5mL.The present invention, without special restriction, is taken out to the operation of the extraction using well known to those skilled in the art
Take the technical scheme of liquid.In an embodiment of the present invention, the extraction is preferred to use needle tubing.The present invention is extracted to described
Position there is no special restriction, disclosure satisfy that extraction liquid be same phase.
After the completion of extraction, the liquid that the present invention extracts the upper and lower distinguishes decrease temperature crystalline, obtains upper strata sample
With lower floor's sample.In the present invention, independently preferably 1~3 DEG C of the speed for the liquid cooling that the upper and lower are extracted/
Min, more preferably 2 DEG C/min.Liquid of the present invention preferably by the extraction is cooled to room temperature.End of the present invention to the cooling
Point temperature does not have special restriction, allows the liquid to be fully crystallized.
After the completion of crystallization, the present invention is preferably crushed the product of the crystallization respectively, obtains upper strata sample and lower floor
Sample.The present invention is operated without special restriction to described broken, using broken technology well known to those skilled in the art
Scheme.In the present invention, the broken preferably Mechanical Crushing, more preferably mortar is crushed.In the present invention, on described
The particle diameter of layer sample and lower floor's sample is preferably independently 0.5~1mm, more preferably 0.6~0.8mm.
To ensure the phase same sex of original material, after the completion of extraction, the present invention is by the remaining liq after the extraction and necessarily
The thickener mixing of volume, obtains modified solution.In the present invention, the thickener does not preferably expand simultaneously at 200~250 DEG C
And physical and chemical character is constant.In the present invention, the thickener preferably includes super absorbent resin.In embodiments of the invention
In, the thickener is preferably the mixture of super absorbent resin and sodium carboxymethylcellulose；The super absorbent resin and carboxylic
The mass ratio of sodium carboxymethylcellulose pyce is preferably 1:1.In the present invention, the super absorbent resin is preferably polyacrylate tree
Fat.The present invention does not have special restriction to the volume of the thickener, is adjusted according to test request.
In the present invention, the mixing is preferably carried out under agitation；The speed of the stirring is preferably 400~
600r/min, more preferably 450~550r/min；The time of the stirring is preferably 15~25min, more preferably 20min.
Modification of the thickener to inorganic phase-changing material is completed in the present invention, in the mixed process.
Obtain after modified solution, mark of the present invention in sample position described in modified solution correspondence above-mentioned technical proposal
Place extracts decrease temperature crystalline after partially liq respectively, obtains being modified upper strata sample and modified lower floor sample.In the present invention, on described
The volume that layer and lower floor extract liquid is preferably independently 0.3~0.6mL, more preferably 0.4~0.5mL.In the present invention, institute
The speed for stating the liquid cooling of the upper and lower extraction is preferably independently 1~3 DEG C/min, more preferably 2 DEG C/min.
After the completion of crystallization, the present invention is preferably crushed the product of the crystallization respectively, obtain being modified upper strata sample and
Modified lower floor sample.The present invention, without special restriction, is broken to the broken operation using well known to those skilled in the art
Broken technical scheme.In the present invention, the broken preferably Mechanical Crushing, more preferably mortar is crushed.In the present invention
In, the particle diameter of the modified upper strata sample and modified lower floor's sample is preferably independently 0.5~1mm, more preferably 0.6~
0.8mm。
Obtain after upper strata sample, lower floor's sample, modified upper strata sample and modified lower floor sample, the present invention is to the upper strata sample
Product and lower floor's sample and the modified upper strata sample and modified lower floor sample carry out differential thermal analysis and thermogravimetric analysis respectively, obtain
Differential thermal analysis result and thermal gravimetric analysis results.The present invention is to the operation of the differential thermal analysis and thermogravimetric analysis without special limit
It is fixed, using the technical scheme of heat analysis well known to those skilled in the art.
Obtain after differential thermal analysis result and thermal gravimetric analysis results, the present invention calculates inorganic-phase variable material according to differential thermal analysis result
Expect to be completely melt the corresponding hot-fluid difference of temperature hot-fluid difference more corresponding with dehydration temperaturre is started than A before and after addition thickener
Compare B；The quality difference value ratio of thermogravimetric analysis point of the inorganic phase-changing material before and after addition thickener is calculated according to thermal gravimetric analysis results
C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1To be completely melt the difference of the heat flow value of the corresponding upper strata sample of temperature and the heat flow value of lower floor's sample；
D2To be completely melt the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of temperature with being modified lower floor's sample
Value；
D3For the difference of the heat flow value and the heat flow value of lower floor's sample that start the corresponding upper strata sample of dehydration temperaturre；
D4To start the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of dehydration temperaturre with being modified lower floor's sample
Value；
M1For the difference of the quality and the quality of lower floor's sample of the corresponding upper strata sample of thermogravimetric analysis point；
M2The difference of the quality of quality and modified lower floor sample for the corresponding modified upper strata sample of thermogravimetric analysis point；
The value that the value of the A is more than 85%, B is more than 70%, and C value be more than 95% when, the volume
Thickener can be effectively improved the lamination of inorganic phase-changing material.
When any one is unsatisfactory for above-mentioned condition in modified obtained A, B, the C of the thickener of volume value, then
The thickener of above-mentioned volume is bad for the lamination improvement of inorganic phase-changing material.
In order to further illustrate the present invention, the inorganic phase-changing material modified effect provided with reference to embodiment the present invention
Method of testing be described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1:
500g calcium chloride hexahydrate solids are put into container, are then heated to melting in water-bath, 5 DEG C of the rate of heat addition/
1h is incubated after min, fusing, temperature control is between 40~60 DEG C, it is ensured that material is completely melt, will not in this phase transition process
There is the phenomenon of crystallization water evaporation.
Calcium chloride hexahydrate in container has occurred that phase lamination, is melted with two identical needle tubing evacuation containers
Each 0.5ml of stratified liquid up and down of liquid, while sample location is marked on container, the solution in dropper is put into
Two hermetic bags of identical, and decrease temperature crystalline processing is carried out, 2 DEG C/min of rate of temperature fall is cooled to room temperature.After the completion of crystallization
Carry out Mechanical Crushing and be pressed into evengranular powder, 5min is crushed with mortar, size controlling is obtained within the scope of 0.5~1mm
Upper strata sample and lower floor's sample.
In order to ensure the phase same sex of original material, the super absorbent resin for weighing inorganic phase-changing material quality 25wt% is (poly-
Acrylates) and sodium carboxymethylcellulose (1:1), it is slowly added into remaining melt liquid, is stirred with mechanical agitator
20min, stir speed (S.S.) is controlled in 500r/min, reaches the purpose for being uniformly distributed two kinds of thickener components.It is effective in order to be formed
Contrast effect after before modified, material samples the principle for must being fulfilled for same position, so does to help to consider being layered this spy
Property.The same test tube using two same sizes of contrast, at the previous graticule of container, each solution for extracting 0.5ml is put into two
The hermetic bag of individual same size carries out decrease temperature crystalline processing, after the completion of crystallization, and the same Mechanical Crushing that carries out is pressed into powder, is changed
Property upper strata sample and modified lower floor's sample.
Inorganic phase-changing material outward appearance comparison diagram is as shown in Figure 1 after before modified.It will be seen from figure 1 that inorganic-phase variable before modified
Material is substantially divided into two layers, and modified inorganic phase-changing material is improving uniformity of melt.
The sample collected is subjected to TA (Thermal Synthetic Analysis) tests, TA is tested including TGA, DTA.TGA full name thermogravimetric point
Analysis, is that a kind of evaluate sample under (10~300 DEG C), describes becoming for weight change with temperature rising in certain temperature range
Gesture.The test can be used for the water content demarcated in calcium chloride hexahydrate；And DTA then describes the thermodynamic behaviour of sample.It is logical
Cross TGA/DTA and test gathered sample, super absorbent resin (polyacrylate of the calcium chloride hexahydrate in 25wt% can be obtained
Class) and the modified thermogravimetric of sodium carboxymethylcellulose and thermodynamic behaviour change.
The TA test curves of the present embodiment sample and lower floor's sample at the middle and upper levels are as shown in Fig. 2 DTA test curves such as Fig. 3 institutes
Show；The TA test curves of modified upper strata sample and modified lower floor sample are as shown in figure 4, DTA test curves are as shown in Figure 5.
Calculated according to the data of Fig. 2~5：
1 is completely melt a little：
DTA (SAP) difference | lower floor-upper strata |：0.28-0.27=0.01
DTA (no SAP) difference | lower floor-upper strata |：0.38-0.30=0.08
| DTA (no SAP) difference |-| DTA (SAP) difference |/| DTA (no SAP) difference | (100%)=0.08-0.01/
0.08=87.5% ＞ 85%
2 start dehydration point：
DTA (SAP) difference | lower floor-upper strata |：0.51-0.49=0.02
DTA (no SAP) difference | lower floor-upper strata |：0.61-0.54=0.07
| DTA (no SAP) difference |-| DTA (SAP) difference |/| DTA (no SAP) difference | (100%)=0.07-0.02/
0.07=71.43% ＞ 70%
3 thermogravimetric analysis points：
TA (SAP) difference | lower floor-upper strata |：36.57%-36.7%=0.13% (dehydration rate difference)
TA (no SAP) difference | lower floor-upper strata |：44.79%-40.71%=4.08%
| DTA (no SAP) difference |-| TA (SAP) difference |/| DTA (no SAP) difference | the ＞ of (100%)=96.8% 95%
Result of calculation shows that 25wt% super absorbent resin (polyacrylate) and sodium carboxymethylcellulose is to six water
The mutually layering modified effect of calcium chloride is good, can avoid layering.
Embodiment 2:
According to the method for embodiment 1, the difference is that using 15wt% super absorbent resin (polyacrylate) and carboxylic
Sodium carboxymethylcellulose pyce is modified to calcium chloride hexahydrate.
The TA test curves and DTA test curves of the present embodiment sample and lower floor's sample at the middle and upper levels are as shown in Figure 6；In modification
The TA test curves and DTA test curves of layer sample and modified lower floor sample are as shown in Figure 7.
Calculated according to Fig. 6 and Fig. 7 data：
1 is completely melt a little：
DTA (SAP) difference | lower floor-upper strata |：0.351-0.372=0.021
DTA (no SAP) difference | lower floor-upper strata |：0.39-0.129=0.261
| DTA (no SAP) difference |-| DTA (SAP) difference |/| DTA (no SAP) difference | (100%)=0.261-0.021/
0.261=91.9% ＞ 85%
2 start dehydration point：
DTA (SAP) difference | lower floor-upper strata |：0.582-0.577=0.005
DTA (no SAP) difference | lower floor-upper strata |：0.605-0.592=0.013
| DTA (no SAP) difference |-| DTA (SAP) difference |/| DTA (no SAP) difference | (100%)=0.013-0.005/
0.013=61.5% ＜ 70%
3 thermogravimetric analysis points：
TA (SAP) difference | lower floor-upper strata |：39.453%-38.817%=0.636% (dehydration rate difference)
TA (no SAP) difference | lower floor-upper strata |：46.99%-41.043%=5.947%
| DTA (no SAP) difference |-| TA (SAP) difference |/| DTA (no SAP) difference | the ＜ of (100%)=89.3% 95%
Result of calculation shows that 15wt% super absorbent resin (polyacrylate) and sodium carboxymethylcellulose is to six water
The mutually layering modified effect of calcium chloride is bad, it is impossible to avoid layering.
Embodiment 3:
According to the method for embodiment 1, the difference is that using 5wt% super absorbent resin (polyacrylate) and carboxylic first
Base sodium cellulosate is modified to calcium chloride hexahydrate.
The TA test curves and DTA test curves of the present embodiment sample and lower floor's sample at the middle and upper levels are as shown in Figure 8；In modification
The TA test curves and DTA test curves of layer sample and modified lower floor sample are as shown in Figure 9.
Calculated according to Fig. 8 and Fig. 9 data：
1 is completely melt a little：
DTA (SAP) difference | lower floor-upper strata |：0.377-0.289=0.088
DTA (no SAP) difference | lower floor-upper strata |：0.410-0.391=0.091
| DTA (no SAP) difference |-| DTA (SAP) difference |/| DTA (no SAP) difference | (100%)=0.091-0.088/
0.091=3.3% ＜ 85%
2 start dehydration point：
DTA (SAP) difference | lower floor-upper strata |：0.548-0.500=0.0048
DTA (no SAP) difference | lower floor-upper strata |：0.540-0.519=0.021
| DTA (no SAP) difference |-| DTA (SAP) difference |/| DTA (no SAP) difference | (100%)=0.021-0.048/
0.021=-56.25% ＜ 70%
3 thermogravimetric analysis points：
TA (SAP) difference | lower floor-upper strata |：41.94%-41.15%=0.79% (dehydration rate difference)
TA (no SAP) difference | lower floor-upper strata |：66.93%-41.01%=22.92%
| DTA (no SAP) difference |-| TA (SAP) difference |/| DTA (no SAP) difference | the ＞ of (100%)=96.5% 95%
Result of calculation shows that 5wt% super absorbent resin (polyacrylate) and sodium carboxymethylcellulose is to six water
The mutually layering modified effect of calcium chloride is bad, it is impossible to avoid layering.
As can be seen from the above embodiments, the method for testing that the present invention is provided can be entered to inorganic phase-changing material modified effect
The accurate objectively analysis of row.
Described above is only the preferred embodiment of the present invention, not makees any formal limitation to the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of method of testing of inorganic phase-changing material modified effect, comprises the following steps：
(1) inorganic phase-changing material is heated to fusing, obtains stratified liquid；Respectively extracted in the upper and lower of the stratified liquid
Partially liq, and mark sample position；
(2) liquid for extracting the step (1) with lower floor at the middle and upper levels distinguishes decrease temperature crystalline, obtains upper strata sample and lower floor's sample
Product；
(3) remaining liq after being extracted in the step (1) is mixed with the thickener of certain volume, obtains modified solution；
(4) mark in the modified solution correspondence step (1) that the step (3) is obtained extracts cooling after partially liq respectively
Crystallization, obtains being modified upper strata sample and modified lower floor sample；
(5) the modification upper strata sample that the upper strata sample and lower floor's sample and the step (4) obtained to the step (2) is obtained
Differential thermal analysis and thermogravimetric analysis are carried out respectively with lower floor's sample is modified, and obtain differential thermal analysis result and thermal gravimetric analysis results；
(6) the corresponding heat of temperature is completely melt before and after addition thickener according to differential thermal analysis result calculating inorganic phase-changing material
Stream difference hot-fluid difference more corresponding with dehydration temperaturre is started than A compares B；
The quality difference value ratio of thermogravimetric analysis point of the inorganic phase-changing material before and after addition thickener is calculated according to thermal gravimetric analysis results
C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1To be completely melt the difference of the heat flow value of the corresponding upper strata sample of temperature and the heat flow value of lower floor's sample；
D2To be completely melt the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of temperature with being modified lower floor's sample；
D3For the difference of the heat flow value and the heat flow value of lower floor's sample that start the corresponding upper strata sample of dehydration temperaturre；
D4To start the difference of heat flow value of the heat flow value of the corresponding modified upper strata sample of dehydration temperaturre with being modified lower floor's sample；
M1For the difference of the quality and the quality of lower floor's sample of the corresponding upper strata sample of heat analysis emphasis；
M2The difference of the quality of quality and modified lower floor sample for the corresponding modified upper strata sample of heat analysis emphasis；
The value that the value of the A is more than 85%, B is more than 70%, and C value be more than 95% when, the thickening of the volume
Agent can be effectively improved the lamination of inorganic phase-changing material.
2. according to the method described in claim 1, it is characterised in that the inorganic phase-changing material includes crystalline hydrate salt class phase transformation
Material.
3. method according to claim 2, it is characterised in that the crystalline hydrate salt phase-change material includes Na2SO4·
10H2O、CaCl2·6H2O or Na2HPO4·12H2O。
4. according to the method described in claim 1, it is characterised in that the thickener does not expand and thing at 200~250 DEG C
Physicochemical character is constant.
5. the method according to claim 1 or 4, it is characterised in that the thickener includes super absorbent resin and/or carboxylic
Sodium carboxymethylcellulose pyce.
6. according to the method described in claim 1, it is characterised in that the step (1) extracts the body of liquid with lower floor at the middle and upper levels
Product independently is 0.3~0.6mL.
7. according to the method described in claim 1, it is characterised in that the liquid drop that the step (2) is extracted with lower floor at the middle and upper levels
The speed of temperature independently is 1~3 DEG C/min.
8. according to the method described in claim 1, it is characterised in that the mixing in the step (3) is carried out under agitation；
The speed of the stirring is 400~600r/min；The time of the stirring is 15~25min.
9. according to the method described in claim 1, it is characterised in that the step (4) extracts the body of liquid with lower floor at the middle and upper levels
Product independently is 0.3~0.6mL.
10. the method according to claim 1 or 9, it is characterised in that the liquid that the step (4) is extracted with lower floor at the middle and upper levels
The speed of body cooling independently is 1~3 DEG C/min.
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