CN107271313B - A kind of test method of inorganic phase-changing material modified effect - Google Patents
A kind of test method of inorganic phase-changing material modified effect Download PDFInfo
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- CN107271313B CN107271313B CN201710604161.5A CN201710604161A CN107271313B CN 107271313 B CN107271313 B CN 107271313B CN 201710604161 A CN201710604161 A CN 201710604161A CN 107271313 B CN107271313 B CN 107271313B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
Abstract
The present invention provides a kind of test methods of inorganic phase-changing material modified effect.The present invention carries out differential thermal analysis and thermogravimetric analysis by the upper and lower level solution to rear inorganic phase-changing material before modified, calculates separately the quality difference value ratio C that is completely melt temperature corresponding hot-fluid difference ratio A, starts dehydration temperaturre corresponding hot-fluid difference ratio B and thermogravimetric analysis point of the inorganic phase-changing material before and after adding thickener according to differential thermal analysis result and thermal gravimetric analysis results；The value that the value of the A is 85% or more, B is 70% or more, and the value of C be 95% or more 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 upper and lower level substance, by the variation of the thermodynamic behaviour of inorganic phase-changing material after testing 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, in particular to a kind of test of inorganic phase-changing material modified effect
Method.
Background technique
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, having quite a few among these is organic phase change material.
Organic phase change material in general performance is relatively stable, 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
It has a certain impact and endangers, while the fire resistance of organic phase change material is poor, does not have fire protecting performance, this is mainly and organic
The chemical characteristic of phase-change material is related.
Inorganic phase-changing material has preferable fire protecting performance, either metal oxide or crystalline hydrate salt class phase transformation material
Material can resist open fire 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, which generally has, to be subcooled and is mutually layered both of these problems.By taking crystalline hydrate salt phase-change material as an example, work as phase
When change material is cooled near phase transformation temperature points, phase transition process will not generally start at once, only when temperature progressively decreases to
When to a certain degree, the phenomenon that phase transition process just abruptly starts to is exactly the surfusion of inorganic hydrated salt class phase transformation material；And it is layered
Phenomenon be exactly inorganic hydrated salt class phase transformation material in melting process itself metal salt cannot be dissolved in fusing crystallization it is water-soluble
Phenomenon in liquid.If can effectively eliminate supercooling and phase lamination can large-scale use inorganic phase-changing material, and
And the fire performance of inorganic phase-changing material can be fully played out.
Supercooling is solved at present generally uses nucleating agent method, it is general by adding certain nucleating agents, thus in temperature-fall period, it is auxiliary
It helps inorganic phase-changing material to form nucleus in time, facilitates crystallization；And solve the method that is mutually layered, generally use add variety classes with
And the method for different amounts of thickener improves.The eradicating efficacy that nucleating agent improves supercooling in general is remembered using temperature sensor
Recording temperature change and drawing cooling curve intuitively to characterize, but what variety classes were mutually layered with the improvement of the thickener of volume
The judgement of effect be all by visually being identified, it is subjective, there is very big drawback and getting sth into one's head property, without one kind
Objective characterizing method evaluates its improvement.
Summary of the invention
The purpose of the present invention is to provide a kind of test methods of inorganic phase-changing material modified effect.Survey provided by the invention
Method for testing can carry out accurate objectively analysis to inorganic phase-changing material modified effect.
The present invention provides a kind of test methods of inorganic phase-changing material modified effect, comprising the following steps:
(1) inorganic phase-changing material is heated to melting, obtains stratified liquid；It is each in the upper and lower of the stratified liquid
Extraction section liquid, and mark sample position；
(2) liquid that the step (1) is extracted with lower layer at the middle and upper levels is distinguished into decrease temperature crystalline, obtains upper layer sample and lower layer
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 modified solution that the step (3) obtains corresponds to the difference extraction section liquid of the mark in step (1)
Decrease temperature crystalline obtains modified upper layer sample and modified lower layer's sample；
(5) the modification upper layer that the upper layer sample and lower layer's sample and the step (4) obtained to the step (2) obtains
Sample and modified lower layer's sample carry out differential thermal analysis and thermogravimetric analysis respectively, obtain differential thermal analysis result and thermal gravimetric analysis results；
(6) it is completely melt that temperature is corresponding before and after adding thickener according to differential thermal analysis result calculating inorganic phase-changing material
Hot-fluid difference ratio A with start the corresponding hot-fluid difference ratio B of dehydration temperaturre；
The of poor quality of thermogravimetric analysis point of the inorganic phase-changing material before and after adding thickener is calculated according to thermal gravimetric analysis results
Value ratio C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1For the difference for being completely melt the heat flow value of the corresponding upper layer sample of temperature and the heat flow value of lower layer's sample；
D2For the difference for being completely melt the heat flow value of the corresponding modified upper layer sample of temperature and the heat flow value of modified lower layer's sample
Value；
D3For the difference for starting the heat flow value of the corresponding upper layer sample of dehydration temperaturre and the heat flow value of lower layer's sample；
D4For the difference for starting the heat flow value of the corresponding modified upper layer sample of dehydration temperaturre and the heat flow value of modified lower layer's sample
Value；
M1For the difference of the quality of the quality and lower layer's sample of the corresponding upper layer sample of thermogravimetric analysis point；
M2For the difference of the quality of the quality and modified lower layer's sample of the corresponding modified upper layer sample of thermogravimetric analysis point；
The value that the value of the A is 85% or more, B is 70% or more, and the value of C be 95% or more when, the volume
Thickener can be effectively improved the lamination of inorganic phase-changing material.
Preferably, the inorganic phase-changing material includes crystalline hydrate salt phase-change material.
Preferably, the crystalline hydrate salt phase-change material includes Na2SO4·10H2O、CaCl2·6H2O or Na2HPO4·
12H2O。
Preferably, the thickener does not expand at 200~250 DEG C and physical and chemical character is constant.
Preferably, the thickener includes super absorbent resin and/or sodium carboxymethylcellulose.
Preferably, the volume that the step (1) extracts liquid with lower layer at the middle and upper levels independently is 0.3~0.6mL.
Preferably, the rate for the liquid cooling that the step (2) is extracted with lower layer at the middle and upper levels independently is 1~3 DEG C/min.
Preferably, the mixing in the step (3) carries out under agitation；The rate of the stirring is 400~600r/
min；The time of the stirring is 15~25min.
Preferably, the volume that the step (4) extracts liquid with lower layer at the middle and upper levels independently is 0.3~0.6mL.
Preferably, the rate for the liquid cooling that the step (4) is extracted with lower layer at the middle and upper levels independently is 1~3 DEG C/min.
The present invention provides a kind of test methods of inorganic phase-changing material modified effect, comprising the following steps: by inorganic phase
Become material to be heated to melting, obtains stratified liquid；In each extraction section liquid in the upper and lower of the stratified liquid, drop respectively
Temperature crystallization, obtains upper layer sample and lower layer's sample；Remaining liq after extraction is mixed with the thickener of certain volume, is changed
Property solution；The decrease temperature crystalline after the difference extraction section liquid of above-mentioned sample position same position, obtain modified upper layer sample and
Modified lower layer's sample；To upper layer sample, lower layer's sample, modified upper layer sample and modified lower layer's sample carry out respectively differential thermal analysis and
Thermogravimetric analysis obtains differential thermal analysis result and thermal gravimetric analysis results；It is counted respectively according to differential thermal analysis result and thermal gravimetric analysis results
Inorganic phase-changing material is calculated to be completely melt the corresponding hot-fluid difference ratio A of temperature before and after adding thickener, start dehydration temperaturre pair
The quality difference value ratio C of the hot-fluid difference ratio B and thermogravimetric analysis point that answer；The value that the value of the A is 85% or more, B is 70% or more,
And when the value of C is 95% or more, the thickener of the volume can be effectively improved the lamination of inorganic phase-changing material.
The present invention passes through nothing after testing before modified using the uniformity for testing modified inorganic phase-changing material upper and lower level substance
The variation 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.The experimental results showed that test method provided by the invention is objective, it can be to inorganic phase-changing material
Modified effect carry out Accurate Determining.
Detailed description of the invention
Fig. 1 be in the embodiment of the present invention 1 before modified after inorganic phase-changing material appearance comparison diagram；
Fig. 2 is the TA test curve of the embodiment of the present invention 1 sample and lower layer's sample at the middle and upper levels；
Fig. 3 is the DTA test curve of the embodiment of the present invention 1 sample and lower layer's sample at the middle and upper levels；
Fig. 4 is the TA test curve of modified upper layer sample and modified lower layer's sample in the embodiment of the present invention 1；
Fig. 5 is the DTA test curve of modified upper layer sample and modified lower layer's sample in the embodiment of the present invention 1；
Fig. 6 is the TA test curve and DTA test curve of the embodiment of the present invention 2 sample and lower layer's sample at the middle and upper levels；
Fig. 7 is that the TA test curve and DTA test of modified upper layer sample and modified lower layer's sample in the embodiment of the present invention 2 are bent
Line；
Fig. 8 is the TA test curve and DTA test curve of the embodiment of the present invention 3 sample and lower layer's sample at the middle and upper levels；
Fig. 9 is that the TA test curve and DTA test of modified upper layer sample and modified lower layer's sample in the embodiment of the present invention 3 are bent
Line.
Specific embodiment
The present invention provides a kind of test methods of inorganic phase-changing material modified effect, comprising the following steps:
(1) inorganic phase-changing material is heated to melting, obtains stratified liquid；It is each in the upper and lower of the stratified liquid
Extraction section liquid, and mark sample position；
(2) liquid that the step (1) is extracted with lower layer at the middle and upper levels is distinguished into decrease temperature crystalline, obtains upper layer sample and lower layer
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 modified solution that the step (3) obtains corresponds to the difference extraction section liquid of the mark in step (1)
Decrease temperature crystalline obtains modified upper layer sample and modified lower layer's sample；
(5) the modification upper layer that the upper layer sample and lower layer's sample and the step (4) obtained to the step (2) obtains
Sample and modified lower layer's sample carry out differential thermal analysis and thermogravimetric analysis respectively, obtain differential thermal analysis result and thermal gravimetric analysis results；
(6) it is completely melt that temperature is corresponding before and after adding thickener according to differential thermal analysis result calculating inorganic phase-changing material
Hot-fluid difference ratio A with start the corresponding hot-fluid difference ratio B of dehydration temperaturre；
The of poor quality of thermogravimetric analysis point of the inorganic phase-changing material before and after adding thickener is calculated according to thermal gravimetric analysis results
Value ratio C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1For the difference for being completely melt the heat flow value of the corresponding upper layer sample of temperature and the heat flow value of lower layer's sample；
D2For the difference for being completely melt the heat flow value of the corresponding modified upper layer sample of temperature and the heat flow value of modified lower layer's sample
Value；
D3For the difference for starting the heat flow value of the corresponding upper layer sample of dehydration temperaturre and the heat flow value of lower layer's sample；
D4For the difference for starting the heat flow value of the corresponding modified upper layer sample of dehydration temperaturre and the heat flow value of modified lower layer's sample
Value；
M1For the difference of the quality of the quality and lower layer's sample of the corresponding upper layer sample of thermogravimetric analysis point；
M2For the difference of the quality of the quality and modified lower layer's sample of the corresponding modified upper layer sample of thermogravimetric analysis point；
The value that the value of the A is 85% or more, B is 70% or more, and the value of C be 95% or more when, the volume
Thickener can be effectively improved the lamination of inorganic phase-changing material.
Inorganic phase-changing material is heated to melting by the present invention, obtains stratified liquid；On the upper layer of the stratified liquid under
Each extraction section liquid of layer, and mark 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 melting by the present invention, obtains stratified liquid.The present invention does not have the operation of the heating
There is special restriction, using the technical solution of heating well known to those skilled in the art.In the present invention, the heating is excellent
It is selected as heating water bath.In the present invention, the rate 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, makes inorganic phase-changing material fusing layering.In the present invention, work as institute
Stating inorganic phase-changing material is CaCl2·6H2When O, the outlet temperature of the heating is preferably 40~60 DEG C, more preferably 45~55
℃。
In the present invention, the heat preservation of end-point temperature is preferably included in after the fusing；The time of the heat preservation is preferred
For 50~70min, more preferably 55~65min.In the present invention, described to be heated to no crystal water steaming in fusing and insulating process
Hair.
After obtaining stratified liquid, the present invention is marked in each extraction section liquid in the upper and lower of the stratified liquid
Sample position.In the present invention, it is independently preferably 0.3~0.6mL that the volume of liquid is extracted in the upper and lower, more preferably
For 0.4~0.5mL.The not special restriction of operation of the present invention to the extraction, using pumping well known to those skilled in the art
Take the technical solution of liquid.In an embodiment of the present invention, the extraction preferably uses needle tubing.The present invention is to the extraction
Position there is no special restriction, can satisfy 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 layer sample
With lower layer's sample.In the present invention, independently preferably 1~3 DEG C of the rate 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 product of the crystallization is preferably crushed by the present invention respectively, obtains upper layer sample and lower layer
Sample.The present invention restriction not special to the broken operation, using broken technology well known to those skilled in the art
Scheme.In the present invention, the broken preferably Mechanical Crushing, more preferably mortar are broken.In the present invention, on described
The partial size of layer sample and lower layer's sample is independently preferably 0.5~1mm, more preferably 0.6~0.8mm.
For the phase same sex for guaranteeing original material, after the completion of extraction, the present invention is by the remaining liq after the extraction and centainly
The thickener of volume mixes, and 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 the embodiment of the present 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
Rouge.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 preferably carries out under agitation；The rate 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.
After obtaining modified solution, the present invention corresponds to the label of sample position described in above-mentioned technical proposal in the modified solution
Decrease temperature crystalline after place's difference extraction section liquid, obtains modified upper layer sample and modified lower layer's sample.In the present invention, on described
The volume that layer and lower layer extract liquid is independently preferably 0.3~0.6mL, more preferably 0.4~0.5mL.In the present invention, institute
The rate for stating the liquid cooling of the upper and lower extraction is independently preferably 1~3 DEG C/min, more preferably 2 DEG C/min.
After the completion of crystallization, the product of the crystallization is preferably crushed by the present invention respectively, obtain modified upper layer sample and
Modified lower layer's sample.The present invention restriction not special to the broken operation, using well known to those skilled in the art broken
Broken technical solution.In the present invention, the broken preferably Mechanical Crushing, more preferably mortar are broken.In the present invention
In, the partial size of the modified upper layer sample and modified lower layer's sample is independently preferably 0.5~1mm, more preferably 0.6~
0.8mm。
After obtaining upper layer sample, lower layer's sample, modified upper layer sample and modified lower layer's sample, the present invention is to the upper layer sample
Product and lower layer's sample and the modified upper layer sample and modified lower layer's sample carry out differential thermal analysis and thermogravimetric analysis respectively, obtain
Differential thermal analysis result and thermal gravimetric analysis results.The present invention limit not special to the operation of the differential thermal analysis and thermogravimetric analysis
It is fixed, using the technical solution of heat analysis well known to those skilled in the art.
After obtaining differential thermal analysis result and thermal gravimetric analysis results, the present invention calculates inorganic-phase variable material according to differential thermal analysis result
Material is completely melt the corresponding hot-fluid difference ratio A of temperature hot-fluid difference corresponding with dehydration temperaturre is started before and after adding thickener
Compare B；The quality difference value ratio of thermogravimetric analysis point of the inorganic phase-changing material before and after adding thickener is calculated according to thermal gravimetric analysis results
C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1For the difference for being completely melt the heat flow value of the corresponding upper layer sample of temperature and the heat flow value of lower layer's sample；
D2For the difference for being completely melt the heat flow value of the corresponding modified upper layer sample of temperature and the heat flow value of modified lower layer's sample
Value；
D3For the difference for starting the heat flow value of the corresponding upper layer sample of dehydration temperaturre and the heat flow value of lower layer's sample；
D4For the difference for starting the heat flow value of the corresponding modified upper layer sample of dehydration temperaturre and the heat flow value of modified lower layer's sample
Value；
M1For the difference of the quality of the quality and lower layer's sample of the corresponding upper layer sample of thermogravimetric analysis point；
M2For the difference of the quality of the quality and modified lower layer's sample of the corresponding modified upper layer sample of thermogravimetric analysis point；
The value that the value of the A is 85% or more, B is 70% or more, and the value of C be 95% or more when, the volume
Thickener can be effectively improved the lamination of inorganic phase-changing material.
When any one of the value of A, B, C obtained when the thickener of the volume is modified is unsatisfactory for above-mentioned condition, 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, below with reference to embodiment to inorganic phase-changing material modified effect provided by the invention
Test method be described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1:
500g calcium chloride hexahydrate solid is put into container, is then heated to melting in water-bath, 5 DEG C of the rate of heat addition/
Min keeps the temperature 1h after fusing, temperature controls between 40~60 DEG C, guarantees that material is completely melt, will not in this phase transition process
There is the phenomenon that crystallization water evaporation.
Calcium chloride hexahydrate in container has occurred that phase lamination, with melting in 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
Identical two hermetic bags, 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
It carries out Mechanical Crushing and is pressed into evengranular powder, be crushed 5min with mortar, size controlling obtains within the scope of 0.5~1mm
Upper layer sample and lower layer's sample.
In order to guarantee 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, stirring rate control in 500r/min, achieve the purpose that be uniformly distributed two kinds of thickener components.It is effective in order to be formed
Contrast effect after before modified, material sample the principle that must satisfy same position, and doing so helps to consider this spy of layering
Property.Comparison equally uses the test tube of two same sizes, and at the previous graticule of container, each solution for extracting 0.5ml is put into two
The hermetic bag of a same size carries out decrease temperature crystalline processing, and after the completion of crystallization, the same Mechanical Crushing that carries out is pressed into powder, is changed
Property upper layer sample and modified lower layer's sample.
Inorganic phase-changing material 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 obviously divided into two layers, and modified inorganic phase-changing material is improving uniformity of melt.
Collected sample is subjected to TA (Thermal Synthetic Analysis) test, TA includes TGA, DTA test.TGA full name thermogravimetric point
Analysis is a kind of assessment sample in certain temperature range under (10~300 DEG C), and description weight rises with temperature and variation becomes
Gesture.The test can be used for demarcating the water content in calcium chloride hexahydrate；And DTA then describes the thermodynamic behaviour of sample.It is logical
It crosses TGA/DTA and tests sample collected, super absorbent resin (polyacrylate of the available calcium chloride hexahydrate in 25wt%
Class) and sodium carboxymethylcellulose modified thermogravimetric and thermodynamic behaviour variation.
The present embodiment at the middle and upper levels the TA test curve of sample and lower layer's sample as shown in Fig. 2, DTA test curve such as Fig. 3 institute
Show；The TA test curve of modified upper layer sample and modified lower layer's sample is as shown in figure 4, DTA test curve is as shown in Figure 5.
Data according to fig. 2~5 calculate:
1 is completely melt a little:
DTA (SAP) difference | lower layer-upper layer |: 0.28-0.27=0.01
DTA (no SAP) difference | lower layer-upper layer |: 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 layer-upper layer |: 0.51-0.49=0.02
DTA (no SAP) difference | lower layer-upper layer |: 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 layer-upper layer |: 36.57%-36.7%=0.13% (dehydration rate difference)
TA (no SAP) difference | lower layer-upper layer |: 44.79%-40.71%=4.08%
| DTA (no SAP) difference |-| TA (SAP) difference |/| DTA (no SAP) difference | the > of (100%)=96.8% 95%
The super absorbent resin (polyacrylate) and sodium carboxymethylcellulose that calculated result shows 25wt% are to six water
The mutually layering modified effect of calcium chloride is good, can be avoided layering.
Embodiment 2:
According to the method for embodiment 1, using the super absorbent resin (polyacrylate) and carboxylic of 15wt% unlike
Sodium carboxymethylcellulose pyce is modified calcium chloride hexahydrate.
The TA test curve and DTA test curve of the present embodiment sample and lower layer's sample at the middle and upper levels are as shown in Figure 6；In modification
The TA test curve and DTA test curve of layer sample and modified lower layer's sample are as shown in Figure 7.
It is calculated according to the data of Fig. 6 and Fig. 7:
1 is completely melt a little:
DTA (SAP) difference | lower layer-upper layer |: 0.351-0.372=0.021
DTA (no SAP) difference | lower layer-upper layer |: 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 layer-upper layer |: 0.582-0.577=0.005
DTA (no SAP) difference | lower layer-upper layer |: 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 layer-upper layer |: 39.453%-38.817%=0.636% (dehydration rate difference)
TA (no SAP) difference | lower layer-upper layer |: 46.99%-41.043%=5.947%
| DTA (no SAP) difference |-| TA (SAP) difference |/| DTA (no SAP) difference | the < of (100%)=89.3% 95%
The super absorbent resin (polyacrylate) and sodium carboxymethylcellulose that calculated result shows 15wt% are to six water
The mutually layering modified effect of calcium chloride is bad, is not avoided that layering.
Embodiment 3:
According to the method for embodiment 1, using the super absorbent resin (polyacrylate) and carboxylic first of 5wt% unlike
Base sodium cellulosate is modified calcium chloride hexahydrate.
The TA test curve and DTA test curve of the present embodiment sample and lower layer's sample at the middle and upper levels are as shown in Figure 8；In modification
The TA test curve and DTA test curve of layer sample and modified lower layer's sample are as shown in Figure 9.
It is calculated according to the data of Fig. 8 and Fig. 9:
1 is completely melt a little:
DTA (SAP) difference | lower layer-upper layer |: 0.377-0.289=0.088
DTA (no SAP) difference | lower layer-upper layer |: 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 layer-upper layer |: 0.548-0.500=0.0048
DTA (no SAP) difference | lower layer-upper layer |: 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 layer-upper layer |: 41.94%-41.15%=0.79% (dehydration rate difference)
TA (no SAP) difference | lower layer-upper layer |: 66.93%-41.01%=22.92%
| DTA (no SAP) difference |-| TA (SAP) difference |/| DTA (no SAP) difference | the > of (100%)=96.5% 95%
The super absorbent resin (polyacrylate) and sodium carboxymethylcellulose that calculated result shows 5wt% are to six water
The mutually layering modified effect of calcium chloride is bad, is not avoided that layering.
As can be seen from the above embodiments, test method provided by the invention can to inorganic phase-changing material modified effect into
The accurate objectively analysis of row.
The above is only a preferred embodiment of the present invention, it is not intended to limit the present invention in any form.It should
It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make
Dry improvements and modifications, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (7)
1. a kind of test method of inorganic phase-changing material modified effect, comprising the following steps:
(1) inorganic phase-changing material is heated to melting, obtains stratified liquid；It is respectively extracted in the upper and lower of the stratified liquid
Partially liq, and mark sample position；
(2) liquid that the step (1) is extracted with lower layer at the middle and upper levels is distinguished into decrease temperature crystalline, obtains upper layer sample and lower layer's sample
Product；
(3) remaining liq after extracting in the step (1) is mixed with the thickener of certain volume, obtains modified solution；
(4) it corresponds to after the mark in step (1) distinguishes extraction section liquid and cools down in the modified solution that the step (3) obtains
Crystallization obtains modified upper layer sample and modified lower layer's sample；
(5) the modification upper layer sample that the upper layer sample and lower layer's sample and the step (4) obtained to the step (2) obtains
Differential thermal analysis and thermogravimetric analysis are carried out respectively with modified lower layer's sample, obtain differential thermal analysis result and thermal gravimetric analysis results；
(6) inorganic phase-changing material is calculated according to differential thermal analysis result and is completely melt the corresponding heat of temperature before and after adding thickener
Flow difference ratio A hot-fluid difference ratio B corresponding with dehydration temperaturre is started；
The quality difference value ratio of thermogravimetric analysis point of the inorganic phase-changing material before and after adding thickener is calculated according to thermal gravimetric analysis results
C；
Wherein, A=(D1-D2)/D1；B=(D3-D4)/D3；C=(M1-M2)/M1；
D1For the difference for being completely melt the heat flow value of the corresponding upper layer sample of temperature and the heat flow value of lower layer's sample；
D2For the difference for being completely melt the heat flow value of the corresponding modified upper layer sample of temperature and the heat flow value of modified lower layer's sample；
D3For the difference for starting the heat flow value of the corresponding upper layer sample of dehydration temperaturre and the heat flow value of lower layer's sample；
D4For the difference for starting the heat flow value of the corresponding modified upper layer sample of dehydration temperaturre and the heat flow value of modified lower layer's sample；
M1For the difference of the quality of the quality and lower layer's sample of the corresponding upper layer sample of heat analysis emphasis；
M2For the difference of the quality of the quality and modified lower layer's sample of the corresponding modified upper layer sample of heat analysis emphasis；
The value that the value of the A is 85% or more, B is 70% or more, and the value of C be 95% or more when, the thickening of the volume
Agent can be effectively improved the lamination of inorganic phase-changing material；
The inorganic phase-changing material includes crystalline hydrate salt phase-change material；
The thickener includes super absorbent resin and/or sodium carboxymethylcellulose；
Mixing in the step (3) carries out under agitation；The rate of the stirring is 400~600r/min；It is described to stir
The time mixed is 15~25min.
2. the method according to claim 1, wherein the crystalline hydrate salt phase-change material includes Na2SO4·
10H2O、CaCl2·6H2O or Na2HPO4·12H2O。
3. the method according to claim 1, wherein the thickener does not expand at 200~250 DEG C and object
Physicochemical character is constant.
4. the method according to claim 1, wherein the step (1) extracts the body of liquid with lower layer at the middle and upper levels
Product independently is 0.3~0.6mL.
5. the method according to claim 1, wherein the liquid drop that the step (2) is extracted with lower layer at the middle and upper levels
The rate of temperature independently is 1~3 DEG C/min.
6. the method according to claim 1, wherein the step (4) extracts the body of liquid with lower layer at the middle and upper levels
Product independently is 0.3~0.6mL.
7. method according to claim 1 or 6, which is characterized in that the liquid that the step (4) is extracted with lower layer at the middle and upper levels
The rate of cooling independently is 1~3 DEG C/min.
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