CN204330641U - A kind of in-situ testing device for studying crystalline polymer transformation behavior - Google Patents
A kind of in-situ testing device for studying crystalline polymer transformation behavior Download PDFInfo
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- CN204330641U CN204330641U CN201520012193.2U CN201520012193U CN204330641U CN 204330641 U CN204330641 U CN 204330641U CN 201520012193 U CN201520012193 U CN 201520012193U CN 204330641 U CN204330641 U CN 204330641U
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Abstract
The utility model relates to a kind of in-situ testing device for studying crystalline polymer transformation behavior, and described device comprises two ingredients, is respectively heating arrangement and in-situ testing device.Described heating arrangement comprises the canister 2 of temperature programmed control thermal station 1 and particular design, and the wall of described canister 2 apart from 4mm place, bottom has a series of circular hole 3.Described in-situ testing device comprises described canister 2, tank 4, thermopair 5, stationary installation 6 and temperature-shrink crack 7.Described tank 4 upper right side is provided with water inlet 8, and lower left is provided with water delivering orifice 9.The compensating wire 10 being connected described thermopair 5 and described temperature-shrink crack 7 is provided with between described thermopair 5 with described temperature-shrink crack 7.Described stationary installation 6 is positioned at directly over described tank 4.The utility model is specially adapted to the in-situ test of the non-constant speed transformation behavior of crystalline polymer non-isothermal, has the advantages such as device is simple, testing result is accurate, cost is low, detecting step is quick.
Description
Technical field
The utility model relates to a kind of pick-up unit, specifically a kind of simply, fast and accurately in-situ test go out the pick-up unit of crystalline polymer transformation behavior.
Background technology
Phase-changing energy storage material (PCM) is a kind of material with stored energy function.Utilize phase-change material heat accumulation and put thermal property, can be used for the storage of aviation field and sun power, industrial exhaust heat, also can be applied to the industry such as electronics, building as temperature control material, there is wide market application foreground.For some macromolecule material products, usually use under the high temperature conditions, therefore during test products performance, measure the content that its phase transition temperature becomes very necessary.The actual production process of macromolecular material as extruded, injection moulding, blowing etc. normally completes under dynamic non-isothermal, therefore has important practice significance and theory value to the research of the transformation behavior under dynamic condition.Research crystalline polymer transformation behavior, has directive function to the research of phase-changing energy storage material, test products performance and polymer processing methodology optimization etc.
At present, the device used when detecting crystalline polymer transformation behavior both at home and abroad mainly comprises: the differential scanning calorimeter be made up of main frame, mechanical refrigeration system, low temperature drier and sample pressure-like machine etc.; By the x-ray diffractometer of the adjusting mechanism system of high stable x-ray source, sample and sample position orientation, ray detector and diffraction pattern Treatment Analysis System's composition; By the infrared spectrometer of light source, monochromator, detector and computer treatmenting information System's composition; And the polarizing microscope etc. to be made up of light source, eyepiece, condenser and Portland lens.Though each tool advantage of these determinators, also there are some defects simultaneously.The structure of these pick-up units is all very complicated, and acquisition cost is high, and some device practical operation is relatively loaded down with trivial details.When detecting degree of transformation as utilized X-ray diffraction method and polarizing microscope, these two kinds of method workloads are large, and can not test continuously and quantitatively.In addition, the compressing tablet of polarizing microscope and sample preparation more difficult; The mensuration mode of infrared analysis method when sample reaches melting is difficult to process, though cause the method possible in theory, practical operation also not easily realizes.Differential scanning calorimetery is usually only for detecting the phase transition process of isothermal crystal and non-isothermal, constant speed crystallization process, and cost is relatively high.
In actual process operation process, the transformation behavior many places of crystalline polymer are under the non-isokinetic conditions of non-isothermal, to the transformation behavior under the non-isokinetic conditions of crystalline polymer non-isothermal, still lack lower, simple to operate, the consuming time short and determinator accurately of cost at present.Therefore, be necessary that developing a kind of simple mechanism measures the transformation behavior of crystalline polymer under non-isothermal, non-constant speed cooling conditions.
Utility model content
The utility model provides a kind of in-situ testing device for studying crystalline polymer transformation behavior, and it can measure the phase transition process of crystalline polymer simply, quickly and accurately.
The in-situ testing device of the crystalline polymer transformation behavior designed by the utility model, the unique point on the Temperature-time change curve obtained by in-situ test, thus determine crystalline polymer transition temperature range.As follows to theoretical analysis of the present utility model: crystalline polymer is cooled to the process of room temperature from melt temperature, can there is certain transformation in the structure of crystalline polymer, change crystal formation into by armorphous, namely occurs so-called " phase transformation ".The latent heat discharged in phase transition process makes the rate of temperature fall of crystalline polymer slow down, crystalline polymer self-temperature is even caused not change within a certain period of time, make a temperature platform appears in the Temperature-time change curve that obtained by in-situ test, feature can determine the generation of crystalline polymer phase transformation accordingly, and obtain its temperature range undergone phase transition.
In-situ testing device for studying crystalline polymer transformation behavior described in the utility model, described device comprises two parts, is respectively heating arrangement and in-situ testing device; Described heating arrangement is temperature programmed control warm table (1); Described in-situ testing device comprises canister (2), tank (4), thermopair (5), stationary installation (6) and temperature-shrink crack (7); Described tank (4) upper right side is provided with water inlet (8), lower left is provided with water delivering orifice (9), is provided with the compensating wire (10) being connected described thermopair (5) and described temperature-shrink crack (7) between described thermopair (5) with described temperature-shrink crack (7); Described stationary installation (6) is positioned at directly over described tank (4).
Warm table 1 described in the utility model is temperature programmed control warm table, and warm table can be changed, and can carry out the warm table of temperature programmed control.
The body prioritizing selection radius of the canister 2 of particular design described in the utility model is 20mm, height is the cylindrical rustless steel container of 10mm, on its wall, the radius of circular hole should control between 0.5 ~ 1.0mm, namely to ensure that chilled water can flow in described canister 2 unobstructedly, ensure the height of the height of water higher than described polymer melt 11 again.
The water inlet 8 of described tank 4 and the water velocity of water delivering orifice 9 need be consistent, constant with the water surface elevation maintained in tank 4.
Thermopair 5 described in the utility model is T-shaped thermopair, thermopair can be changed, also common K type thermopair can be changed to, meanwhile, the compensating wire 10 for connecting described thermopair 5 and described temperature-shrink crack 7 described in the utility model also correspondingly should be replaced by the compensating wire being applicable to described K type thermopair.
Stationary installation 6 described in the utility model is fixture, and replaceable is other stationary installations, ensures that described thermopair 5 polymer melt 11 inside in described canister 2 maintains static.
The concrete detecting step of the in-situ testing device for studying crystalline polymer transformation behavior described in the utility model is as follows:
(1) open temperature programmed control thermal station 1, arranging heating-up temperature is 190 ~ 230 DEG C;
(2) treat that programmable temperature control thermal station 1 temperature reaches preset temperature, canister 2 is positioned over preheating 5min in programmable temperature control thermal station 1;
(3) put into bottom canister 2 gradually by polymkeric substance (about 1g), the complete melting of thing to be polymerized is melt, then is incubated 15min;
(4) canister 2 is taken off, T-shaped thermopair 5 is inserted the half position that melt center is about thickness, and this canister 2 is put into the tank 4 containing chilled water, be fixed in the melt in canister 2 by stationary installation 6 by T-shaped thermopair 5, test end temp is identical with room temperature (about 20 DEG C);
(5) temperature value in the whole temperature-fall period of above-mentioned (4) step is gathered with the temperature-shrink crack 7 of connecting T-shaped thermopair;
(6) to temperature value and the time value Plotting data Temperature-time change curve of above-mentioned (5) step collection, according to temperature time dependent unique point determination crystalline polymer transition temperature range on this change curve.
The utility model is specially adapted to the in-situ test of crystalline polymer non-isothermal, non-constant speed cooling transformation behavior, has the features such as device is simple, testing result is accurate, cost is low, detecting step is quick.
Accompanying drawing explanation
Fig. 1 is the structural representation of heating arrangement in the in-situ testing device for studying crystalline polymer transformation behavior.
Wherein: temperature programmed control thermal station 1, canister 2, circular hole 3.
Fig. 2 is the structural representation of the in-situ testing device situ proving installation for studying crystalline polymer transformation behavior.
Wherein: canister 2, tank 4, thermopair 5, stationary installation 6, temperature-shrink crack 7, water inlet 8, water delivering orifice 9, compensating wire 10, crystalline polymer melt 11.
The high density polyethylene original position temperature lowering curve of Fig. 3 to be the trade mark of the Jilin Petrochemical adopting the utility model device to record be 9455F.
The Low Density Polyethylene original position temperature lowering curve of Fig. 4 to be the trade mark of the Lanzhou Petrochemical adopting the utility model device to record be 2426K.
The high density polyethylene original position temperature lowering curve of Fig. 5 to be the trade mark of the DOW Chemical adopting the utility model device to record be 40055E.
Embodiment
Below in conjunction with accompanying drawing, carry out description that is clear, integrality to the utility model, described embodiment is only the utility model part embodiment, and scope of the present utility model is not by the restriction of these embodiments.
Embodiment 1:
In-situ testing device structural representation for studying crystalline polymer transformation behavior described in the utility model as shown in Figure 1 and Figure 2.
Described device comprises two parts, is respectively heating arrangement and in-situ testing device.Described heating arrangement comprises the canister 2 of temperature programmed control thermal station 1 and particular design, described canister 2 for radius be 20mm, height is the cylindrical rustless steel container of 10mm, on described canister 2 bottom distance 4mm place wall on offer the circular hole 3 that 30 radiuses are 0.75mm, to make chilled water enter in described canister 2, polymer melt 11 is cooled.Described in-situ testing device comprises described canister 2, tank 4, T-shaped thermopair 5, stationary installation (fixture) 6 and temperature-shrink crack 7.Described tank 4 upper right side is provided with water inlet 8, and lower left is provided with water delivering orifice 9, to make the moment in described tank 4 be full of chilled water, makes the coolant temperature around described polymer melt 11 constant.The thermocouple wire 10 being connected described thermopair 5 and described temperature-shrink crack 7 is provided with between described thermopair 5 with described temperature-shrink crack 7.Described stationary installation 6 is positioned at directly over described tank 4, for fixing described canister 2.
The concrete detecting step of the in-situ testing device for studying crystalline polymer transformation behavior described in the utility model is as follows:
(1) open temperature programmed control thermal station 1, arranging heating-up temperature is 210 DEG C;
(2) treat that programmable temperature control thermal station 1 temperature reaches preset temperature 210 DEG C, canister 2 is positioned over preheating 5min in programmable temperature control thermal station 1;
(3) be that the high density polyethylene 1.0g of 9455F adds bottom canister 2 gradually by the trade mark of Jilin Petrochemical, the complete melting of thing to be polymerized is melt, then is incubated 15min;
(4) canister 2 is taken off, T-shaped thermopair 5 is inserted the half that melt center is about thickness, and this canister 2 is put into the tank 4 containing chilled water, the polymer melt be fixed in canister 2 by T-shaped thermopair 5 by stationary installation (fixture) 6 is inner, and test end temp is identical with room temperature (about 20 DEG C);
(5) temperature value in the whole temperature-fall period of above-mentioned (4) step is gathered with the temperature-shrink crack 7 of connecting T-shaped thermopair;
(6) temperature value and time value data that above-mentioned (5) step gathers are mapped, drafting Temperature-time change curve.
By above-mentioned steps, this change curve is the transition temperature range of the high density polyethylene of 9455F according to the trade mark of temperature time dependent unique point determination Jilin Petrochemical.
The trade mark is as shown in Figure 3 that the Temperature-time change curve of the high density polyethylene of 9455F significantly can find out that the present embodiment 1 is from 127.43 DEG C, temperature deviate from original linear track over time, when temperature is down to below 118.64 DEG C, temperature is tending towards linear track again over time.Can determine that the phase transformation initial temperature of this high density polyethylene under this test technology condition is 127.43 DEG C thus, phase transformation end temp is 118.64 DEG C.
Embodiment 2:
In-situ testing device structural representation for studying crystalline polymer transformation behavior described in the utility model as shown in Figure 1 and Figure 2.
Described device comprises two parts, is respectively heating arrangement and in-situ testing device.Described heating arrangement comprises the canister 2 of temperature programmed control thermal station 1 and particular design, described canister 2 for radius be 20mm, height is the cylindrical rustless steel container of 10mm, on described canister 2 bottom distance 4mm place wall on offer the circular hole 3 that 30 radiuses are 0.5mm, to make chilled water enter in described canister 2, polymer melt 11 is cooled.Described in-situ testing device comprises described canister 2, tank 4, T-shaped thermopair 5, stationary installation (fixture) 6 and temperature-shrink crack 7.Described tank 4 upper right side is provided with water inlet 8, and lower left is provided with water delivering orifice 9, to make the moment in described tank 4 be full of chilled water, makes the coolant temperature around described polymer melt 11 constant.The compensating wire 10 being connected described thermopair 5 and described temperature-shrink crack 7 is provided with between described thermopair 5 with described temperature-shrink crack 7.Described stationary installation 6 is positioned at directly over described tank 4, for fixing described canister 2.
The concrete detecting step of the in-situ testing device for studying crystalline polymer transformation behavior described in the utility model is as follows:
(1) open temperature programmed control thermal station 1, arranging heating-up temperature is 200 DEG C;
(2) treat that programmable temperature control thermal station 1 temperature reaches preset temperature 200 DEG C, canister 2 is positioned over preheating 5min in programmable temperature control thermal station 1;
(3) be that the Low Density Polyethylene 1.0g of 2426K adds bottom canister 2 gradually by the trade mark of Lanzhou Petrochemical, thing to be polymerized is completely molten is melt, then is incubated 15min;
(4) canister 2 is taken off, T-shaped thermopair 5 is inserted the half that melt center is about thickness, and this canister 2 is put into the tank 4 containing chilled water, be fixed in the melt in canister 2 by stationary installation (fixture) 6 by T-shaped thermopair 5, test end temp is identical with room temperature (about 20 DEG C);
(5) temperature value in the whole temperature-fall period of above-mentioned (4) step is gathered with the temperature-shrink crack 7 of connecting T-shaped thermopair;
(6) temperature value and time value data that above-mentioned (5) step gathers are mapped, drafting Temperature-time change curve.
By above-mentioned steps, this change curve is the transition temperature range of the Low Density Polyethylene of 2426K according to the trade mark of temperature time dependent unique point determination Lanzhou Petrochemical.
The trade mark is as shown in Figure 4 that the Temperature-time change curve of the Low Density Polyethylene of 2426K significantly can find out that the present embodiment 2 is from 102.69 DEG C, temperature deviate from original linear track over time, when temperature is down to below 93.03 DEG C, temperature is tending towards linear track again over time.Can determine that the phase transformation initial temperature of this Low Density Polyethylene under this test technology condition is 102.69 DEG C thus, phase transformation end temp is 93.03 DEG C.
Embodiment 3:
In-situ testing device structural representation for studying crystalline polymer transformation behavior described in the utility model as shown in Figure 1 and Figure 2.
Described device comprises two parts, is respectively heating arrangement and in-situ testing device.Described heating arrangement comprises the canister 2 of temperature programmed control thermal station 1 and particular design, described canister 2 for radius be 20mm, height is the cylindrical rustless steel container of 10mm, on described canister 2 bottom distance 4mm place wall on offer the circular hole 3 that 30 radiuses are 1.0mm, to make chilled water enter in described canister 2, polymer melt 11 is cooled.Described in-situ testing device comprises described canister 2, tank 4, T-shaped thermopair 5, stationary installation (fixture) 6 and temperature-shrink crack 7.Described tank 4 upper right side is provided with water inlet 8, and lower left is provided with water delivering orifice 9, to make the moment in described tank 4 be full of chilled water, makes the coolant temperature around described polymer melt 11 constant.The compensating wire 10 being connected described thermopair 5 and described temperature-shrink crack 7 is provided with between described thermopair 5 with described temperature-shrink crack 7.Described stationary installation 6 is positioned at directly over described tank 4, for fixing described canister 2.
The concrete detecting step of the in-situ testing device for studying crystalline polymer transformation behavior described in the utility model is as follows:
(1) open temperature programmed control thermal station 1, arranging heating-up temperature is 210 DEG C;
(2) treat that programmable temperature control thermal station 1 temperature reaches preset temperature 210 DEG C, canister 2 is positioned over preheating 5min in programmable temperature control thermal station 1;
(3) be that the high density polyethylene 1.0g of 40055E adds bottom canister 2 gradually by the trade mark of DOW Chemical, thing to be polymerized is completely molten is melt, then is incubated 15min;
(4) canister 2 is taken off, T-shaped thermopair 5 is inserted the half that melt center is about thickness, and this canister 2 is put into the tank 4 containing chilled water, the polymer melt be fixed in canister 2 by T-shaped thermopair 5 by stationary installation 6 is inner, and test end temp is identical with room temperature (about 20 DEG C);
(5) temperature value in the whole temperature-fall period of above-mentioned (4) step is gathered with the temperature-shrink crack 7 of connecting T-shaped thermopair;
(6) temperature value and time value data that above-mentioned (5) step gathers are mapped, drafting Temperature-time change curve.
By above-mentioned steps, this change curve is the transition temperature range of the high density polyethylene of 40055E according to the trade mark of temperature time dependent unique point determination DOW Chemical.
The trade mark is as shown in Figure 5 that the Temperature-time change curve of the high density polyethylene of 40055E significantly can find out that the present embodiment 3 is from 125.18 DEG C, temperature deviate from original linear track over time, when temperature is down to below 104.24 DEG C, temperature is tending towards linear track again over time.Can determine that the phase transformation initial temperature of this tygon under this test technology condition is 125.18 DEG C thus, phase transformation end temp is 104.24 DEG C.
The foregoing is only embodiment of the present utility model, be not limited to the utility model.The utility model can have various suitable change and change.All do within spirit of the present utility model and principle any amendment, equivalent replacement, improvement etc., all should be included within protection domain of the present utility model.
Claims (10)
1., for studying an in-situ testing device for crystalline polymer transformation behavior, it is characterized in that:
Described device comprises two parts, is respectively heating arrangement and in-situ testing device; Described heating arrangement comprises the canister (2) of warm table (1) and particular design; Described in-situ testing device comprises canister (2), tank (4), thermopair (5), stationary installation (6) and temperature-shrink crack (7); Described tank (4) upper right side is provided with water inlet (8), lower left is provided with water delivering orifice (9), is provided with the compensating wire (10) being connected described thermopair (5) and described temperature-shrink crack (7) between described thermopair (5) with described temperature-shrink crack (7); Described stationary installation (6) is positioned at directly over described tank (4).
2. device according to claim 1, is characterized in that:
Described warm table (1) is temperature programmed control thermal station.
3. device according to claim 1, is characterized in that:
Described canister (2) for radius be 20mm, height is the cylindrical rustless steel container of 10mm, described canister (2) wall has a series of circular hole (3).
4. device according to claim 3, is characterized in that:
Described serial circular hole (3) is positioned on the wall apart from 4mm place, described canister (2) bottom.
5. the device according to claim 3 or 4, is characterized in that:
Described circular hole (3) radius is 0.5 ~ 1.0mm, totally 20 ~ 35.
6. device according to claim 1, is characterized in that:
The water inlet (8) of described tank (4) and the water velocity of water delivering orifice (9) need be consistent.
7. device according to claim 1, is characterized in that:
Described thermopair (5) is T-shaped thermopair.
8. device according to claim 1, is characterized in that:
Described temperature-shrink crack (7) is the special temperature-shrink crack of described thermopair (5).
9. device according to claim 1, is characterized in that:
Described for connecting the special compensating wire that described thermopair (5) is described thermopair (5) with the compensating wire (10) of described temperature-shrink crack (7).
10. device according to claim 1, is characterized in that:
Described stationary installation (6) is fixture.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569032A (en) * | 2015-01-08 | 2015-04-29 | 安徽大学 | In-situ testing device for studying phase transformation behavior of crystalline polymer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104569032A (en) * | 2015-01-08 | 2015-04-29 | 安徽大学 | In-situ testing device for studying phase transformation behavior of crystalline polymer |
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Granted publication date: 20150513 Termination date: 20160108 |