Experiments, similar to those conducted using distilled water, were also carried out using 0.1 M NaCl solution. Results of the sorption of brine on time dependence were similar to results of moisture sorption.
0,0 0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 1,8
0 24 48 72 96 120 time (h)144 168 192 216 240
weight change (%)
FATRAFOL 804 STAFOL 914 PVC PVC/30B5 PVC/Na5
PVC/Na5/PEG/IDP PVC/Na/5PEG PVC/30B 3/TCP PVC/30B5/TCP PVC/30B5/IDP
PVC/Na3/DEG/TCP PVC/Na3/DEG/DCP PVC/Na3/DEG1
Fig. 30 Weight change of samples during exposing in 0.1 M NaCl solution as a function of time
Table 5 Measured and calculated values of brine (0.1 M NaCl) diffusivity and equilibrium weight gain of prepared samples and commercial membranes
system c (%)
Diffusion Coefficient x
1014 (m2/s)
cs (%)
STAFOL 914 0,41 7,04 0,52
FATRAFOL 804 0,12 916,00 0,16
FATRAFOL 803 0,08 35,54 0,16
PVC 0,09 11,83 0,19
PVC/30B5 0,45 0,57 1,80
PVC/Na5 0,86 25,02 0,89
PVC/Na5/PEG/IDP 0,81 0,22 1,90
PVC/Na5/PEG 1,62 10,73 1,67
PVC/30B 3/TCP 0,36 11,13 0,47
PVC/30B5/TCP 0,50 38,27 0,52
PVC/30B5/IDP 0,49 5,77 0,51
PVC/Na3/DEG/TCP 1,01 3,92 1,02
PVC/Na3/DEG/DCP 1,11 13,37 1,25
PVC/Na3/DEG1 1,52 19,64 1,56
When one compares the result presented in Table 4 with those given in Table 5, one notice that clay is much less effective in reducing the diffusivity of brine than distilled water, and brine is adsorbed to a much lesser extent on the clay particles. These expectations are simi-lar as in Rana’s research [35].
As further Figures 31 and 32 show, differences between percentage areal weight change and percentage weight change are minimal. It could be say that materials containing nano-filler Cloisite® 30B performed the best resistance to sorption of brine than .
-0,01
percentage areal weight change percentage areal weight change after drying
Fig. 31 Percentage areal weight change before and after drying
-0,5
percentage weight change percentage weight change after drying
Fig. 32 Percentage weight change during exposing before and after drying
CONCLUSION
Significant progress in the development of polymer/clay nanocomposites has been made over the past one and a half decades.
Clay was chosen as filler due to the its low loading range. The ability of clays to organize and direct polymer nanocomposites synthesis comes from a number of unique structural and chemical properties. From the smectite group, the best known and widely utilized clay is montmorillonite.
There are many articles with information about improving barrier properties by adding nanofilles. It is necessary to check this theory practically.
Because of this PPVC was chosen as polymer matrix. It is an example of common plastics material with good barrier properties as a pure material. In fact, the research of barrier properties of PVC/clay nanocomposites has only begun.
Nanocomposite samples with two types of fillers, namely Cloisite Na+ and Cloisite 30B, were prepared using different amount of intercalation and co-intercalation agents.
Then, these samples were compared with commercial membranes.
In present work, barrier properties using Permeability, WVTR, Diffusion coefficient and mass changes at saturation were determined by measuring the changes in weight. It was found out that our prepared samples have significantly better barrier properties than com-mercial membranes. Generally it could be say, the addition of Cloisite 30B and subse-quent co-intercalation lead to the better barrier properties, namely permeability decreased about 23% by Water method and 70% by Desiccant method. Permeation experiments are thus preferable to sorption experiments, and these might even be used to estimate effec-tiveness of a given processing techniques to exfoliate platelets.
It could be also said, that enhancement of barrier properties was achieved using only 3wt%
of nanofiller. From comparing diffusion coefficients of some materials in different solu-tions could be found out that increasing diffusion coefficient value was corresponded with reducing mass change at saturation. This result could be explained based on the hydrophilic nature of the clay surface that tends to immobilize some of the moisture. Moreover it could be deduced that materials with 3wt% nanofiller content had lower diffusion coefficient than with 5wt%.
It is necessary to note that barrier properties depend on type of nanofiller, using intercala-tion and co-intercalaintercala-tion agents and on intercalaintercala-tion/exfoliaintercala-tion degree of nanofiller in polymer matrix.
At the end, we could suggest, that new types of materials utilized as insulation membranes were found.
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LIST OF USED SYMBOLS AND ABBREVIATIONS
PCN Polymer/clay nanocomposites XRD X-ray diffraction
CEC Cation exchange capacity PVC Poly(vinyl chloride) PA 6 Polyamide 6
PE Polyethylene
PET Polyethyleneterephtalate PP Polypropylene
PEO Polyethyleneoxide PS Polystyrene
UPVC Non-plasticized polyvinyl chloride PPVC Plasticized polyvinyl chloride MMT Montmorillonite
P Permeability Slope of the straight line
Saturation vapour pressure at test temperature
Relative humidity at the source and at the vapour sink Test area
Time
Water vapour transmission rate Weight change
Bm m0 m1
c m1
m2
m3 Mt M∞
cs
t
Change of weight
Weight of samples before measurement Weight of samples after time t
Water content
Mass of the test specimen after initial drying and before immersion Mass of the test specimen after immersion
Mass of the test specimen after initial drying and final drying Mass gain at reduced time
Maximum mass gain at the equilibrium state Water content at saturation
time of immersion of the test specimen in water or humid air
LIST OF FIGURES
Fig. 1 Polymer/clay nanocomposites ... 10
Fig. 2 Ion-exchange intercalation ... 12
Fig. 3 Ion-dipole intercalation ... 12
Fig. 4 The in-situ polymerization ... 13
Fig. 5 The melt intercalation process ... 14
Fig. 6 Si-Tetrahedron and Al-Octahedron ... 20
Fig. 7 The tetrahedral sheet ... 21
Fig. 8 The octahedral sheet ... 21
Fig. 9 The structure of 2:1 layered silicate ... 23
Fig. 10 The tortuous path migration... 26
Fig. 11 Weight decrease as a function of time ... 43
Fig. 12 Weight decrease on time dependence – materials with smaller weigh decrease than unfilled PVC compound ... 44
Fig. 13 Graphic comparison of calculated water vapour transmission rate comparison of samples ... 45
Fig. 14 Percentage comparison of mathematical WVTR to unfilled PVC compound both after 1 day and 1 month measuring ... 45
Fig. 15 Graphic permeability comparison of samples ... 46
Fig. 16 Percentage comparison of moisture permeability of tested samples to unfilled PVC compound both after 1 day and 1 month measuring ... 47
Fig. 17 Weight-gain as a function of time ... 48
Fig. 18 Comparison of permeability measured using Water and Desiccant methods ... 49
Fig. 19 Comparison of WVTR measured by Water and Desiccant methods ... 49
Fig. 20 Weight changes during swelling as a function of time ... 51
Fig. 21 FTIR spectra of octane, in which PVC samples were swelled ... 52
Fig. 22 FTIR spectra of PVC/Na3/DEG 1 during swelling ... 53
Fig. 23 FTIR spectra of PVC/30B5/IDP ... 53
Fig. 24 Weight changes of samples before and after drying ... 54
Fig. 25 Determination of water-soluble matter lost during immersion in water at 23°C ... 55
Fig. 26 Determination of water content absorbed after 192 hour immersion in water at 23°C ... 57 Fig. 27 Determination of water-soluble matter lost during immersion in water at 23°C ... 58 Fig. 28 Time dependence on water content absorbed after 2 hour immersion in
boiling water ... 59 Fig. 29 Determination of water content absorbed after 2 hour immersion in boiling
water ... 59 Fig. 30 Weight change of samples during exposing in 0.1 M NaCl solution as a
function of time ... 60 Fig. 31 Percentage areal weight change before and after drying ... 62 Fig. 32 Percentage weight change during exposing before and after drying ... 62
LIST OF TABLES
Table 1 Composition of the PVC compound used for foil production ... 34 Table 2 Some typical properties of Cloisite® 30B and Cloisite® Na+ ... 35 Table 3 Composition of PVC/clay nanocomposites ... 38 Table 4 Calculated values of moisture diffusivity and equilibrium moisture content
of prepared samples and commercial membranes ... 56 Table 5 Measured and calculated values of brine (0.1 M NaCl) diffusivity and
equilibrium weight gain of prepared samples and commercial membranes ... 61 Table 6 Calculated data of water vapour transmission method after 1 day using
Water method ... 74 Table 7 Calculated data of water vapour transmission method after 1 month using
Water Method ... 75 Table 8 Calculated data of water vapour transmission method after 1 day using
Desiccant method... 76 Table 9 Calculated data of water vapour transmission method after 1 month using
Desiccant Method ... 76 Table 10 Calculated data of solvent resistance method ... 77 Table 11 Calculated water-soluble matter lost during immersion at 23°C ... 77
APPENDIX
Table 6 Calculated data of water vapour transmission method after 1 day using Water method
system after 24 hours WVT [g/h.m2] ∆ % P [g/Pa.s.m] ∆ % PVC/Na5/DEG0.5 58,01 53,50 583,15 4,48E-10 4,29E-10 484,35 PVC/Na3/DEG0.5 3,68 1,35 -56,61 3,09E-11 1,16E-11 -59,65
PVC/Na5/DEG1 9,00 8,09 6,03 8,22E-11 7,37E-11 7,23
PVC/Na3/DEG1 7,63 5,14 -10,21 7,46E-11 5,36E-11 -2,63 PVC/Na5/DEG/DCP 4,02 0,50 -52,64 3,80E-11 5,24E-12 -50,36 PVC/Na3/DEG/DCP 1,79 0,34 -78,92 1,37E-11 3,41E-12 -82,06 PVC/Na5/DEG0,5/TCP 3,09 1,02 -63,64 3,01E-11 1,02E-11 -60,71 PVC/Na3/DEG0,5/TCP 23,45 30,10 176,08 2,73E-10 3,48E-10 256,71 PVC/Na5/DEG/TCP 3,23 1,84 -61,96 3,73E-11 2,07E-11 -51,28 PVC/Na3/DEG/TCP 2,07 1,38 -75,59 2,02E-11 1,30E-11 -73,60 PVC/Na5/DEG/IDP 33,07 22,50 289,41 3,98E-10 2,72E-10 419,40 PVC/Na3/DEG/IDP 2,04 0,23 -75,99 2,02E-11 1,98E-12 -73,64
PVC/Na5/PEG 3,24 1,22 -61,80 3,86E-11 1,37E-11 -49,58
PVC/Na5/PEG/DOP 7,83 2,26 -7,81 7,75E-11 2,53E-11 1,17 PVC/Na5/PEG/TCP 4,27 2,50 -49,71 4,23E-11 2,48E-11 -44,74 PVC/Na5/PEG/IDP 6,77 2,82 -20,27 4,98E-11 2,05E-11 -34,97
PVC/Na5 10,56 7,97 24,33 9,17E-11 6,71E-11 19,71
PVC/30B5 3,57 1,78 -58,02 3,14E-11 1,54E-11 -59,07
PVC/30B5/IDP 6,01 4,17 -29,26 5,88E-11 4,32E-11 -23,20 PVC/30B5/TCP 2,80 1,67 -67,07 2,95E-11 1,74E-11 -61,48 PVC/30B 3/TCP 2,17 1,76 -74,39 2,28E-11 1,86E-11 -70,26
PVC/IDP 2,72 1,74 -67,92 2,65E-11 1,89E-11 -65,41
PVC/TCP 5,36 3,10 -36,86 5,30E-11 3,20E-11 -30,86
FILM 902 0,96 0,19 -88,74 7,80E-12 1,37E-12 -89,82
Blood can 0,64 0,09 -92,45 2,08E-11 2,69E-12 -72,84
FATRAFOL 803 0,81 0,67 -90,41 8,44E-11 6,96E-11 10,12
STAFOL 914 0,48 0,11 -94,39 2,52E-11 3,93E-13 -67,15
PVC 8,49 6,66 0,00 7,66E-11 6,16E-11 0,00
Table 7 Calculated data of water vapour transmission method after 1 month using Water Method
system after 1 month WVT [g/h.m2] ∆ % P [g/Pa.s.m] ∆ % PVC/Na5/DEG0.5 2,67 1,76 251,91 2,04E-11 1,42E-11 206,65
PVC/Na3/DEG0.5 1,24 0,53 63,30 1,02E-11 3,86E-12 53,81
PVC/Na5/DEG1 2,02 1,76 166,48 1,83E-11 1,61E-11 175,15
PVC/Na3/DEG1 0,71 0,16 -6,04 6,81E-12 1,19E-12 2,53
PVC/Na5/DEG/DCP 0,86 0,08 13,92 8,14E-12 5,84E-13 22,57
PVC/Na3/DEG/DCP 0,89 0,08 17,94 6,74E-12 1,44E-13 1,47
PVC/Na5/DEG0,5/TCP 0,84 0,15 10,34 8,13E-12 1,47E-12 22,45 PVC/Na3/DEG0,5/TCP 0,65 0,11 -13,69 8,30E-12 2,07E-12 25,02 PVC/Na5/DEG/TCP 0,65 0,07 -14,69 7,66E-12 6,12E-13 15,43
PVC/Na3/DEG/TCP 0,67 0,07 -11,35 6,67E-12 5,16E-13 0,42
PVC/Na5/DEG/IDP 1,37 0,46 81,08 1,64E-11 5,72E-12 147,81
PVC/Na3/DEG/IDP 0,70 0,12 -7,00 6,97E-12 1,08E-12 5,04
PVC/Na5/PEG 0,54 0,09 -28,25 6,29E-12 8,04E-13 -5,23
PVC/Na5/PEG/DOP 1,35 0,89 78,22 1,22E-11 8,43E-12 83,26
PVC/Na5/PEG/TCP 0,72 0,19 -4,58 7,16E-12 1,84E-12 7,87
PVC/Na5/PEG/IDP 0,87 0,11 14,83 6,37E-12 5,81E-13 -4,07
PVC/Na5 0,81 0,29 7,37 7,25E-12 2,59E-12 9,25
PVC/30B5 0,73 0,10 -3,21 6,46E-12 8,16E-13 -2,67
PVC/30B5/IDP 0,52 0,01 -30,80 4,60E-12 8,09E-13 -30,76
PVC/30B5/TCP 0,52 0,09 -31,60 5,48E-12 9,48E-13 -17,50
PVC/30B 3/TCP 0,51 0,07 -32,46 5,31E-12 7,15E-13 -20,05
PVC/IDP 0,83 0,17 9,83 7,88E-12 2,07E-12 18,69
PVC/TCP 1,23 1,08 62,10 1,19E-11 1,07E-11 79,81
FILM 902 1,49 0,33 96,70 1,22E-11 2,78E-12 84,32
Blood can 0,47 0,05 -37,33 1,54E-11 1,74E-12 132,31
FATRAFOL 803 0,56 0,59 -25,90 5,81E-11 6,12E-11 775,89
STAFOL 914 0,43 0,17 -43,31 2,69E-11 1,07E-11 305,21
PVC 0,76 0,08 0,00 6,64E-12 1,09E-12 0,00
Table 8 Calculated data of water vapour transmission method after 1 day using Desiccant method
system after 24 hours WVT [g/h.m2] ∆ % P [g/Pa.s.m] ∆ % PVC/Na3/DEG1 0,45 0,21 73,42 3,84E-12 1,62E-12 -24,20 PVC/Na3/DEG/DCP 0,28 0,01 8,70 2,36E-12 1,28E-13 -53,52 PVC/Na3/DEG/TCP 0,25 0,05 -1,38 2,50E-12 4,18E-13 -50,67 PVC/30B5/IDP 0,15 0,05 -42,66 1,69E-12 5,48E-13 -66,65 PVC/30B5/TCP 0,16 0,06 -35,99 1,58E-12 6,03E-13 -68,77 PVC/30B 3/TCP 0,19 0,13 -25,17 1,71E-12 1,13E-12 -66,29 PVC/Na5/PEG 0,17 0,08 -33,27 1,92E-12 9,15E-13 -62,08 PVC/Na5/PEG/IDP 0,36 0,07 41,66 2,96E-12 1,50E-13 -41,72
PVC/Na5 0,43 0,10 65,27 3,67E-12 8,70E-13 -27,68
PVC/30B5 0,26 0,19 2,17 9,48E-12 6,85E-12 86,94
FILM 902 0,36 0,03 38,77 2,86E-12 1,43E-13 -43,52
Blood can 0,12 0,04 -54,91 3,76E-12 1,45E-12 -25,84
FATRAFOL 803 0,22 0,09 -13,39 1,31E-11 5,43E-12 158,03
STAFOL 914 0,26 0,02 0,64 1,22E-11 1,34E-12 139,72
PVC 0,26 0,12 0,00 5,07E-12 2,45E-12 0,00
Table 9 Calculated data of water vapour transmission method after 1 month using Desic-cant Method
system after 1 month WVT [g/h.m2] ∆ % P [g/Pa.s.m] ∆ %
PVC/Na3/DEG1 0,57 0,15 28,18 5,00E-12 1,01E-12 -42,92
PVC/Na3/DEG/DCP 0,45 0,02 1,33 3,82E-12 2,86E-13 -56,45
PVC/Na3/DEG/TCP 0,36 0,03 -18,41 3,60E-12 2,70E-13 -58,95
PVC/30B5/IDP 0,22 0,03 -49,89 2,59E-12 2,55E-13 -70,48
PVC/30B5/TCP 0,26 0,06 -42,24 2,47E-12 5,63E-13 -71,81
PVC/30B 3/TCP 0,29 0,08 -35,51 2,62E-12 5,72E-13 -70,11
PVC/Na5/PEG 0,32 0,04 -28,48 3,58E-12 4,43E-13 -59,21
PVC/Na5/PEG/IDP 0,53 0,05 17,71 4,45E-12 9,85E-13 -49,30
PVC/Na5 0,53 0,08 19,50 4,60E-12 7,02E-13 -47,52
PVC/30B5 0,20 0,03 -56,19 7,11E-12 1,08E-12 -18,95
FILM 902 0,60 0,01 33,60 4,80E-12 2,13E-13 -45,28
Blood can 0,31 0,03 -29,70 1,01E-11 9,90E-13 15,60
FATRAFOL 803 0,22 0,09 -50,12 2,31E-11 8,98E-12 162,93
STAFOL 914 0,26 0,02 -42,04 1,62E-11 1,54E-12 84,22
PVC 0,45 0,14 0,00 8,77E-12 2,92E-12 0,00
Table 10 Calculated data of solvent resistance method