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Carbon Membranes from Polyamideimide and Polyetherimide

Carbon Membranes from Polyamideimide and Polyetherimide

CARBON MEMBRANES FROM POLYAMIDEIMIDE AND POLYETHERIMIDE FOR NITROGEN AND METHANE SEPARATION AND ITS OWN PARAMETER STUDY

ABSTRACT

Carbon membranes well prepared from polyamideimide and polyetherimide had been studied to determine the effects of diverse parameters on membrane qualities. Their homes were analyzed to comprehend its scope in methane purification. Numerous compositions were tried to learn the maximum polymer composition as well as the optimum blend composition. These were pyrolyzed at various temps reflective essay example to study the effect of pyrolysis temperature on the morphology of the membrane. Efforts have been made for obtaining a narrow pore distribution as nitrogen and methane have comparable sizes. Examination of the microstructure of membranes using XRD confirms the variants in chain packing density and d-spacing of polymer chains therefore of a transformation in pyrolysis temperatures. CHN analysis uncovered the percentage composition of unique elements in the membrane as it was important to control amount of oxygen in the membrane. Glass transition temp is found using DSC to verify best blending of polymers. TGA has been done to learn how the polymer composition affects degradation temperature and to study the chemical improvements happening during pyrolysis. SEM images, both cross section, and surface have been taken to analyze pore composition of the membrane.

Keywords: Polyetherimide, Polyamideimide, Pyrolysis, XRD, SEM, CHN.

INTRODUCTION

Membranes have been extensively received as a promising technology in gas separation techniques. This is because of its high stability, low capital expenditure and low energy consumption which overshadow standard gas separation techniques such as for example cryogenic distillation, liquid absorption, pressure swing adsorption etc. These established conventional tactics are recognized for their complexity in functions and high energy intensity. For this reason, researchers are making attempts for an alternative way that promises to give high-cost effectiveness and convenient handling (1).

Polymer membranes have been widely studied for his or her request in gas separating units, nonetheless they always faced disadvantages like low thermal and chemical substance stability. Henceforth studies have been centered on carbon membranes, which are the novel and advanced type of membranes. They have already been giving promising results ever since and marked a fresh benchmark for the selectivity of gasses. Excellent capability to withstand temperature and chemicals made carbon membranes a new branch of review for the researchers to follow. (2)

Carbon membranes are prepared by pyrolysing polymer membranes. Pyrolysis is the most significant part of the preparation of carbon membrane. There are different pyrolysis elements that affect membrane homes. During pyrolysis the parameters like pyrolysis temp, heating rate, atmospheric condition, soaking time etc. can affect the transport houses of the membrane. These factors are chosen wisely based on the application of the membrane. (3)

Material selection is the prime point concerning in preparation of carbon membrane. There are wide varieties of precursor polymers designed for preparation of carbon membrane (4). Selection of polymer is the essential aspect as pyrolysis of unique polymer provides carbon membrane with completely different properties. The precursor polymer should meet minimum criteria such as for example it should not really soften nor liquefies during pyrolysis. It should be able to withstand high temperature (5).

Polyamidimides and polyetherimides are being recently studied and are found to be presenting satisfactory results because of its high melting point and thermal stability (6).
Fuertes and Centeno utilized polyetherimide to prepare backed carbon membrane for gas separation (7). They carried out gas permeability research for individual gasses aswell as for various mixtures of gasses. In addition they used phenolic resins because of their studies (8).

Different polymers are often blended to effectively incorporate the desirable homes of the blending polymers. Gas separation houses of carbon membranes are enhanced while combining different materials. New studies ‘re going on investigating the blending techniques for an optimized result (9).

Pore size control is probably the most challenging elements in carbon membrane preparation. Nitrogen and methane is definitely having a kinetic diameter of 3.6°A and 3.8°A respectively (10). So as a way to separate them by molecular sieving incredibly narrow pore distribution needs to be obtained. To get incredibly certain pore size, pyrolysis heat range was changed accordingly.

Two types of polymers were chosen to be able to understand the effect of individual polymer on membrane homes. Membrane parameters such as for example polymer concentration, pyrolysis heat were varied to comprehend the morphological and also chemical changes occurring in the membrane. Comparison of carbon membrane with polymer membrane was carried out, which showed interesting benefits which can be further used to study gas permeation real estate of the membranes. Results revealed these membranes can be utilised for the separation procedure for nitrogen from methane.

EXPERIMENTAL

Material

Polyamideimide (PAI) polymer and Polyetherimide (PEI) polymer which happen to be required for the planning of polymer membrane were acquired from UTM, Malaysia. N-methyl 2-pyrrolidone (NMP) was the solvent applied and it had been purchased from Merck Lifestyle Science Private Limited, Mumbai, India. Methanol utilized for washing was bought from Titan Biotech Small, Rajasthan, India. Acetone was purchased from Merck Specialities Individual Limited, Mumbai, India. All reagents had been used without the further purification.

Polymer Membrane Preparation

Polymers that were chosen for preparation were polyamideimide and polyetherimide. The solvent utilized was N-Methyl-2- pyrolidone. The polymer concentration in NMP was varied from 2- 20 wt.% as demonstrated in the Table 1. Unique batches of polymer choice were made by dissolving the corresponding quantity of polymer in 25ml NMP. Polyamideimide-polyetherimide ratio in the solution was varied as 25/75%, 50/50%, 75/25%, 0/100% and prepared different batches accordingly. For complete dissolution, the solution was held for magnetic stirring for 3 hrs. The temperatures was raised up to 80oC once in a while for 10 minutes, to avoid undissolved particles in the answer. Later the answer was sonicated in a sonication bath. The answer was therefore casted on a glass plate by using a casting rod. The casting rode that was applied has a dimension of 450I?m. The glass plate was maintained in the atmosphere for just two days for evaporation of the solvent. Later it had been kept inside a vacuum oven at 60oC for complete removal of NMP.

Table 1: Polymer Batches

Sample Code

Total Polymer (%)

PAI/PEI wt percentage (%)

PM-01

2

25/75

PM-02

9

25/75

PM-03

12

25/75

PM-04

15

25/75

PM-05

18

25/75

PM-06

20

25/75

Carbon Membrane Preparation

Polymer membrane was lower into a rectangular piece and transferred into an alumina crucible. It was then kept in the tubular furnace by VBCC for pyrolysis. It had been a horizontal furnace with alumina tube. Nitrogen environment was chosen for pyrolysis. The flow rate of nitrogen was maintained at 25ml/min. Polymer membranes with PAI/PEI composition of 25/75% was only further more used to make carbon membrane because they showed good structural steadiness in comparison to other batches.

For pyrolysis distinct protocols were followed. The protocols are as proven below,

1) 50 to 250 oC at a ramp level of 13.3 Co/min.
(2) 250 oC to (Tmax-15) oC at a ramp level of 3.85 Co/min.
(3) (Tmax-15) oC to Tmax oC at a ramp rate of 0.25 Co/min.
(4) Soak at Tmax for 2 h. (11)

After pyrolysis, it had been kept for organic cooling before taking out. The different batches of carbon membranes based on different pyrolysis protocol were prepared as granted in the Table 2. Polymer membrane with 9% polymer concentration was the membrane employed for studying different pyrolysis protocols.

Table 2: Carbon Membrane Batches

Sample Code

Total Polymer (%)

Pyrolysis Temperature(oC)

CM-01

2

600

CM-600

9

600

CM-450

9

450

CM-800

9

800

CM-03

12

600

CM-04

15

600

CM-05

18

600

CM-06

20

600

Characterization of Synthesized Membranes

Various techniques were useful for the characterization of polymer along with their derivative carbon membranes. Differential Scanning Calorimetry (DSC) was used to discover glass transition heat range of polymer membranes and also to study the blending of polymers. Under nitrogen ambiance, scans from 50 to 450oC at the heating rate of 10oC/min were performed on a DSC Perkin Elmer version 6000.

Thermogravimetric examination (TGA) was used to review the thermal degradation of the polymer membranes. Degradation heat of the membrane, plus the weight loss through the process, is analyzed. It had been carried out on a TGA Perkin Elmer 4000 version, in nitrogen atmosphere at a flow charge of 30 mL min-1. The temperatures range was from 50 up to 750 oC.

X-ray Diffractometer (XRD) was used to study the structural changes in membrane due to variation in pyrolysis heat range. Perkin Elmer 1621 wide-angle X-ray diffractometer was the instrument used to study the microstructural adjustments in membrane. Using Bragg’s law the average d-spacing of the membrane was evaluated. It is as displayed below,

nI� = 2d sin I?, where n is an intrinsic number, I� may be the X-ray wavelength, d is for the inter-level spacing between the polymer chains and I? is the diffraction angle.

CHN analysis was conducted to review the variation in the elemental composition with pyrolysis temperature. Elementar Vario EL was the equipment used here for examination. Compostion of oxygen was observed using separate apparatus.

Scanning Electron Microscopy (SEM) was used to receive pore size of the membrane together with get a

closer how to start an analysis essay graphic of the membrane. JEOL Style JSM – 6390LV may be the model used for the analysis.

RESULTS AND DISCUSSION

Physical properties

Both PAI and PEI met the requirements for preparing carbon membrane with promising outcomes. While contents of PAI in membrane manufactured the membrane considerably more brittle, which is due to its aromatic rings, (10) PEI gave structural support to the membrane. So PAI/PEI content was fixed at 25/75% for all your batches down the road.

As two polymers will be employed, the miscibility of the precursors needs to be tested and glass changeover temperatures of the membrane was taken as the criteria for the evaluation. For the polymer blends, Tg was discovered to be in between of that of specific polymers. Tg of PEI and PAI are 217°C and 280°C respectively. And from the Table 3 it is clear that both polymers are totally miscible and was correctly blended together.

Table 3: Glass Changeover Temperature

Sample Code

PAI/PEI wt Percentage (%)

Glass Transition Temperatures (oC)

PM-25

25/75

233

PM-50

50/50

249

PM-75

75/25

265

PM-100

0/100

219

Effect of polymer concentration on thermal characteristics

Unlike polymer membrane, carbon membrane was thermally and chemically steady. Thermal stability can be analyzed by TGA. TGA analysis of most polymer membranes is displayed in Shape 1. It demonstrates concentration does not have much effect on degradation heat of membranes. Nonetheless it gives an insight into find the pyrolysis protocol that needs to be followed. There will vary pyrolysis protocols for preparation of carbon membranes, predicated on kind of precursors used, one process is fixed.

Figure 1: Thermal evaluation of Polymer Membranes

Figure 1 illustrates the excess fat variation of polymer membranes during the heating process up to 800°C. In line with the TGA thermo-diagram, the degradation temperatures (Td) is definitely 550°C and was thought as the temperatures corresponding to 15% weight loss. This indicates the high thermal level of resistance of the membrane. The total weight loss at 800°C, with 10°/min heating fee, was roughly 60%. The enhanced thermal steadiness of the membrane highlights its quality as a precursor for the planning of carbon molecular sieve membranes.

Effect of polymer concentration on structure of membrane

Figure 2: XRD of Carbon Membrane of diverse concentrations

Effect of polymer focus on structure of carbon membrane is shown in Body 2. As the focus of polymer was elevated from 2% to 20%, peak intensification occurred, resulting in a more compact framework. Pore size was decreased and membrane with higher packing density is created.

Effect of pyrolysis heat range on microstructure of membrane

Structural examination on carbon membranes was performed by obtaining XRD spectra as a function of pyrolysis temperature. As shown in Shape 3, the XRD spectrum for membrane well prepared at 450oC is a merger of two peaks at 22.7o and 18.8o. With upsurge in pyrolysis heat range, the peaks joined right into a single but intensified peak with a shift toward small pore sizes; indicating a decrement in average d-spacing.

Figure 3: XRD of Carbon Membrane prepared at different temperatures

d-spacing in carbon membrane refers to interlayer distances, with increase in temperature smaller sized structures are formed. 800 °C was determined to be the optimum pyrolysis heat range as membrane having high density and packing effectiveness are formed at this temperature. (1)

Effect of pyrolysis heat range on membrane composition

In order to study how pyrolysis heat range changed the chemical substance composition of the membrane, elemental evaluation has been carried out for both polymers along with carbon membrane. In Shape 4, the idea zero in x-axis corresponds to precursor membrane and it gets the lowest carbon content and they started to increase with upsurge in pyrolysis temperature. However different elemental contents like oxygen, nitrogen and hydrogen was decreased with upsurge in temperature.

Presence of oxygen substances in the carbon membrane area could make the membrane extra hydrophilic and can trigger swelling of membranes (11). For the better functionality of carbon membrane oxygen content has to be less than 4% (12).When pyrolysis temperature in increased, oxygen content is reduced. Membrane well prepared at 800oC possesses oxygen content less than 4%.

So the result of pyrolysis temperature on hydrophilictiy of the carbon membrane was analyzed to study the affect of oxygen in the membrane. From the Table 4 it is clear that as pyrolysis temperature is increased, amount of drinking water absorbed is decreased, so increasing the hydrophobic nature of carbon membranes. This can be explained by the decrease in oxygen containing group in membrane with pyrolysis heat.

Figure 4: Elemental analysis of membranes

Table 4: Hydrophilicity of carbon membranes

Sample-Code

Pyrolysis Temperature (°C)

Wet weight of the membrane (g)

Dry weight of the membrane (g)

Amount of water absorbed (g)

CM-450

450

0.0588

0.0553

0.0035

CM-600

600

0.0523

0.0503

0.0020

CM-800

800

0.0687

0.0607

0.0008

Morphology of Membranes

The surface area and cross-section morphologies of carbon membranes along with polymer membranes had been investigated by SEM (Scanning Electron Microscopy) techniques.

Surface image of polymer membrane can be shown in Physique 6. It reveals a smooth and defect free of charge surface without any deformation. Cross section of the polymer membrane can be shown below. In comparison to carbon membrane it generally does not have uniform pore distribution. All the pores are elongated skin pores and the membrane created is very dense. Thickness of polymer membrane was observed to come to be 250I?m.

The honey-comb structure of carbon membrane displays the pore structure in the membrane (Physique 5). It really is clear from the impression that the membrane is definitely rich in pores and has a significant uniform pore distribution. The membrane was having a sponge-like matrix unlike polymer membrane. This uniform pore distribution enables carbon membrane to possess large selectivity over polymer membrane.

  1. (b)

Untitled.pngUntitled.png

Figure 5: SEM pictures: (a) Top surface and (b) Cross section of Carbon Membrane

  1. (b)

1.jpg4.jpg

Figure 6: SEM photos: (a) Top surface and (b) Cross section of PolymerMembrane

CONCLUSION

Different polymer blends had been tried for the preparation of polymer membrane and membranes produced from Polyamideimde/Polyetherimide (25/75wt.%) exhibited more attractive performance than the other blends. Polymer concentration was varied from 2-20% and at 9% it had been found to come to be exhibiting best outcomes. Polymer membranes ready from PAI/PEI were transparent hydrophilic membranes. Polymer membranes had been thermally unstable in comparison to carbon membrane and had been found to possess degradation temperature around 450oC. Complete miscibility of both polymers was verified and the cup transition temp of the polymer membrane was also found.

For the planning of carbon membrane numerous protocols were used for pyrolysis, and 800oC was identified to be the ideal temperatures for pyrolysis. Thermal analysis of membrane had carried out, which proved the higher thermal balance of the carbon membrane. Morphological studies implies that carbon membrane well prepared at 800oC have desired pore size in comparison to other membranes prepared at lower temps. XRD research of the carbon membrane revealed that as heat increases, smaller sized membranes are received, which reduces the permeability of the membrane. All of the membranes have demonstrated promising results which can be further more investigated for gas separation research.

References

1. Carbon membranes from blends of PBI and polyimides for N2/CH4 and CO2/CH4. Seyed Saeid Hosseini, Tai Shung Chung. s.l. : Journal of Membrane Research, 2009, Vol. 328. 174-185.

2. A assessment on the latest production of carbon membranes for gas separation. A.F. Ismail, L.I actually.B. David. s.l. : J. Membr. Sci., 2001, Vol. 193. 1.

3. Fabrication of carbon membranes for gas separation–a analysis. S.M. Saufi, A.F. Ismail. s.l. : Carbon, 2004, Vol. 42. 241-259.

4. Gas permeation through micropores of carbon molecular sieve membranes derived from kapton polyimide. Suda H, Haraya K. s.l. : Chem B, 1997, Vol. 101. 3988-94.

5. DH, Morthon-Jones. Polymer processing. London : Chapman and Hal, 1984. Chapter 2.

6. Relationship between chemical structure of aromatic polyimides and gas permeation homes of their carbon molecular sieve membranes. H.B. Recreation area, Y.K. Kim, J.M. Lee, S.Y. Lee, Y.M. Lee. s.l. : J. Membr. Sci., 2004, Vol. 229. 117.

7. Carbon molecular sieve membranes from polyetherimide. Fuertes Stomach, Centeno TA. s.l. : Microporous Mesoporous Mater, 1998, Vol. 26. 23-6.

8. Supported carbon molecular sieve membranes based on phenolic resin. Centeno TA, Fuertes AB. s.l. : J Membr Sci, 1999, Vol. 160. 201-211.

9. Gas separation homes of carbon molecular sieve membranes derived from polyimide/polyvinylpyrrolidone blends: aftereffect of the molecular pounds of polyvinylpyrrolidone. Y.K. Kim, H.B. Recreation area, Y.M. Lee. s.l. : of the molecular excess fat of polyvinylpyrrolidone, 2005, Vol. 251. 159.

10. Ahmad Fauzi Ismail, Dipak Rana, Takeshi Matsuura ,Henry C. Foley. Carbon-based Membranes for Separation Processes. London : Springer, 2011.

11. Carbon molecular sieve membranes derived from Matrimid polyimide for nitrogen/methane separation. Xue Ning, William J. Koros. s.l. : Carbon, 2014, Vol. 66. 5 1 1 – 5 2 2.

12. Interaction, miscibility and phase. E. Földes, E. Fekete, F.E. Karasz, B. Pukánszky. s.l. : Polymer, 2000, Vol. 41. 975.

13. Gas permeation and micropore composition of carbon molecular sieving membranes modified by oxidation. Kusakabe K, Yamamoto M, Morooka S. s.l. : J Membr Sci , 1998, Vol. 149. 59-67.

14. Characterization of ultramicroporous carbon membranes with. Jones CW, Koros WJ. s.l. : Ind Eng Chem Res, 1995, Vol. 34. 158-163.

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