PET Recycling Process Flow Diagram

Project planning of a sustainable process
for PET waste recycling

Equipment design and dimensioning
Members of PSE (Group 1)
Aagam Atulkumar Shah Joydeep Bagchi Prachi Nilesh Shah
Esma Yeliz Aksungur Jyotimay Baishya Prakriti Gupta
Gayathri Venkatarathnam Nithya Simha Sunay Hesenov
Name, Vorname|
Dortmund Ort, Datum
, 01.12.2022
INTRODUCTION
Name, Vorname| Ort, Datum 2

Introduction
Recycling of
20kt/year
PET
Mechanical Chemical Thermal

Recycling Recycling Conversion
Aminolysis Ammonolysis Glycolysis Hydrolysis Methanolysis Chemolysis
Fewer
More waste
operational
streams
steps
Name, Vorname|
Bagchi, Joydeep |Ort, Datum 01.12.2022
Dortmund, 3
𝑃𝑜𝑙𝑦𝑒𝑡h𝑦𝑙𝑒𝑛𝑒 𝑡𝑒𝑟𝑒𝑝𝑡h𝑎𝑙𝑎𝑡𝑒 𝐸𝑡h𝑦𝑙𝑒𝑛𝑒 𝑔𝑦𝑙𝑐𝑜𝑙 𝐵𝑖𝑠(2 − h𝑦𝑑𝑟𝑜𝑥𝑦𝑒𝑡h𝑦𝑙) 𝑡𝑒𝑟𝑒𝑝h𝑡h𝑎𝑙𝑎𝑡𝑒
𝑃𝐸𝑇 𝐸𝐺 𝐵𝐻𝐸𝑇
𝑁𝑎2 𝐶𝑂 3
+¿
210 ° C , 2 ¯
¿
Name, Vorname|
Dortmund, 4
EQUIPMENT DESIGN

REACTION KINETICS
Name, Vorname|
Dortmund, 6
REACTION KINETICS
 Heterogenous solid-liquid reaction mixture at low temperature
 Homogenous liquid-liquid reaction mixture at high temperature(starting from 170˚C)
 BHET oligomers are obtained in the weight ratio of 1:10 with respect to BHET
monomer.
 Operating conditions: 2 bar ,
[1] López-Fonseca, R., Duque-Ingunza, I., de Rivas, B., Flores-Giraldo, L. and Gutiérrez-Ortiz, J.I., 2011. Kinetics of catalytic glycolysis of PET wastes with sodium carbonate.
[2] Chen et. Al 2012, Kinetics of glycolysis of poly(ethylene terephthalate) under microwave irradiation
Name, Vorname|
Dortmund, 7
REACTION SCHEME PET:EG 1:10
 (mole basis)
PET particle size range = 0.75 - 1 mm
PET:Na2CO3 200:1
(mole basis)
 Pseudo first order kinetics is followed due to excess of EG.
 r(PET) = k1’ (CPET) – k2’(CBHET) k1’(h-1) = k1 * CEG * CNa2CO3 k2 ’
(h-1) = k2 * CNa2CO3
= 4.33(CPET) – 1.13(CBHET) r(PET) in kmol/(m3-h)
C in kmol/m3
 Activation Energy of the reaction is found to be 158±10 kJ/mol
[1] López-Fonseca, R., Duque-Ingunza, I., de Rivas, B., Flores-Giraldo, L. and Gutiérrez-Ortiz, J.I., 2011. Kinetics of catalytic glycolysis of PET wastes with sodium carbonate.
Name, Vorname|
Dortmund, 8
REACTOR DESIGN
Name, Vorname|
Dortmund, 9
REACTOR DESIGN
 Reactor type: Cascade of Continuous Stirred Tank Reactors(n=4)
 Length to Diameter(L/D) ratio chosen for each reactor = 3.74

Length Diameter Total Volume(m3) Overall total Overall
(m) (m) Surface surface Volume(m3)
Area(m2) area(m2)
3.740 1.000 7.448 2.938 29.794 11.755
 Maximum filling in tank = 80% so,

Overall Reaction Reaction volume for
Volume(m3) each tank(m3)
9.403 2.350
[3] Levenspiel, O., 1998. Chemical reaction engineering. John wiley & sons.
Name, Vorname|
Dortmund, 10
REACTOR DESIGN
 Material of construction for tank : Carbon Steel
 Type of Impeller: Flat 6-blade disc turbine
 Impeller Diameter: 1/3rd of tank diameter i.e. 0.33 m

Height of Impeller: 2/3rd of tank height i.e. 2.50 m
 Number of baffles = 4
Width of each baffle = 1/12th of tank diameter i.e. 83 mm
[4] Woods DR. Rules of Thumb in Engineering Practice. Weinheim Chichester: Wiley-VCH; John Wiley distributor; 2007. doi:10.1002/9783527611119
[5] Perry, Robert H.; Green, Don W. (2008): Perry's chemical engineers' handbook. 8th ed McGraw-Hill.
[8] Chemical Reactor Material Selection: https://en.wikipedia.org/wiki/Chemical_reactor_materials_selection ; Last accessed 27.11.2022
Name, Vorname|
Dortmund, 11
REACTOR DESIGN
 The stirring rate of the impeller is found to be 600±10 rpm
 Impeller Reynold Number IRe = Dimp = Diameter of Impeller(m)
N = Speed of stirrer(rps)
= 1.47 *10^7 ρ = Density of reaction mixture(kg/m3)
 Power drawn by impeller P = μ = Viscosity of reaction mixture (Pa-s)
= 1631.476 kW Po = Power Number
 Shaft Power = 16 = 216.9487 kW
 Motor Power = 1.3 * Shaft Power = 282.033 kW
 Net contribution as heat dissipated by stirrer = 0.2 * 282.033 = 56.406 kW
[4] Woods DR. Rules of Thumb in Engineering Practice. Weinheim Chichester: Wiley-VCH; John Wiley distributor; 2007. doi:10.1002/9783527611119
[5] Perry, Robert H.; Green, Don W. (2008): Perry's chemical engineers' handbook. 8th ed McGraw-Hill.
Name, Vorname|
Dortmund, 12
Po = 2
 [5] Perry, Robert H.; Green, Don W. (2008): Perry's chemical engineers' handbook. 8th ed McGraw-Hill.
Name, Vorname|
Dortmund, 13
MASS BALANCE
 Assumptions of ideal CSTR are considered: Initial Final
steady state, uniform composition and Component
kmol/h kg/h kmol/h kg/h
temperature throughout the mixture,
concentration in tank is same as PET 13.02 2500 3.255 625
concentration at outlet EG 130.208 8072.92 120.443 7467.45
 Mass balance around the reactor Na2CO3 0.0651 6.9006 0.0651 6.9006
 Reaction Mixture Density
at 210˚C = 965 kg/m3 BHET 0 0 9.765 2254.972
BHET
Volumetric Flow Rate into (dimer) 0 0 0.443892 225.49
the reactor = 10.65 m3/h Total 143.293 10579.8 133.972 10579.8
Name, Vorname|
Dortmund, 14
ENERGY BALANCE
 Assumptions of ideal CSTR are considered:
steady state, uniform composition and temperature throughout the mixture,
temperature of mixture at inlet is equal to temperature of mixture at outlet
Uniform Temperature Reaction Term Jacket Stirrer

Steady state
 Enthalpy of Reaction is found to be 12kJ/mol of reacted amount of PET(ΔHR)

Reaction Term = 12*11.75*((4.33*0.3)-(1.13*0.89))*10/36 = 11.487 kW
 Energy of Jacket = Stirrer – Reaction = 44.919 kW

Name, Vorname|
Dortmund, 15
ENERGY BALANCE
 Quality of steam considered for the temperature difference of 10K : Saturated steam at
220˚C and 23 bar, λvap = 1858.2 kJ/(kg-K)
 Total amount of steam(S): = 44.919/1858.2 = 87.024 kg/h
 Amount of steam in each reactor = 87.024/4 = 21.756 kg/h
 Material of insulation: Glasswool(thermal conductivity = 0.035 W/m-K)
[6] S. Veiseh et. Al 2009, mathematical models for thermal conductivity density relationship in fibrous thermal insulations for practical applications
[7] Saturated steam property: https://www.engineeringtoolbox.com/saturated-steam-properties-d_457.html; Last accessed on 27.11.2022
Name, Vorname|
Dortmund, 16
CASCADE DESIGN
Shah,
Name,Prachi Nilesh
Vorname| | Dortmund,
Ort, Datum 01.12.2022 17
DESIGN OF STIRRED TANK CASCADE
Vapor pressure curve for EG
7
5
- Absolute vapor pressure (bar)
Pressure (bar)
4
A, B, C – Antoine constants
3
2 T – temperature (°C)
1
0
Operating Conditions for reactor:
80 100 120 140 160 180 200 220 240 260 280
T – 210 °C
Temprature (°C) P – 2 bar
[1] ‘Antoine equation’, https://en.wikipedia.org/wiki/Antoine_equation#:~:text=The%20Antoine%20equation%20is%20a,Antoine%20(1825%E2%80%9
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 18
X versus 𝜏 curve for single CSTR
0.9
0.8 𝑥 𝐴 𝑥 𝐴𝑒
0.7 𝑘1 𝜏=
0.6
𝑥 𝐴𝑒 − 𝑥 𝐴
Conversion [X] (-)
0.5
0.4
0.3
– Conversion
0.2 – Equilibrium Conversion
0.1
0 - Residence time (hr)
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5
Residence time [ 𝜏] (hr) - Rate constant (hr-1)
[2] López-Fonseca, R., Duque-Ingunza, I., de Rivas, B., Flores-Giraldo, L. and Gutiérrez-Ortiz, J.I., 2011. Kinetics of catalytic glycolysis of PET wastes with sodium
carbonate. Chemical engineering journal, 168(1), pp.312-320.
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 19
X versus 𝜏 curve for PFR
0.9
𝑥 𝐴𝑒
( )
0.8
0.7 𝑘1 𝜏=𝑥 𝐴𝑒 ln
0.6 𝑥 𝐴𝑒 − 𝑥 𝐴
Conversion [X] (-)
0.5
0.4
0.3 – Conversion
0.2
– Equilibrium Conversion
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
- Residence time (hr)
Residence time [ 𝜏] (hr) - Rate constant (hr-1)
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 20
X versus 𝜏 curve for cascade system
0.8
𝐶 𝑃𝐸𝑇 , 𝑖−1 − 𝐶 𝑃𝐸𝑇 ,𝑖
0.7
𝑥=
0.6 𝐶 𝑃𝐸𝑇 , 𝑖−1
Conversion [X] (-)
0.5
0.4
0.3
- Concentration of PET at outlet of ‘ith’
0.2 reactor (mol m-3)
0.1
0
- Concentration of PET at inlet of ‘ith’
0 0.2 0.4 0.6 0.8 1 1.2 1.4
Residence time [ 𝜏] (hr)
reactor (mol m-3)
– Conversion
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 21
Rate versus Concentration Curve
7000
6000
5000
𝐶 𝑃𝐸𝑇 ,𝑖 −1 𝐶 𝑃𝐸𝑇 ,𝑖
-r (mol m-3 hr-1)
4000
′
3000 −𝑟 = −
2000 𝜏 𝜏
1000
0
0 200 400 600 800 1000 1200 1400
-1000
No. of CSTR required in series – 4
-2000
Cpet (mol m-3)
Residence time of each CSTR – 0.21 hr
-r Vs. Cpet -1/𝜏1 -1/𝜏2 -1/𝜏3 -1/𝜏4
Approximate size of each CSTR - 2.35 m-3
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 22
FILTER DESIGN
FOR RECYCLING
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 23
Filtration Unit I
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 24
ROTARY VACUUM DRUM FILTER
Table 1 Hildebrand solubility parameter ‘δ’ of PET and EG
Substance δ [MPa1/2]
PET 20.5
EG 29.9- 33.0
PET is not soluble in EG at room temperature and only dissolves

at temperature well beyond 100 °C.
[1] ‘Hildebrand solubility parameter’, https://en.wikipedia.org/wiki/Hildebrand_solubility_parameter.
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 25
Unreacted PET
Small fraction of
Unreacted PET, EG Unreacted PET, EG
BHET, Dimers BHET, Dimers
FILTER
Inlet streams (kg/hr) Outlet streams (kg/hr)
Unreacted PET 624.96 Solids in cake 1990.614
Dimers 225.49 Solids in filtrate 54.629
BHET 2254.97 BHET 2254.97
EG 7467.45 EG 6272.66
Na2CO3 Na2CO3 6.9006
6.9006
Total 10579.77
Total 10579.77
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 26
A-
Equation 1 Filtration area calculation

rw - wash flow rate (m3 m-2 s-1)
Equation 3 wash flow rate tw - wash time tw (s)
Solid content - 5-6 wt %

Equation 2 Constant pressure filtration
formula Required area - 4.7 m2
Equation 4 wash time
Cake discharge method – Scraper Discharge
Filter Cloth – Polypropylene or Polyester
Wash Liquid – Water
[1]Sinnott, R.K., 2005. Coulson & Richardson’s chemical engineering, vol. 6. Chemical engineering design, 4.
[2]McCabe, W.L., Smith, J.C. and Harriott, P., 1993. Unit operations of chemical engineering (Vol. 5, p. 154). New York: McGraw-hill.
[3]‘ROTARY VACUUM DRUM FILTER BASICS’, https://www.micronicsinc.com/filtration-news/rotary-vacuum-drum-filter-basics/.
[4]‘Filter Media Chemical Resistance Chart’, https://www.standardfilter.com/products/filter-media-chemical-resistance-chart/.
[5]Couper, J.R., Penney, W.R., Fair, J.R. and Walas, S.M., 2005. Chemical process equipment: selection and design. Gulf professional publishing.
Shah,
Name,Prachi Nilesh
Ort, Datum 01.12.2022 27
CRYSTALLIZATION – I
PRINCIPLE OF WORKING
Venkatarathnam,
Name, Vorname| Ort,Gayathri
Datum | Dortmund, 01.12.22 28
CRYSTALLIZATION - I Melt crystallization
Purity high (Not at high viscosity)
BHET,
monomers
𝐶 𝑒𝑞 <0.01 gg−1
and
Unreacted Dimers
PET Precipitation
EG, Na2CO3
catalyst
Evaporative
crystallization
BHET crystals Mother liquor
+ +
EG loss Product loss
Cooling
1. Kramer, Herman J.M; Bermingham, Sean K.; van Rosmalen, Gerda M. crystallization
(1999): Design of industrial crystallisers for a given product quality. In Journal
of Crystal Growth. DOI: 10.1016/S0022-0248(98)01179-8 Heuristics for method selection [1]
Venkatarathnam,
CRYSTALLIZATION - I
Solubility curve of BHET in EG Slope of generated
3.5 Feed stream weight ratio and temperature
Crystallization temperature range solubility curve 0.012 oC-1
Weight ratio of BHET to EG [ gg-1]
3.0 i.e.,> 0.005 oC-1 [1]

2.5
2.0
1.5
1.0
Yuan et
al
0.5
0.0
0 20 40 60 80 100 120
Temperature [ oC]
1. Kramer, Herman J.M; Bermingham, Sean K.; van Rosmalen, Gerda M. (1999): Design of industrial crystallisers for
a given product quality. In Journal of Crystal Growth. DOI: 10.1016/S0022-0248(98)01179-8
Venkatarathnam,
CRYSTALLIZATION - I
12.00
Solubility curve of BHET in EG
Weight ratio of BHET to EG [gg-
10.00
8.00
x = Mole fraction of BHET
γ = Activity coefficient of BHET
1]
6.00
∆HSL = Melting enthalpy of BHET in EG (kJ.mol-1)

4.00
R = Universal Gas constant = 8.314 (J.mol-1K-1 )
2.00 Tm = Melting point of BHET (K)
Yuan et al
T = Corresponding temperature of mole fraction (K)
0.00
0 10 20 30 40 50 60 70 80 90
Temperature [oC]
1. Mullin, J.W., 2001. Crystallization. Fourth edition. Butterworth-Heinemann, A division of Reed
Educational and Professional Publishing Ltd.
2. Yao, Haoyu; Yan, Dongxia; Lu, Xingmei; Zhou, Qing; Bao, Yinan; Xu, Junli (2022): Solubility Melting point of BHET = 108.61 oC [2]
determination and thermodynamic modeling of bis-2-hydroxyethyl terephthalate (BHET) in different
solvents. In Chinese Journal of Chemical Engineering 45. DOI: 10.1016/j.cjche.2021.03.024.
Venkatarathnam,
CRYSTALLIZATION - I
Plot of mole fraction of BHET against temperature
1.0
Melting point of BHET (108.61 oC)
Mole fraction of BHET [-]
0.8
0.6
Melting point of BHET = 108.61 oC [1]
0.4
0.2
Yuan et al
0.0
0 10 20 30 40 50 60 70 80 90 100 110 120
Temperature [oC]
1. Yao, Haoyu; Yan, Dongxia; Lu, Xingmei; Zhou, Qing; Bao, Yinan; Xu, Junli (2022): Solubility determination and thermodynamic modeling of bis-2-hydroxyethyl terephthalate
(BHET) in different solvents. In Chinese Journal of Chemical Engineering 45. DOI: 10.1016/j.cjche.2021.03.024.
Venkatarathnam,
CRYSTALLIZATION - I
[1] Scribbr. www.steemit.com/steemstem/@josalarcon2/crystallizers-which-ones-to-use. Accessed 29 November 2022.
Venkatarathnam,
CRYSTALLIZATION - I
Assumptions: Heat required for cooling and
Yield of crystals [1]
 Final mother liquor in saturation crystallization
with the deposited crystals.
𝑌 =𝑊 ( 𝐶1 − 𝐶 2 )  Actual yield > Theoretical yield 𝑄= ( 𝑚 𝑓 𝐶 𝑝 ∆ 𝑇 ) +𝑌 𝐻 𝑆𝐿
due to the retention of the
mother liquor with BHET crystals.
Y = Yield of crystallizer (kg.hr-1)
mf = Feed mass flowrate to the crystallizer(kg.hr-1 )
W = Initial mass of solvent (kg.hr-1)
Cp = specific heat capacity of feed stream (kJ.kg -1K-1)
C1 = Initial solution concentration (kg anhydrous salt.kg solvent -1)
∆T = Cooling and crystallization temperature range (K)
C2 = Final solution concentration (kg anhydrous salt.kg solvent ) -1
Y = Yield of crystallizer (kg.hr-1 )

HSL = Melting enthalpy of BHET of EG (kJ.mol-1)
2248.86 kg.hr-1 (40% Loss of EG)
1. Mullin, J.W., 2001. Crystallization. Fourth edition. Butterworth-Heinemann, A

704784.73 kJ.hr-1
division of Reed Educational and Professional Publishing Ltd.
Venkatarathnam,
CRYSTALLIZATION – II
CRYSTALLIZER DESIGN
Aksungur,
Name, Esma Yeliz
Vorname| | Dortmund, 01.12.22
Ort, Datum 35
CYSTALLIZATION - II
Mixed suspension, mixed product
Forced circulation crystallizer
removal (MSMPR) crystallizer [1]
 steady-state operation
 perfect mixing within the crystallizer
 no crystal in the feed
 no crystal breakage into finite particles
 uniform supersaturation exists all time
[1] Myerson, Allan S. (Ed.) (2002): Handbook of industrial crystallization. 2nd ed. Boston, Oxford: Butterworth-Heinemann.
[2] McCabe, W.L., Smith, J.C. and Harriott, P., 1993. Unit operations of chemical engineering New York: McGraw-hill.
Aksungur,
Name, Esma Yeliz
Ort, Datum 36
CYSTALLIZATION - II
𝑫 𝒎𝒆𝒂𝒏
 Residence time 𝝉= Growth rate
𝟒𝑮
𝒅𝑳
 ∆L Law for MSMPR 𝑮=
𝒅𝒕
grow in uniform supersaturation field
have the same growth rate
[1] Lewis, Alison; Seckler, Marcelo; Kramer, Herman J. M.; van Rosmalen, Gerda (2015): Industrial crystallization.
Fundamentals and applications. Cambridge, United Kingdom: Cambridge University Press.
[2] McCabe, W.L., Smith, J.C. and Harriott, P., 1993. Unit operations of chemical engineering New York: McGraw-hill .
Aksungur,
Name, Esma Yeliz
Ort, Datum 37
CYSTALLIZATION - II
110
𝒅𝑳
y = 0.3542x + 49.083 𝑮=
100 𝒅𝒕
D50(µm)
90
G= 5.9E-09 m.s-1
Experimental D...[1]
80
80 100 120 140 160
Crystallization time (min)

[1] Yuan, Peiquan; Liu, Baoshu; Sun, Hua (2021): Optimization of the Crystallization Process of Bis(2 ‐hydroxyethyl) Terephthalate. In
Crystal Research and Technology 56 (11)
[2] McCabe, W.L., Smith, J.C. and Harriott, P., 1993. Unit operations of chemical engineering New York: McGraw-hill.
Aksungur,
Name, Esma Yeliz
Ort, Datum 38
CYSTALLIZATION - II 110
Growth rate (m.hr-1) 3.542E-07

Mean diameter of the crystal (m) 0.000095 100
𝑫 𝒎𝒆𝒂𝒏
D50(µm)
Residence time (hr) 1.1175
𝝉=
Crystal production rate (kg.hr-1) 2248.8600 𝟒𝑮
90
Experimental ...
Weight ratio (BHET/EG) 0.8963 80
80 100 120 140 160
Density of slurry (kg.m-3) 1255.5581
Crystallization time (min)
𝑝𝑟𝑜𝑑𝑢𝑐𝑡𝑖𝑜𝑛𝑟𝑎𝑡𝑒×𝑟𝑒𝑠𝑖𝑑𝑒𝑛𝑐𝑒𝑡𝑖𝑚𝑒
𝑉 𝑐𝑟𝑦𝑠= 2 m3
𝑠𝑙𝑢𝑟𝑟𝑦 𝑑𝑒𝑛𝑠𝑖𝑡𝑦
[1] Bennett, Richard C. (2002): Crystallizer selection and design. In Allan S. Myerson (Ed.): Handbook of industrial Volume of the crystallizer
crystallization. 2nd ed. Boston, Oxford: Butterworth-Heinemann, pp. 115–140.
Aksungur,
Name, Esma Yeliz
Ort, Datum 39
CYSTALLIZATION - II
θ 30 (m) 1.2084
/ 1.2 : 1[2] (m) 1.0070
(m 0.027 m (m) 0.0270
(m) 0.2829
(m3) 0.0772
(m3) 1.9238
Total Volume (m3) 2.0010
= Angle D = Diameter
[1] Couper, James R. (2012): Chemical process equipment. Selection and design. 3rd ed. Waltham, Mass.: Butterworth- H = Height V = Volume
Heinemann.
[2] Woods DR. Rules of Thumb in Engineering Practice. Weinheim Chichester: Wiley-VCH; John Wiley distributor; 2007.
Aksungur,
Name, Esma Yeliz
Ort, Datum 40
CYSTALLIZATION - II
prevents undesired nucleation

 Seeding
influences crystal size distribution
the general crystal weight ratio of 0.1-1 % in EG[1]

 Proposed
with the usual size of nucleate crystals 0.1 to 10 m[2]
[1] Beckmann, Wolfgang (2013): Crystallization. Basic concepts and industrial applications. Weinheim: Wiley-VCH.
[2] Woods DR. Rules of Thumb in Engineering Practice. Weinheim Chichester: Wiley-VCH; John Wiley distributor; 2007.
Aksungur,
Name, Esma Yeliz
Ort, Datum 41
CYSTALLIZATION - II
 Continuous injection of 5 – 40 % of slurry into the crystallizer [1]
[1] Perry, Robert H.; Green, Don W. (2008): Perry's chemical engineers' handbook. 8th ed. New York: McGraw-Hill Professional.
[2] Scribbr. www.steemit.com/steemstem/@josalarcon2/crystallizers-which-ones-to-use. Accessed 29 November 2022.
Aksungur,
Name, Esma Yeliz
Ort, Datum 42
CYSTALLIZATION - II
 Material selection
EG is not aggressive to most materials Carbon steel

BHET is non-corrosive
BHET dimer
Design of support
[1] Ullmann, Fritz (Ed.) (2005-): Ullmann's encyclopedia of industrial chemistry. 7th ed. [Hoboken, N.J.]: John Wiley & Sons.
[2] Perry, Robert H.; Green, Don W. (2008): Perry's chemical engineers' handbook. 8th ed. New York: McGraw-Hill Professional.
Aksungur,
Name, Esma Yeliz
Ort, Datum 43
FILTER DESIGN
FOR PRODUCT RECOVERY
Baishya,
Name, Jyotimay|
Vorname| Ort,Dortmund,
Datum 01.12.2022 44
Filtration Unit II
Baishya,
Name, Jyotimay|
Datum 01.12.2022 45
SEPARATION OF BHET CRYSTALS
• The product from Crystallizer needs to be separated
• Crystal size – 0.000095 m [1]
• Pressure driven mechanism in batch operation
*Plate and Frame Press Filter chosen for Filtration
[1] Yuan, P., Liu, B. and Sun, H., 2021. Optimization of the Crystallization Process of Bis (2‐hydroxyethyl) Terephthalate.
Crystal Research and Technology, 56(11), p.2100025.
Baishya,
Name, Jyotimay|
Datum 01.12.2022 46
PLATE AND FRAME PRESS FILTER
• Batch operated filtration system
• Square plates and frames arranged in alternate order
• Cakes deposited in frames
[1]
[1] Holdich, R.G., Rushton, A. and Ward, A.S., 2008. Solid-liquid filtration and separation technology. John Wiley & Sons.
Baishya,
Name, Jyotimay|
Datum 03.11.22
01.12.2022 47
DESIGN OF FILTER *Mass fraction of
unreacted PET and
• Design is based on only BHET and EG as basis dimers = 0.0057
Filtration equation for constant pressure

[1]
1. = time of filtration (sec) 10. = solid fraction in feed
2. = specific resistivity of cake () 11. = moisture of cake
3. = viscosity of fluid ()
4. = concentration of solids in feed ()
5. = area ()
ρs 6. = pressure drop ()
𝑐= [1]
( 1− 𝑚𝑠 ) 7. = filter medium resistance ()
Baishya,
Name, Jyotimay|
Vorname|
Baishya, Dortmund,
Ort,Dortmund,
Jyotimay| 03.11.22
Datum 01.12.2022 48
ASSUMPTIONS OF CONSTANTS
Specific resistivity of cake () 4.42E10 [1] *all the assumptions are made for a
Solid fraction in feed (s) 0.47 pressure of 10 bar and 25°C
Moisture of cake (m) 1.25 [2]
Solid concentration in feed (c) 2248.8600
Pressure Drop () 10E5
Resistance of filter medium () 10E11 [3]
[1] Cornehl, B., Weinkötz, D. and Nirschl, H., 2013. Downscaling cake filtration—correlations between compressibility of lysozyme crystal filter cakes and filter area. Engineering in Life
Sciences, 13(3), pp.271-277.
[2] Zerin, I. and Datta, E., 2018. A Review Article on Applications of Filter Cloth. Int. J. Cloth. Sci, 5, pp.1-6.
[3] Mamghaderi, H., Gharabaghi, M. and Noaparast, M., 2018. Optimization of role of physical parameters in the filtration processing with focus on the fluid flow from pore. Minerals
Engineering, 122, pp.220-226.
Baishya,
Name,
Baishya,Jyotimay|
Jyotimay| Datum
Dortmund,03.11.22
01.12.2022 49
CALCULATION OF VISCOSITY
Viscosity versus temp curve
60 [1]
50 48
Viscosity ((𝑁 𝑠𝑒𝑐)/𝑚^2 )
40
30 Viscosity of Ethylene glycol at 25°C

20 15.5 15 (𝑁 𝑠𝑒𝑐)/𝑚^2
10 7
3.8 2.4 1.8 1.2
0
0 20 40 60 80 100 120 140 160
Temperature (°C)
[1] Engineering ToolBox, (2003). Ethylene Glycol Heat-Transfer Fluid Properties.
Baishya,
Name, Jyotimay|
Datum 01.12.2022 50
CALCULATION OF AREA AND PLATE AND FRAME SIZE
 Using the equations and considering a filtration time of 1 hour
Mass flow of filtrate (kg/hr) 2245.141
Volume flow of filtrate (/hr) 3.36
Area of filter () 36.12
Number of plates 18
Size of each square plates and frames (m) 1.001
EG in cake (kg/hr) 627.265
BHET in cake (kg/hr) 2203.883
Total mass of cake ( 2831.148
Average density of cake () 1193.001
Baishya,
Name, Jyotimay|
Datum 01.12.2022 51
FRAME THICKNESS
 Cake volume in filter per hour = 2.373
 For 15 frames with equal sides 1.001 m

frame thickness will be 0.1578 m
1.001 × 1.001 × 0.008
1.001 × 1.001 × 0.1578
Baishya,
Name, Jyotimay|
Datum 01.12.2022 52
WASHING OF CAKE
The obtained rate of wash is
0.21 209.37 kg
 Volume of wash liquid is[1]assumed to be 0.15 times volume of filtrate
The time of washing is

[1]
2.4 hours
0.5 hours
𝑡 𝑐𝑦𝑐𝑙𝑒 =𝑡 𝑓𝑖𝑙𝑡𝑟𝑎𝑡𝑖𝑜𝑛+𝑡 𝑤𝑎𝑠h𝑖𝑛𝑔 +𝑡 𝑑𝑜𝑤𝑛𝑡𝑖𝑚𝑒 3.9 hours/cycle

[1]
Baishya,
Name, Jyotimay|
Datum 01.12.2022 53
PRODUCT SPECIFICATION FROM FILTER AFTER WASHING
 Considering an washing efficiency of 95% [1]
Water (502.48 kg)
EG – 31.36 kg
Feed
Filter II BHET – 2703.88 kg
Water - 488.18
Water – 14.3 kg
EG – 595.901 kg
[1] Zerin, I. and Datta, E., 2018. A Review Article on Applications of Filter Cloth. Int. J. Cloth. Sci, 5, pp.1-6.
Baishya,
Name, Jyotimay|
Datum 01.12.2022 54
ROTARY DRYER

DESIGN OF
UTILITIES AND SUBSIDIARIES

HEAT EXCHANGERS
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 57
Heat exchangers
Heater Heat Exchanger

 Used for liquids and gases  Easy handling of high viscous or solid
 Applied for heating up to 900 °C systems
 Slower heating time  High flowrates
 Higher energy bills  Efficiency up to 90%
Sunay,Vorname|
Hasanov|Ort,
Dortmund, https://heat-exchanger-world.com/electric-heaters-compared-to-heat-exchangers-competitors-
Name, Datum 01.12.22 58
or-supplements
Heat Exchangers
Characteristics Plate and Frame Shell and Tube Scraped Surface
Cost per square foot Low Low High
Maintenance cost Medium Low High
Use with particulates Poor Good/Excellent Excellent
Amount of regeneration High Medium None
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 https://www.csidesigns.com/blog/articles/heat-exchanger-how-to-select-the-right-one 59
Shell and Tube Heat Exchanger
Large surface to Simple mechanical Well-established Can easily be cleaned.

volume ratio. layout (promising for fabrication methods
pressure operations). and design techniques
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 60
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 61
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 62
Utilities
Heating Agent for HE-1 and HE-2:
Cooling Agent for HE-3, HE-4 and HE-5:
DOWNTHERM Q
Cooling Water
- mixture of diphenylethane and alkylated aromatics
- superior alternative to hot oils - cheaper
- higher thermal stability and film coefficient

- higher heat capacity
- non-corrosive to lots of common metal alloys
- economical in long term - safer
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 SUBASGAR. (2018). Thermal Design of a Shell and Tube Heat Exchanger. January, 536–550. 63
Shell and tube sizing
 Location of fluid Process mixture in tube, heating/cooling agent in shell
 Flow Type Counter Current
 Number of passes 1 shell, 4 passes
 Tube pattern Equilateral triangle
 Shell type Split ring floating head
 Material Type 304 stainless steel
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 64
Final Data
Parameters HE-1 HE-2 HE-3 HE-4 HE-5
Area (m2) 16.25 28.08 9.42 8.42 13.7
Duty (kW) 648.8 642.6 563.5 426.6 195.8
Overall U (W/m2*K) 434.5 557.4 534.1 547.8 320.5
Velocity in Tube (m/s) 1.55 1.3 1.38 1.6 1.05
Velocity in Shell (m/s) 0.8 0.9 0.7 0.5 0.2
Pressure Drop in Tube 2.46 0.9 0.4 0.7 0.5

(bar)
Pressure Drop in Shell 0.15 0.36 0.13 0.06 0.007

(bar)
Sunay,Vorname|
Name, Hasanov|Ort,
Dortmund,
Datum 01.12.22 65
HOPPER AND STORAGE
TANK DESIGN
Shah
Name,Aagam |Dortmund,
Vorname| 01.12.2022
Ort, Datum 66
Shah
Vorname| 01.12.2022
Ort, Datum 67
CONICAL HOPPER
 Industrial application
 Easy handling – flat-based tanks
 Complete drainage and discharge control
 Angle of 30° optimum value
 200:1 PET to catalyst ratio taken Fig 1. Schematic diagram of conical hopper
 Drawback: Not easy to drain only solid particle
Image: https://toledometalspinning.com/home-v3/products/product-catalog/seamless-hopper-cone-funnels
Shah
Vorname| 01.12.2022
Ort, Datum 68
EG STORAGE TANK
 Ethylene glycol storage tank depending on the recycling stream
 Non-corrosive and stable
 HDPE is the better option
 Stainless steel or carbon steel can be used but expensive
 EG required is 2888.825kg/hr
Shah
Vorname| 01.12.2022
Ort, Datum 69
DESIGN
 Fresh EG is pumped into the hopper
 Outside diameter of the hopper can be fixed by considering 8 to 10 times of particle size
 Safety volume chosen
 Optimum height-to-diameter ratio for the storage tank is 1.5:1
 Actual buffer time is estimated
Shah
Vorname| 01.12.2022
Ort, Datum 70
Table: Tank calculation having pure EG
Maximum value considered 3 m³
Height 2.05 m
Diameter 1.365 m
Table: Designing of Hopper (cone+ cylinder)

m³
Maximum value considered 3
Fixed outlet Diameter 0.005 m

Height calculated 2.046 m
Inlet Diameter 2.356 m
Shah
Vorname| 01.12.2022
Ort, Datum 71
EQUATIONS
Shah
Vorname| 01.12.2022
Ort, Datum 72
MIXER DESIGN
Name,
Simha,Vorname|
Nithya | Ort, Datum 01.12.2022
Dortmund, 73
MIXER DESIGN
Vessel
Agitation
Impeller
Baffle
Fig 1 Construction of a
[1] https://www.comsol.de/blogs/simulating-an-ideal-stirred-tank-reactor-system/l; Last accessed on 27.11.2022
Mixter [1]
Name, Vorname|
Simha, Ort, Datum01.12.2022
Nithya | Dortmund, 74
INITIAL DATA FOR THE MIXER
Components Density[kg m-3] Volumetric flow rate [m3 h-1]
PET flakes 1340

1.8656
Ethylene glycol 1110
7.2072
Sodium carbonate 2540
2.3622
L/D ratio is taken as 3
[1] Perry, Robert H.; Green, Don W. (2008): Perry's chemical engineers' handbook. 8th ed McGraw-Hill
Name, Vorname|
CALCULATION FOR THE MIXER
Properties Value units
Diameter of tank 1,8
m
Tank height 5,3
m
Total volume flow 12,50
m3/hr
Impeller Diameter 0,9
m
Impeller Reynold’s number 19575
-
Speed of Rotation 3,3
rps
Power required for impeller 11099
W
[1] D. Qi, “Chapter 5 - Equipment in Rare-Earth Solvent Extraction-Separation Process: Mixer-Settler of Solvent Extraction,” Hydrometallurgy of Rare Earths,
pp. 591-630, 2018.
[2] SEEFRIED Verfahrenstechnik, GmbH, "Solid-liquid mixing," SEEFRIED Verfahrenstechnik GmbH, 27 11 2022. [Online]. Available: https://www.s-vt.net/solid-
liquid-mixing/?lang=en
Name, Vorname|
OUTLOOK

Discussed so far….
 Glycolysis: Process Flow Diagram
 Extensive Equipment Design and Dimensioning
 Calculation of Plant Utilities and Design

Future Agenda
 Process and Instrumentation Diagram
 Optimization of recycle streams back to reactor
 Process Heat Integration
 Cost Estimation of Process


PET Recycling Process Flow Diagram

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Project planning of a sustainable process

for PET waste recycling

Name, Vorname| Ort, Datum 2

Mechanical Chemical Thermal

Aminolysis Ammonolysis Glycolysis Hydrolysis Methanolysis Chemolysis

Name, Vorname| Ort, Datum 5

 Length to Diameter(L/D) ratio chosen for each reactor = 3.74

 Maximum filling in tank = 80% so,

 Type of Impeller: Flat 6-blade disc turbine

 Impeller Diameter: 1/3rd of tank diameter i.e. 0.33 m

Uniform Temperature Reaction Term Jacket Stirrer

 Enthalpy of Reaction is found to be 12kJ/mol of reacted amount of PET(ΔHR)

 Energy of Jacket = Stirrer – Reaction = 44.919 kW

 Total amount of steam(S): = 44.919/1858.2 = 87.024 kg/h

 Amount of steam in each reactor = 87.024/4 = 21.756 kg/h

 Material of insulation: Glasswool(thermal conductivity = 0.035 W/m-K)

PET is not soluble in EG at room temperature and only dissolves

[1] ‘Hildebrand solubility parameter’, https://en.wikipedia.org/wiki/Hildebrand_solubility_parameter.

Equation 1 Filtration area calculation

Solid content - 5-6 wt %

3.0 i.e.,> 0.005 oC-1 [1]

∆HSL = Melting enthalpy of BHET in EG (kJ.mol-1)

[1] Scribbr. www.steemit.com/steemstem/@josalarcon2/crystallizers-which-ones-to-use. Accessed 29 November 2022.

Y = Yield of crystallizer (kg.hr-1 )

1. Mullin, J.W., 2001. Crystallization. Fourth edition. Butterworth-Heinemann, A

have the same growth rate

Crystallization time (min)

Growth rate (m.hr-1) 3.542E-07

prevents undesired nucleation

the general crystal weight ratio of 0.1-1 % in EG[1]

EG is not aggressive to most materials Carbon steel

*Plate and Frame Press Filter chosen for Filtration

Filtration equation for constant pressure

30 Viscosity of Ethylene glycol at 25°C

[1] Engineering ToolBox, (2003). Ethylene Glycol Heat-Transfer Fluid Properties.

 For 15 frames with equal sides 1.001 m

1.001 × 1.001 × 0.008

1.001 × 1.001 × 0.1578

The time of washing is

𝑡 𝑐𝑦𝑐𝑙𝑒 =𝑡 𝑓𝑖𝑙𝑡𝑟𝑎𝑡𝑖𝑜𝑛+𝑡 𝑤𝑎𝑠h𝑖𝑛𝑔 +𝑡 𝑑𝑜𝑤𝑛𝑡𝑖𝑚𝑒 3.9 hours/cycle

Name, Vorname| Ort, Datum 55

Name, Vorname| Ort, Datum 56

Heater Heat Exchanger

Characteristics Plate and Frame Shell and Tube Scraped Surface

Cost per square foot Low Low High

Maintenance cost Medium Low High

Use with particulates Poor Good/Excellent Excellent

Amount of regeneration High Medium None

Large surface to Simple mechanical Well-established Can easily be cleaned.

- superior alternative to hot oils - cheaper

- higher thermal stability and film coefficient

- economical in long term - safer

 Flow Type Counter Current

 Number of passes 1 shell, 4 passes

 Tube pattern Equilateral triangle

 Shell type Split ring floating head

 Material Type 304 stainless steel

Area (m2) 16.25 28.08 9.42 8.42 13.7

Duty (kW) 648.8 642.6 563.5 426.6 195.8

Overall U (W/m2*K) 434.5 557.4 534.1 547.8 320.5

Velocity in Tube (m/s) 1.55 1.3 1.38 1.6 1.05

Velocity in Shell (m/s) 0.8 0.9 0.7 0.5 0.2