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23-Chem-A1 Process Balances and Chemical Thermodynamics · May 2016

Question 3 of 6: Crystallization and Rotary-Filter Entrainment

Nivaar worked solution (AI-drafted; not reviewed by a licensed engineer)

Notes on this paper

National Exams — May 2016 — 04-Chem-A1 Process Balances and Chemical Thermodynamics. Three-hour, open-book exam; any non-communicating calculator permitted. Format: six questions in two parts — Part A (Q1–Q3, Process Mass & Energy Balances) and Part B (Q4–Q6, Chemical Thermodynamics). Candidates answer two from Part A and two from Part B; four equally-weighted questions (25 marks each) constitute a complete paper. All six are solved below for completeness. Property data are stated explicitly in each Given block.

Reference texts: Felder, Rousseau & Bullard, Elementary Principles of Chemical Processes (4th ed., Wiley) — combustion/metallurgical stoichiometry, tie-substance balances and reactive mass balances; Himmelblau & Riggs, Basic Principles and Calculations in Chemical Engineering (8th ed., Prentice Hall) — ore/metallurgical balances and heat-of-reaction bookkeeping; Smith, Van Ness, Abbott & Swihart, Introduction to Chemical Engineering Thermodynamics (8th ed., McGraw-Hill) — reaction equilibrium, van’t Hoff analysis and VLE with activity coefficients; supporting data from Perry’s Chemical Engineers’ Handbook (9th ed.) and the NIST Chemistry WebBook.

Question 3: Crystallization and Rotary-Filter Entrainment (Part A — 25 marks)

Question text not reproduced: the examination questions are © Engineers and Geoscientists BC. Open the official past paper (linked at the top of this page) to read the question, then follow the worked solution below.

Given. Feed 1000 kg/hr, 60 wt% naphthalene ($M=128.17$) / 40 wt% benzene ($M=78.11$), cooled from 80 to 10 °C. At 10 °C the mixture lies in the “liquid + solid naphthalene” field; from the phase diagram the liquid (filtrate) lies on the naphthalene liquidus at mole fraction benzene $x_{Bz}\approx0.80$, i.e. $x_{naph}\approx0.20$. Measured filtrate rate = 505 kg/hr.

Find. (a) entrainment ratio, kg entrained mother-liquor per kg crystals; (b) the effect of that entrainment on naphthalene recovery and on cake purity, compared with an ideal (entrainment-free) separation.

00.20.40.60.81-10020406080naphthalene liquidusbenzeneliquid @10°C, x(Bz)≈0.80feed x(Bz)=0.52Mole fraction benzene, x(Bz)Temperature (°C)
Figure 2 — Benzene–naphthalene solid–liquid phase diagram (schematic, after Walas). Cooling the feed ($x_{Bz}=0.52$) to 10 °C crosses the naphthalene liquidus; solid naphthalene precipitates and the equilibrium mother liquor moves to $x_{Bz}\approx0.80$ (the tie line shown).

Approach. Convert the liquidus mole fraction to a mass fraction, close a benzene balance to find the ideal (entrainment-free) liquid and solid rates, then compare the measured filtrate rate against the ideal liquid rate: the shortfall is mother liquor retained (entrained) in the cake, which shifts recovery and purity.

  1. Liquidus composition (mole → mass). At 10 °C the filtrate is $x_{naph}=0.20$; on a mass basis $$w_{naph}=\frac{0.20(128.17)}{0.20(128.17)+0.80(78.11)}=\frac{25.6}{88.1}=0.291.$$ So the equilibrium mother liquor is 29.1 wt% naphthalene, 70.9 wt% benzene.
  2. Ideal (entrainment-free) split — benzene balance. If the cake were pure crystals, all 400 kg/hr of benzene would report to the liquid: $$L^\ast=\frac{400}{1-0.291}=564\ \text{kg/hr},\qquad S^\ast=1000-564=436\ \text{kg/hr crystals.}$$ The ideal naphthalene recovery would be $S^\ast/600=\boxed{72.6\%}$ at 100% purity.
  3. (a) Entrainment from the measured filtrate. Only 505 kg/hr of liquid actually leaves as filtrate, so the balance of the mother liquor is trapped in the cake: $$\dot m_{ent}=L^\ast-505=564-505=59.2\ \text{kg/hr,}\qquad \frac{\dot m_{ent}}{S^\ast}=\frac{59.2}{436}=\boxed{0.136\ \text{kg liquor / kg solids.}}$$
  4. (b) Effect on recovery and purity. The cake is now crystals plus entrained liquor: $\text{cake}=1000-505=495$ kg/hr. Naphthalene in the cake is the crystals plus the naphthalene dissolved in the entrained liquor $(0.291\times59.2=17.2$ kg): $$n_{naph}^{cake}=436+17.2=453\ \text{kg/hr}\;\Rightarrow\;\text{recovery}=\frac{453}{600}=\boxed{75.5\%},\quad \text{purity}=\frac{453}{495}=\boxed{91.5\%.}$$

Physically, the entrained mother liquor is a two-edged sword: it carries a little extra naphthalene into the cake, nudging naphthalene recovery up from the ideal 72.6% to 75.5%, but because that liquor is benzene-rich it dilutes the crystals, dropping cake purity from a nominal 100% to 91.5%. Better washing of the cake would recover the trapped benzene and restore purity.

QuantityIdeal (no entrainment)With entrainment
Filtrate (mother liquor)564 kg/hr505 kg/hr
Cake436 kg/hr (pure)495 kg/hr
Entrainment ratio00.136 kg/kg
Naphthalene recovery72.6%75.5%
Cake purity100%91.5%