ZAKŁAD DYDAKTYCZNY TECHNOLOGII CHEMICZNEJ WYDZIAŁ CHEMII UNIWERSYTET WARSZAWSKI

Continuous process of sodium bicarbonate

production by Solvay method

Manual to experiment nr 10

Instructor: Dr Tomasz S. Pawłowski

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Goal of the experiment

The goal of the experiment is introduction of industrial, continuous

process of sodium bicarbonate production by Solvay method.

Experiment description

Chemical, laboratory installation to sodium bicarbonate production by

Solvay method is the model of industrial installation. It consists of two,
main units: the tower where the brine (water saturated with sodium
chloride) is being saturated by ammonia and the tower (carbonating
column) where ammoniated brine is being saturated by carbon dioxide.
Both reactors are connected to each other. During the sodium
bicarbonate production process reactors are being fed continuously by:
carbon dioxide, ammonia and brine. Continuous process demands the
substrates feeding rate and the carbonating column temperature keeping
on the stable level. Sodium bicarbonate suspension is periodically being
collected, then filtrated and the chloride as well as ammonia
concentrations in the filtrate have to be stable. Chloride and ammonia
concentrations are controlling by means of the titration analysis.

Experiment execution

Before experiment execution put the protective apron, glasses (unless

the correction glasses are worn) and the latex gloves on. Read the
material safety data sheets (MSDS) of the substances used during
experiment. Check the equipment status up, turn the lifts and electric
slats on.

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The numbering of the apparatus of the chemical installation describing

in the manual is based on the scheme presented below:

Legend:

1. Carbon dioxide cylinder,

2. Ammonia cylinder,
3. Carbon dioxide rotameter,
4. Ammonia rotameter,
5. Carbon dioxide manostat,
6. Ammonia manostat,
7. Peristaltic pump,
8. Graduated cylinder with brine,
9. Valve,
10. Valve,
11. Absorption column,
12. Valve,
13. Valve,
14. Carbonating column,
15. Motor stirrer,
16. Thermostat,
17. Valve,
18. Vessel with ammoniated brine.

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1. Fill the both towers (nr 11 and 14) with the ammoniated brine from
the vessel nr 18 to specified level. Use the peristaltic pump (nr 8)
and rubber hose. During filling turn the water thermostat on (nr
16).
2. Prepare the burettes to all titration analysis (with NaOH, HNO3 and
AgNO3 standard solutions), indicators (potassium chromate, methyl
orange, phenolphthalein) and formaldehyde. Determine sodium
chloride concentration in the brine according to the receipt below:

Pipette 10 ml brine solution to 250 ml volumetric flask and fill up

to the mark with distilled water. Then, from the solution obtained,
take 5 ml to Erlenmeyer flask and add a little bit distilled water and
a few drops of potassium chromate solution as indicator. The
solution prepared titrate by 0.1 M AgNO3 to get brown colour of the
precipitation.

NaCl (GNC ) concentration calculate according to the formula:

v p · 0.005846 · 1000
GNC  g/l
0.2

where: – volume in ml of 0.1 M AgNO3 used to titration, –

correction with regard to indicator = 0.2 ml, 0.2 – volume in ml of
origin solution used to analysis ( 1/50 from 10 ml), 0.005846 –
amount in g of NaCl correspond with 1 ml of 0.1 M AgNO3.
3. After filling of both reactor columns by ammoniated brine turn the
peristaltic pump and motor stirrer (nr 15) of carbonating column
on.
4. Open the valve nr 10. Open valves (main and reducer valve) of the
CO2 cylinder (nr 1). The value of CO2 flow should be defined,
controlled on rotameter nr 3 and kept on the stable level. Write the
hour of starting the carbonating process.
5. Prepare, label and weight three Erlenmeyer flasks and Petri dishes.
Fit the kit to filter under low pressure.
6. After about one hour of carbonating process, when the white
suspension of sodium bicarbonate is appeared in the carbonating
column, put the labeled flask under tap, down of the carbonating
column, open the valve nr 17 and let the suspension up to defined
(marked) level.
7. Open valves (main and reducer valve) of the NH3 cylinder (nr 2). The
value of NH3 flow should be defined, controlled on rotameter nr 4
and kept on the stable level. Turn the peristaltic pump on and start
brine feeding of absorption column. Write to the table attached (see
below on the pattern): the hour when the process has started and
the brine volume in the graduated cylinder (nr 8).

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8. At 10 minutes intervals through the valve nr 17, collect, by

dropping the suspension up to marked level on carbonating column,
three portions of it to Erlenmeyer flasks. Each portion cool in cold
water, weight and then filter under low pressure.
9. Measure the filtrate volume and the mass of the wet sodium
bicarbonate. All results write to the table.
10. From the filtrate of the last portion prepare basic solution which
will be used to titration in order to determine the chloride and
ammonia concentrations:

Pipette 10 ml of filtrate to 250 ml volumetric flask and fill up to the

mark with distilled water – such prepared solution is basic solution
to carry out all titrations described below.

11. Carry out three types of titrations:

Determination of chloride and free and weakly bounded ammonia:

Place 5 ml of the basic solution in Erlenmeyer flask and dilute with

small amount of distilled water. Then titrate with 0.1 M HNO3
solution in the presence of the methyl orange (to the first change of
colour) in order to determine free and weakly bounded ammonia.
Then, to the same solution add a few drops of K2CrO4 solution and
titrate with 0.1 M AgNO3 to get brown colour of the precipitation.
Concentrations of the free and weakly bounded ammonia and
chloride anions calculate from the below formulas.

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Concentration of the free and weakly bounded ammonia (GNH, ):

v · 0.0017 · 1000
GNH,  g/l
0.2

where: v – volume in ml of 0.1 M HNO3 used to titration, 0.0017–

amount in g of NH3 correspond to 1 ml of 0.1 M HNO3, 0.2 – volume
in ml of origin solution used to analysis ( 1/50 from 10 ml).

Chloride concentration (GC ):

v p · 0.003546 · 1000
GC  g/l
0.2

where: v – volume in ml of 0.1 M AgNO3 used to titration, p –

correction with regard to indicator = 0.2 ml, 0.2 – volume in ml of
origin solution used to analysis ( 1/50 from 10 ml), 0.003546 –
amount in g of chloride correspond with 1 ml of 0.1 M AgNO3.

Determination the total concentration of ammonia:

Pipette 5 ml Basic solution to Erlenmeyer flask. Neutralize with 0.1

M HNO3 in the presence of the metyl orange. Add 4 ml of 40%
formaldehyde (before neutralized in the presence of the
phenolphthalein) and leave for 1 minute to react. Then titrate the
educed acid with 0.1 M NaOH in the presence of phenolphthalein to
the pink color.

Total concentration of ammonia (GNH,"#".):

v · 0.0017 · 1000
GNH,"#".  g/l
0.2

where: v – volume in ml of 0.1 M NaOH used to titration, 0.0017–

amount in g of NH3 correspond to 1 ml of 0.1 M NaOH, 0.2 –
volume in ml of origin solution used to analysis ( 1/50 from 10 ml).

12. After collection the last portion of sodium bicarbonate suspension

turn the all cylinder valves (with CO2 and NH3) off. Empty and clean
carbonating column.

13. Clean the laboratory equipment and make the laboratory stand
ready to the next experiment.

14. On the basis of approved and signed table with results prepare the
report of the experiment according to requirements below.

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Report of the experiment should include

1. Goal of the experiment,

2. Experiment description:

a) scheme of the apparatus,

b) description of the operations performed and the conditions
and parameters of the process,
c) measurement results (results sheet).

3. Elaboration of the results:

a) chemical equations,
b) mathematical elaboration of the results obtained:

• Extent of sodium intake in two methods:

a) as the ratio of number of NH4Cl moles in the final solution

(filtrate) to initial number of NaCl moles (exist in the brine, in
graduated cylinder):

GNH,& · 35.46
UN I  · 100%
17 · GC

where: GCl – chloride concentration in the filtrate, 35.46 i 17 –

molar mass of chloride and ammonia, GNH3,zw – bounded
ammonia in the filtrate:

GNH,&  GNH,"#". GNH, g/l

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b) calculated from the weight efficiency of sodium bicarbonate

(W):

GNHCO
UN II  · 100%
W

where: GNHCO – weight of dry sodium bicarbonate in [g/h], –

theoretical efficiency of sodium bicarbonate calculated by
means of the formula:

S · 84
W g/h
58.5

where: – NaCl amount introduced into the carbonization

with the brine solution in [g/h], 84 and 58.5 – molar mass of
sodium bicarbonate and sodium chloride.

• Extent of utilization of ammonia (123 ):

423,5
123  · 100%
423,676.

4. Discussion of the results,

5. Conclusions.