List of content

Chapter 1
Introduction………………………………….………………….…3
Chapter 2
Sulphure melter………………………………..…..........................4
Air drying……………………………………..…………………...5
SO3 production……………………………….…………………...9
Sulphonation………………………………...……........................12
Gas liquid separator………………………………………………15
Cyclone…………………………………………...........................16
Electrostatic precipitator………………………………………….17
and so3 absorber
chapter 3
production of sodium silicate…………………………………….19
methods of production……………………………………………19
uses of sodium salicate…………………………...........................21
chapter 4
Multi-tube falling film reactor………………………..…………..22
Chapter 5
Washing tower plant……………………………………………...24
Chapter 6
Liquid detergent………………………………………………….27
References………………………………………………………..28

List of figure
Figure 1 sulphur melter………………………………………………………….…4

Figure 2 viscosity VS temperature curve………………………………….………..5

Figure 3 air drying unit…………………………………………….……………….6

Figure 4 Mole fraction of water in the air VS temperature…..……………………..7

Figure 5 SO3 conversion unit…………………………………………………..…...9

Figure 6 MTFFR unit……………………………………………………..………..12

Figure 7 cyclone…………………………………………………..………………..16

Figure 8 ESP and SO2 absorber…………………………..………………………..17

Figure 9 bock diagram for sodium silicate process.…………………………….….20

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Figure 10 MTFFR………………………….…………………………………….…22

Figure 11 spray drying tower…………….……………………………………………………………….…..23

Figure 11 simplified powder detergent plant…………………………………….…26

List of table
Table 1 air drying specifications……………………………………………………8

Table 2 conversion reactor specification…………………………………..………11

Table 3 working condition of MTFFR…………………………………………….14

Table 4 MTFFR specifications……………………………………………………..15

Table 5 Sulfonation reactor models..................................................................15

Table 6 gas-liquid separator specifications…………………………..…………….16

Table 7 cyclone specifications…………………………………………………...…16

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introduction
Detergents are chemicals that are effective surface and coming
instead of soap in many of the uses and areas , in the home and even
the factory are preferred in some uses because of its specification is
better than soap in hand uses this .The chemical composition is different
for the installation of soap, but the same mechanism by the soap, not
adversely affected by hard minerals in the water.
Have emerged detergents this first appeared in Germany during
the First World War because of the substantial shortfall in the fatty
materials necessary for the soap industry at that time. And then
spread in all countries .
At the beginning of the second half of the twentieth century past
sales exceeded sales of detergents , soap world , where replaced in the
field of laundry and household cleaning and industrial, with the
exception of templates soaps are still used to clean the body, which began
shampoo replaced by now.
In order to achieve good results for washing is required three main
factors in tandem with each other, namely:

1 - Chemical agent : This is provided by the soap and detergents.

2 - Mechanical agent : This is secured by a washing machine .
3 - Heat agent : This is secured by raising the temperature of water
`washing .`
Detergents There are many types of detergents , each type of
cleaning detergent its own , but often divided detergents mainly to :

1 - General detergent laundry , or detergents for all purposes.

2 - cleaners Uses easy.
3 - Detergents harsh surfaces .
4 - Detergent dishwashers mechanism.

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 Chapter 2
production of sulphonic acid
2.1sulphure melter

Figure 1 sulphur melter

When the solid sulphur quality is very poor, to improve it, the addition of
a separate melting and filtering day tank is foreseen. Addition of
chemicals and/or filtering earths may be required for the sulphur
purification. The solid sulphur to be purified is loaded to the melter and
addition of chemicals is subsequently done. The additional melter,
usually an underground vessel to facilitate the loading of solid
pretreatment agents, is therefore provided with a mixer - agitator and a
submersed pump to transfer the treated sulphur to filtration and to
the standard sulphur melter which melted by indirect contact with steam
producing from coils at temp 150°C at max; because above this temp the
viscosity with reach high valve and this will effect the pump that pumped
the melted sulfure to burner.

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Figure2 viscosity VS temperature curve

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2.2 Process Air Drying

Figure 3 air drying unit

Air drying is a fundamental step in the sulphonation process. The process

air to be used for S03 generation and for its subsequent dilution must be
dehumidified to keep moisture from reacting with S03 which can lead to
the formation of oleum and give rise to such problems as corrosion
and the reduction of sulphonation reaction conversion yield.
The air required for sulphur combustion and the production of S03 is
filtered and dehumidified to a dew point which is lower than -70°C.
This is because less vapor is needed to saturate the air, so vapor
condenses as the temperature falls. In normal conditions, the dew point
temperature will not be greater than the air temperature because relative
humidity cannot exceed 100%.

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 Figure 4 Mole fraction of water in the air VS temperature

In the plant this operation is carried out as follows:

The air, which is filtered to eliminate dust, flows to the process air
blower, which conveys it to the cooling unit where it is cooled to about
5°C. The blower operates at a very low pressure (0.6 bar gauge max.).
This low pressure, however, is sufficient for conveying the air both
through the S03 production unit and the sulphonation unit. The process
air-cooling unit consists of a chilling group and two refrigerating
exchangers carrying cooling water and ethylene glycol at a temperature of
around 0°C. This unit is designed to provide constant humidity
condensation in the process air, regardless of the existing climatic
conditions. At this stage the air is cooled and partially dehydrated. The
cooled, compressed air is then subsequently dried with a desiccant (silica
gel or alumina) in two parallel absorbers operating in sequence, i.e. one
on air drying and the other on regeneration. Switching over from the
absorption phase to the regeneration phase occurs automatically; the time
intervals, however, are constant. Part of the heat generated by sulphur

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combustion and the conversion from S02 to S03 can be utilized for
regeneration.

The most outstanding characteristics of this process section are:

- Simple design and mechanical reliability.

- Low operating pressure.
- Oversized absorption beds for longer operating cycles.
- Lowest dew point with highest energy efficiency.

• air drying detailed design

-Table 1 air drying specifications

Parameters Volume(m3) Diameter(m) Height(m) Efficiency(%)

Value 8.5 1.53 4.6 99.9

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2.3 SO3 Production

figure 5 SO3 conversion unit

In order for SO3 gas in air to be delivered to the sulphonator unit for the
sulphonation to take place, liquid sulphur must be burned. The liquid
sulphur must be delivered to the Sulphur Burner at 1:1 ratio.

The reaction that takes place at the Sulphur Burner is as follows:

S + O2 → SO2

The sulphur burner will also be connected to a tank of fuel -methane

(CH4) and a pump which will be necessary for plant start up purposes.
Excess air will be available in the sulphur burner to ensure that all the
sulphur present has reacted in order to reach the 99.9%. sulphur
efficiency, but also to ensure that the toxic sulphur does not pass un-
reacted into the later stages as this can damage the catalytic reactor and its
catalyst.
The reaction depicted above is very exothermic to produce an outlet gas
stream temperature of approximately 1048oC and therefore the sulphur
burner must be followed by air cooling that will cool the gas stream to
430°C.

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The cooled SO2 along with the other inert gases possessed by the stream
will be then delivered to a Catalytic Reactor. The catalytic reactor
contains 4 beds packed with the catalyst Vanadium (V) Oxide (V2O5).
The catalyst will help greatly in obtaining a good yield in the following
reversible reaction:

2SO2 + O2 →2SO3

The catalytic reactor will produce 99.9% conversion from SO2 to SO3,
for this to occur 4 beds will be necessary. The conversions that take place
in each bed are as follows:

1st bed: 0%-65%.

2nd bed: 65%-90%

3rd bed: 90%-96%

4th bed: 96%-99.9%

Each catalytic bed is followed by a condenser in order to cool the gases

down and in doing so obtaining a greater conversion to SO3. According
to the Le Chatelier’s Principle which states that if a dynamic equilibrium
is disturbed by a change in conditions, the system moves to counteract the
change and thus restore equilibrium. Therefore the following factors are
necessary in order to drive the reversible reaction to the right and obtain a
greater conversion:

• Decrease in temperature, as the reversible reaction above is exothermic

and a decrease in temperature would bring about a system move to the
right producing more SO3.

The heat exchanger after the catalytic bed has the task of cooling the gas
stream from approximately 620°C to 440°C. After the second bed, the
Heat Exchanger will cool the gas from approximately 512 °C to 450 °C
and then deliver to the third bed.
After the third bed the stream will exit at approximately 467°C and is fed
into the fourth Heat Exchanger which will cool it to 267°C.

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• SO2 conversion detailed design
- Table 2 conversion reactor specification:

Parameter Reactor Type Length(m) Diameter(m) Volume(m3) MOC

type of
catalyst
Value PFR V2O5 9.31 3.1 70.46 S.S

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2.4 Sulphonation

Figure 6 MTFFR unit

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Air with 7% SO3 is pumped to the Sulphonator, where it is contacted
with LAB and the following reaction occurs.

This reactor consists of a vertical bundle of long, small-diameter tubes, the

number of which depends on the plant production capacity. The S03-gas is
fed to the upper part of the reactor and equally distributed to each reaction
tube. The organic feedstock and S03-gas are fed co-currently. The liquid film
which is formed inside the tubes comes in contact with the gaseous reactant.
The length and diameter of the tubes have been optimized through a
computer model to provide best product quality performance. The special
design of the multi tube falling film reactor ensures accurate dosing of the
organic feedstock and S03 gas keeping the exact mole ratio between them.
Each individual tube is machined with utmost mechanical precision so to
ensure identical performance in gas and liquid flow distribution. The liquid
flow can be actually checked and further adjusted to dosing accuracy within
0.5%. This accuracy is achieved with metal washers and nozzles of special
design which ensure high precision within the entire range of feedstock
characteristics and production capacity. In addition to these mechanical
features which ensure as such the best possible geometric distribution,
the reactor design has unique performances of gas liquid self-adjustment.
Even in case of differences in the liquid flow, the corresponding gas flow is
proportional to the overall film thickness, which is established by the
viscosity profile as a direct function of the sulphonation degree in each
single tube.

The Mole Ratio Control System

Sulphonation process control via optimized mass balance: The exact mole
ratio between the S03 and the organic feed is essential for obtaining the
maximum degree of conversion and excellent colour with all types of
feedstock. The best theoretical sulphonation yield for a given organic
feedstock is obtained by optimizing the SO3/organic mole ratio and
equally distributing the reactants in the sulphonation reactor. Any excess
S03, especially in areas of the reactor where the cooling is critical, will
cause local charring, which will degrade both the product colour and the
degree of conversion.

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In fact, optimum conversion of raw material to sulphonate is nearly a
direct function of mole ratio, while at mole ratios even slightly higher
than optimum (usually in the range of 1.02-1.05 mole S03 to 1 mole
organic), the product darkens rapidly and coloured by-products are
generated. To further improve product quality scientists has developed
and successfully implemented an SO/organic Mole Ratio Control System
based on the use of mass flow meters.

• OPERATING CONDITIONS OF MULTITUBE FILM

REACTOR
-Table 3 working condition of MTFFR

Parameter Feedstock (LAB)

SO3/organic mole ratio 1.01-1.03
SO3 concentration (%vol) 5-8
Cooling water temperature (°C) 34-36
Acid outlet temperature (°C) 45
Ageing temperature (°C) 50-55

Main features of the unit:

•Outstanding performances in terms of product quality.

•High operating flexibility because of the capability to process any raw

material used in detergent and surfactant industry.

•High reliability and operation easiness.

•Very high heat transfer efficiency that enables an accurate control of the
temperature profile in the reactor.

•Low pressure drop (0,3 Kg/cm2 average) resulting in a reduced energy

consumption of the whole sulphonation plant.

•High reliability and longer lifetime because of useing sophisticated

corrosion resistant alloys in critical parts.

•Very high heat transfer efficiency that enables an accurate control of the
temperature profile in the reactor.

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• uses of sulfonic acid

1-Detergents and surfactants

2-Dyes

3-Acid catalysts

4-Drugs

• Multi-tube falling film reactor detailed design

-Table 4 MTFFR specifications

parameter No. of FFR Length(m) Diameter(m) MOC

tubes thickness
Value 60 .0012 7.54 .0187 CS

-Table 5 Sulfonation reactor models

No. of tubes 1 24 36 48 60 84
LAB Kg/hr 5 1000 1500 2000 2500 3000

2.5 Gas liquid separator

The separation of liquid droplets and mists from gas streams is analogous
to the separation of solid particles and, with the possible exception of
filtration, Where the carryover of some fine droplets can be tolerated it is
often sufficient to rely on gravity settling in a vertical or horizontal
separating vessel .
In some cases demisting pads are frequently used to improve the
performance of separating vessels where the droplets are likely to be
small, down to 1µm, and where high separating efficiencies are required.

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Table 6 gas-liquid separator specifications
Parameter Value
Diameter (m) 1.9
Height (m) 3.3
MOC Carbon steel

2.6 Cyclone

Cyclone separators are also frequently used for gas liquid separation.
They can be designed using the same methods for gas solids cyclones.
The inlet velocity should be kept below 30 m/s to avoid pick-up of liquid
form the cyclone surfaces.

Figure 7 cyclone

-Table 7 cyclone specifications

Parameter Value
Diameter(m) .16
MOC Carbon steel

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2.7 Electrostatic precipitator and so2 absorber

Figure 8 ESP and SO2 absorber

Electrostatic precipitators are capable of collecting very fine particles,

<2 µm, at high efficiencies. However, their capital and operating costs are
high, and electrostatic precipitation should only be considered in place of
alternative processes, such as filtration, where the gases are hot or
corrosive. The exhaust gas, containing small amounts of non-converted
S02, unreacted S03 and some entrained organic acid, has to be cleaned
before emission to ambient atmosphere. The organic aerosol and fine S03
droplets are first separated from the exhaust gas flow in an electrostatic
precipitator (ESP) and reprocessed in the plant. The ESP consists of a
bundle of tubes mounted vertically with each tube containing an axially
mounted electrode. The potential difference established between the
electrodes and the walls of the tubes electrically charges the impurities
located in the gas stream. These forces cause the particulates to migrate

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toward the positive anode (the tube wall) where they coalesce on the
surface and drain off under the influence of gravity. The gaseous stream
containing the residual unconverted S02 is then treated in a packed
scrubber column, where water and caustic soda solution are continuously
added and recycled. The S02 reacts with the caustic soda to give sodium
sulphite, which is discharged as aqueous solution. The feeding of the
caustic soda solution is done automatically and is controlled so as to
maintain the scrubber liquor at the required pH. This reaction is
performed by means of a specially designed packed column where
intimate contact between the gas and liquid phases is obtained counter-
currently. The liquid enters the top of the column and flows downward
through the column, which is filled with plastic rings to ensure sufficient
surface contact and avoid the formation of preferential pathways of the
liquid through the bed. The liquid leaving the bottom of the column is
continuously re-circulated to the column and is overflowed to the
downstream oxidation unit. Part of the NaHSO3 which is oxidized to
NaHS04 by the excess of air contained in the exhaust gas, is then
discharged from the scrubbing column at about 10% concentration and
constant pH (about 8.5).The amount discharged is directly proportional to
the amount of non-converted S02. The clean, water saturated gas is then
discharged to the atmosphere.

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 chapter 3

3.1 The production of sodium silicate

Sodium silicate is a product with unlimited possibilities. It is a chemical
compound of silicon dioxide (SiO2produced from pure silver sand),
disodium oxide (Na2O) and water. There are two methods for the
production of sodium silicate:

• Methods of production

1-Hydrothermal production of sodium silicate

With the hydrothermal process, also known as the 'wet process', silver
sand (SiO2) is reacted with caustic soda (NaOH) and water. The result is
an alkaline liquid sodium silicate with a molar ratio less than 2.5.

2-The furnace process for sodium silicate

With the furnace process, soda (Na2CO3) and sand are fused at
temperatures over 1000 °C. The result is a glass-like sodium silicate with
a molar ratio that is usually greater than 2.5 (standard ± 3.4). The
resulting product (commonly called cullet) can be dissolved under
conditions such as pressure, temperature and time to produce neutral
silicate. Molar ratios up to 3.5 are possible.

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• Hydrothermal production of sodium silicate

Figure 9 bock diagram for sodium silicate process

Sodium silicate solution is obtained by chemical attack of silica sand with

caustic soda through a two-steps reaction path, as per following reactions:

2NaOH → Na2O + H2O

Na2O + nSiO2 → Na2O*nSiO2 n

Caustic soda fed to the reactors undergoes a dissociation generating

sodium oxide which, in its turn, reacts with silica contained in the sand so
producing sodium silicate.
The reaction process, occurring in presence of 12 bar pressure saturated
steam, is carried out batch-wise inside stirred reactors, autoclaves type,
where silica sand, caustic soda solution at 50% and water are charged in
appropriate quantities.
The reaction is exothermic reaction.
At 48°Bé density, the finished sodium silicate solution contains 41.8% of
dry material, the remaining being water

The plant includes the following sections:

Raw materials dosing.

Solid and liquid raw materials dosing is carried out by means of reactors
weighing systems.
Opportunely sieved silica sand is charged into the reactors by means of
screw conveyors while caustic soda solution and water are fed by pipes,
carefully respecting the quantities required by the batch.

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•Reaction

Two autoclaves type reactors, working in parallel configuration, are

generally foreseen.
Operating conditions maintained in the reactors during the 8 hours cycle
are: pressure 11- 12 bar and temperature 188-192°C.
Sodium silicate solution leaving the reactors at high temperature is cooled
down to a temperature suitable for the following treatment of filtration.

•vessel
the product is leaving the reactor going to the vessel with conical bottom
to facilitate the settling of unreacted silicon dioxide, the vessel involving
three suction pump located vertically to the product to the next stage.

•Filtration of sodium silicate solution

Sodium silicate solution is carefully filtered before its final storage.
Filter-press type filter is used.

uses of sodium silicate

1-In the fabricate of Silica Gel

2-In foundry

3-In mining and development

3-In cleanser make

4-In paper industry

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 Chapter 4
multi-tube falling film reactor

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Nozzle-set: A complete unit comprising a female part, a male part,
respective tightening arrangement, tightening bolts and sealing system.

Reactor tube: A conventional tube, total length 5-7 m, and fixed to the
female part of the nozzle-set. The reactor tube represents in this way the
zone for the chemical reaction taking place, and transfers heat of reaction
to the surrounding and circulating cooling liquid.

Multi-tube falling film reactor has a complete reactor unit including from
two to more than hundred reactor-elements together with separate
chambers for distribution of gaseous reactant, liquid organic reactant,
cooling liquid, collecting chamber for finished product and connections
for all material flows. organic chamber defined and limited by a
cylindrical plate fixed to a cylindrical spacer fixed to a counter-flange
bolted and sealed to the lowest cylindrical plate.

Calibration of nozzle-set: Manual and time consuming work for all

individual nozzle-sets, at least the reactor head must be fully assembled to
accomplish this procedure. A quantity of organic reactant normally
corresponding to the nominal capacity of is the reactor, is fed to the
common organic chamber, and all the individual flows leaving nozzle-
sets or reactor tubes, are carefully determined by weighing. Based on the
measuring results from this procedure, an arithmetic average for the
individual flows 20 is calculated, for instance Xav. Any deviation outside
a predetermined and acceptable range, will have to be adjusted for by
replacement of the shims having thicknesses different from the ones
originally installed. Normally this procedure will have to be 25 repeated
until several times to reach a range described by:

Xav=1%

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 Chapter 5

5.1 Washing Powder Plant

Figure11 spray drying tower

Spray-Drying processes produce the highest quality of detergent than any

other process. The Blender process is most suited for smaller batch type
processes and therefore it is unsuitable for use with the production rate of
10 tonnes/hr, whereas the Spray-Drying process is very suitable for a
large scale continuous process such as this one. The agglomeration
process is another method that can be used to produce detergent, however
this process does not produce the great quality detergent; therefore this
method is not applicable. Builder, surfactant and solid additives are stored
in Silos, the Silos have De-dusting Filters to remove any solid dust that is
produced. The Silos deliver a certain amount of pre-determined weight to
a Weight Conveyor, this is delivered to a Pre-mixing Screw where the
solids are mixed evenly together. A De-ducting Filter is also present to
remove dust that is produced on the Weight Conveyor, this air is filtered

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out, the solid is returned back to the Pre-mixing Screw and the remaining
clean air is released to the atmosphere. Liquid Additives are delivered to a
Liquid Vessel, where they are mixed and pumped to a Slurry Crutcher
along with the Solid Additives. The mix is then transferred to a Magnetic
Filter, where lumps that can clog Spray-Drying Tower nozzles are
removed. The resulting stream is transferred to an Ageing Vessel, where
it is homogenized. The stream is then separated into two and passed
through another subsequent Filter to ensure that no clogging takes place.
Any filtered out lumps removed by the Filters are transferred to a
Recovery Slurry Vessel, which is filtered and pumped back as a Liquid
Additive. After the Filters, the slurry is pumped to a High Pressure Pump,
which pumps the slurry to a high displacement circuit that splits the
stream into 4. These 4 streams are sprayed into theSpray-Dryer. A Hot
Air-Generator supplies the Spray-Drying Tower with hot air needed for
the drying to take place. The hot air flows in from the bottom of the
Tower counter-currently at approximately 400oC to the detergent falling
from the top. Air is pumped into the Hot-Air Generator by a Combustion
Air Fan. The outlet air leaves the Drying Tower at a temperature of
approximately 85OC to a De-dusting Filter that filters out any solid
particles that have been transferred from the slurry and return it back to
the Drying Tower. The air is then dried and fed back to the Hot-Air
Generator. Subsequently, the dried slurry leaves the Spray-D it. The
stream is lead to a Vessel where it drying Tower from the bottom and is
transported by a conveyor belt to Crystallization Unit Conveyor where it
is lifted to a height through cooling down the stream and crystallizing is
dropped down to a Vibrating Sleeve that removes the wet agglomerated
product, which is approximately 1% of the stream. The resulting product
is then passed onto the Additives Mixer where perfume and enzymes are
added. The final product can then be transported to packaging and
storage.

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Figure 12 simplified powder detergent plant

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 Chapter 6

Liquid detergent

Liquid detergent is a type of detergent i.e. cleaning agent. Its popular use
is to wash woolen cloth but it is also used for washing of utensils
specially glass and crockery, and for automobile wash. Now a days it is
widely used in washing machines, laboratories etc.
The manufacture of liquid detergent is a neutralization process of acid
slurry by caustic Soda keeping pH 7 to 9. Acid slurry and water is mixed
slowly in the mixer, after that it is neutralized by the aq. Solution of
caustic soda to get the required pH. AOS is used as foam booster while
urea is a buffering agent and also create transparency. Lastly colour and
perfume is added.

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References

Coulson & Richardson’s CHEMICAL ENGINEERING VOLUME 6

www.desmetballestra.com

https://www.iitsrl.it/sulfonation

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