Note: 1

When silica gel is regenerated, it is necessary to record temperature and the

liquid level in trichloroethylene evaporator as a record of regeneration in every
regular interval.
And at the time, steam heating in orger to evaporate trichloroethylene in
certain rate.
Ordinary evaporating rate of trichloroethylene is 100-1300 per hour.
Note: 2
When liquid temperature and vapour pressure in trichloroethylene
evaporator rise abnormally too high, stop regenerating operation and check the
inside of tower, pipeline and etc., Ordinary liquid temperature is 87-93 0C. Because
it may occur that silica gel in the tower is reduced to powder, and that is blockade
in pipes and etc., with powdered silica gel.
When trichloroethylene in the vessel part of trichloroethylene evaporator
decrease to bottom of vessel, stop steam heating. Then charge trichloroethylene
product into it again and restart up regeneration of silica gel.
Replacement of Silica Gel:
Silica gel is reduced to powder by the moisture, gradually, when it has been
used in certain period. So, it has been in certain period. So, it makes pressure
drop in the column and adsorbing capacity decrease. Therefore, it is necessary to
replace the silica gel with fresh one periodically, or to shift the silica gel.
At first trichloroethylene has been discharge from the column to
trichloroethylene evaporator take wet silica gel out of the column and dry it in the
air day light for about 2 days.
Dried gel is shifted to remove small pieces of bend with sieve sized about
10 mesh. Large bead is used again with fresh gel.

47
Trichloroethylene Production Section
Fractionator:
This is a tower to recover production perchloroethylene volume of liquid
charged at first is so much because of this process is a batch system. So this
equipment need a vessel in which liquid is saved.
Evaporator perchloroethylene is purified by refluence in tower. At first light
component which compose mainly trichloroethylene are distilled out from
fractionator and then pure perchloroethylene component is distilled out.
Perchloroethylene Drying column:
The column which removes moisture involved in pure perchloroethylene
component which is already removed acidic materials. This column is filled with
silica gel same as trichloroethylene drying column.
Feed Tan :
This is the storage tan of crude perchloroethylene component which is
recovered in dehydrochlorination section and has about 10m3 of volumes.
Reflux tan :
These are the reflux tan for, fractionator. Distillate, from fractionator
condensed in condenser, flow into reflux drum, and a part of it is sent to
fractionator as reflux and other part of it is sent to another vessel as an initial
boiling fraction or as perchloroethylene.
No.1 receiver:
This is a receiver tank of heavy component which is discharged from the
bottom of fractionator. The liquid in the tank is sent to dehydrochlorination
section, and is dehydrochlorinated to recover trichloroethylene and
perchloroethylene from it.
No.2 receiver:
The liquid in this tank is sent to trichloroethylene tank and is returned to
fractional distillation section.
48
This is a receiver tank of light component which is distilled out from the
fractionator.
Alkali tank:
This is a store tank for NaOH (10%) which is used for alkali washing of pure
perchloroethylene component.
Washing Drum:
This is a drum in which pure perchloroethylene component flowed the
fractionator is washed by alkali for effective washing, it provides with pump which
is available to mix alkali and pure perchloroethylene component.
No.1 Settler:
This is a settler in which the mixed liquid sent from the washing drum is
separated into alkali and pure perchloroethylene components.
No.2 Settler:
This is a tank which pure perchloroethylene component separated from
alkali is washed with water.
Product tank:
This is product tank for perchloroethylene which is drying column and the
product is measured and stored in this tank. Some amount of stabilizer is added
into perchloroethylene in this tank.
Reboiler:
This is a falling film type heat exchanger in which the vapour distilled from
the fractionator is condensed.

49
Cooler:
This is a shell and tube type heat exchanger in which pure perchloroethylene
component sent from reflux drum is cooled.
Feed pump:
This is a pump which feeds crude perchloroethylene components as a raw
material to fractionator from feed tank.
Alkali pump:
This is a pump which is used for mixing of pure perchloroethylene and
alkali in washing drum.
Recycle pump:
This is a pump which transfers the product from product tank to drum
filling equipment.
Stabilizer injection pump:
This is a pump which injects stabilizer into trichloroethylene and
perchloroethylene at the top of tower. Trichloroethylene and perchloroethylene
are apt tp decompose to form acid sustains while they are distilled, in the absence
of stabilizer, generated acidic material may gradually corrode towards and heat
exchanger.
To prevent the tower and exchanger from corrosion, stabilizer is injected,
using this stabilizer injection pump.

50
Testing and Preparation for Start Up:
General:
Trichloroethylene production section is almost the same as fractional
distillation section except batch wise operation.
Equipment:
Fractionator:
Cleaning inside:
The inside of the tower is washed and cleaned by steam or water, but this
operation may be substituted by an initial operation.
Steam is blown into vessel part of fractionator or tower through pipe
which is settled to a pare nozzle or another nozzle.
Water is charged through reflux nozzle of the top of tower. Following operation
must be referred according to articles of maintenance of equipment.
When temperature in tower rise up higher than 80 0C, hot bolting must be
done.

Perchloroethylene drying column:

Cleaning inside:
Operate according to No.2 trichloroethylene drying column.
Filling of silica gel:
Operate according to No.2 trichloroethylene drying column.
Feed tank:
Cleaning inside:
Wash and clean by water or steam using brushes or wire brushes.
Reflux tank:
51
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
No.1 Receiver:
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
No.2 Receiver:
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
Alkali tan :
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
Washing Drum:
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
No.1 Settler:
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
No.2 Settler:
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
No.2 Settler:
Cleaning inside:
Wash and clean by water or stream using brushes or wire brushes.
52
Product tan :
Cleaning inside:
Don’t use wire brush for cleaning.
Graduating on scale:
Graduate on the scale in accordance with the amount of charged water in
the vessel comparing with the calculated valve.
Reboiler:
Cleaning inside:
Wash and clean the inside of tubes by water or stream using brushes or
wire brushes.
Condenser:
Operate according to heat exchanger of dehydrochlorination section.
Cooler:
Operate according to heat exchanger of dehydrochlorination section.
Pumps:
Operate according to manual attached to pumps.
Stabilizer injection pump:
After assembling the pump make test operation of pumps using
perchloroethylene or water.
Test run with steam:
If necessary, test run with steam will be done, but usually this operation
may be substituted by an initial operation.
Feed water to vessel part of fractionator and heat it with steam directly or
using reboiler indirectly.

53
 Evaporate the water through the column. Section of fractionator and
condense the steam with condenser.
Remove the water from drain valve in reflux pipe line. The boiling water in the
fractionator is circulated to reboiler with recycle pump for the operation test of
recycle pump.
Feed the cooling water to condenser.
Make the irrigation test.
At the same time make a hot boiling, check the internal press of fractionator
and work of temperature recorder and flow recording controller.
After the trail run has finished.
Remove the water from all the equipments as well as possible.
Note:
Checking the instruments and pumps follows the instruction for the
instrument or pumps.

Normal operation:
Preparation:
feed the cooling water to condenser and cooler. Control the irrigation of
water to let the water flow smoothly and constantly.
Turn on the temperature recorder and flow recording controller.
Open the valve of reflux drum and open the reflux pipe line fully.
Feed the caustic soda aqueous solution from alkali tank to washing tank.
Prepare stabilizer injection pump and the stabilizer which is injected into
pipe line between fractionator and condenser.
Feed the crude perchloroethylene:
The crude perchloroethylene from dehydrochlorination section, stored in
feed tank, is fed to the vessel section of fractionator with feed pump.
54
Circulating the liquid:
Using recycle pump, the liquid fed to fractionator is circulated to reboiler
through fractionator.
In the case recycle pump breaks down or there are the leakage from recycle
pump, with thermosiphon let the liquid circulate.

Heating the liquid:

With FRC manual control, open the valve of steam line used for heating the
liquid (opening ratio 40-50%).

Note:
Gradual heating is necessary to avoid rapid temperature increases.
The temperature at the bottom and top of fractionator rise, and
trichloroethylene and perchloroethylene evaporate and condense at the
condenser.
And condensates are fed to reflux drum and being to reflux to fractionator
trough rotameter.
The distillate from fractionator is returned as total reflux fractionator through
rotameter. Control the valve of steam heating reboiler with flow recording
controller, so that the reflux would be about 2,200kg/hr.
When the reflux and temperature at the top ad bottom of fractionator settle
down, and the control valve of FRC controlling the steam used for reboiler settle
down, let a part of the distillate discharged from fractionator is discharged to
No.2 receiver.

55
 When the temperature of the vapour at the top of the tower reaches about
0
115 C change the reflux drum B to A.
When the temperature of the vapour at the top of tower rise near to 119 0C,
analyze the reflux about distillation range.
If distillation range of the reflux passes the spec.,
Fees the distillation, which has been let to No.2 receiver, to washing drum
by changing the low component pipe line to the product pipe line, as pure
perchloroethylene.
In the operation of distillation carefully handlings are required as follows.
Control the FRCV (valve of flow recording controller), used for steam to
heat the liquid with reboiler, to adjust reflux ratio to 10:1 or turn the discharging
valve in product pipeline in order to adjust ratio to 10:1
Inspect, observe, the internal press, of fractionator if the press, is raising by
degrees.
After the stop of operation, make a cleaning of tower.
When the temperature at the top of the tower reaches 121 0C analyze the
reflux about distillation range.
If is on spec., feed to product line some part of the distillate (1/10 of reflux).
If off spec., stop feeding a part of the distillate to product pipe line and turn the
reflux to total reflux for about 60 min.
Then, analyze the reflux about distillation range again.
If on spec., feed a part of the distillate to product pipe line.
Moreover, when the temperature of vapour at the top of fractionator is over
1210C, analyze the reflux about distillation range again and repeat above
mentioned operation stop operating on fractionation, when the temperature of
the vapour at the top and bottom of fractionator is rising over about 121 oC and
about 1400C and distillation range of the reflux does not pass the spec.,
56
 If it is decided to stop for the operation of the temperature of the vapour and
analysis of the reflux.
The distillate discharged from reflux drum as pure perchloroethylene is
cooled through cooler is fed to washing drum.
The liquid begins to flow inti washing drum then work alkali pumps, stir the aq.
Solution and perchloroethylene by circulating with alkali pump to remove the acid
substance contained in perchloroethylene.
The ejector between alkali pump and washing tank accelerates the effect of
this circulation.
Observe and confirm that the liquid is circulated in good condition.
Measure the concentration of alkali aqueous solution required to washing
tank from alkali tank in accordance with the results of measurement.
Pure perchloroethylene removed the acid substance with washing column
using 10% of NaOH aqueous solution is fed to No.1 settler in No.1 settler and
separated from alkali aqueous solution in this vessel. Pure perchloroethylene
separated from alkali aqueous solution is fed to No.2 settler.
Alkali aqueous solution separated from perchloroethylene is exhausted from
No.1 settler to trench as waste. It is no good that alkali aqueous solution is
discharged from No.1 settler too much and that perchloroethylene is discharged
from No.1 settler with alkali aqueous solution. It had better feed alkali aqueous
solution required to washing drum.
Pure perchloroethylene from No.1 settler is washed with water in No.2
settler to remove the alkali aqueous solution remained in perchloroethylene.
If too much, perchloroethylene discharged with water from No.2 settler to
the trench increase. So, it had better feed the water required to No.2 settler.

57
 Water if fed to No.2 settler at the time start alali pump. And control the feed
of water.
Pure perchloroethylene washed with water and separated from the water
continuously, is to fed drying column, demoistened in the column and fed to
product tanc.
Perchloroethylene is added stabilizer at product tanc. After the circulating
with product pump the liquid is analyzed.
When the cloud point of perchloroethylene is more than 15-20 0C, repeat the
drying of product once more anyway. And change the used drying column for
renewed one.
When the distillation range of perchloroethylene is not in the range of
spec., once more, mae the fractionation of perchloroethylene with fractionator
and or repeat it, until the perchloroethylene product pass the spec.,

Note:
It is necessary to tae care for analysis of the reflux, during the operation in
order to passes the spec., for perchloroethylene product.
When perchloroethylene does not pass to spec., about the acidity, repeat the
washing with alali aqueous solution and water for perchloroethylene product.
Stop the operation:
Stop the steam used for heating the liquid with reboiler.
Turn off the valve of FRC and main valve of steam line.

58
Stop the reflux:
Stop the reflux after the liquid level of reflux drum falls under the point of
liquid over flow nozzle. If the operation stops for long time (more than one day).
The liquid in the reflux pipe line is returned to fractionator, or recovered from
drain valve in the reflux pipe line.
Stop the operation of stabilizer injection pump. When feed of steam is
stopped, the vapour temperature at the top of fractionator begins to fall.
Stop the operation of stabilizer injected pump. The residue in fractionator
is fed to No.2 receiver with recycle pump.
Before this operation, charge cooling water. After the flow the distillate to
washing drum comes to a stop.
Stop the operation of alkali pump, then stop washing with washing drum,
and stop washing with No.2 settler or stop the feed of water used for washing at
No.2 settler.
If the stop of the operation lasts for long time (more than one day).
Perchloroethylene in the pipe line for washing and drying of
perchloroethylene is collected from the drain valve of cooler, washing drum, No.1
settler, No.2 settler and drying column.
Turn off the instruments:
Stop the cooling water:
The perchloroethylene product in product tank is transferred to drum
filling equipment.
Method for drum filling is in accordance with manual for drum filling
equipment.
Note:
Falling nozzle for the product is covered with clothes, to removes dust and
something lie that contained in the product.
59
 Utilities
Description:
The utilities used for trichloroethylene plant are as follows
1. 10kg/cm2G steam
2. 3kg/cm2G steam
3. Cooling water (include washing tower)
4. Brine
5. Nitrogen
6. Caustic soda
7. Sulfuric acid
10kg/cm2G steam is used for heating at No.2 fractionator reboiler in fractional
distillation section and at reboiler in trichloroethylene production section. And
after its pressure is reduced to 4kg/cm 2G, the steam is used at
dehydrochlorination reactor in dehydrochlorination section. 3kg/cm2G steam is
used for heating at reactor cooler in synthesis section, No.1 fractionator
reboiler and also at trichloroethylene evaporator in tractional distillation
section.
Cooling water is used for coolant at heat exchangers, pumps, vent
condensers, towers and etc., in all sections.
Washing water is condensed for process operation such as washing
gases, washing liquids and others. And also, it is consumed for washing inside
of equipment such as towers, vessels and others
Nitrogen is mainly used for purging the air or acetylene in equipment of
100, 200 and synthesis section.
Brine is used for cooling as a coolant at acetylene cooler and sulfuric
acid circulation cooler in acetylene purification section for cooling acetylene gas
and sulfuric acid which is used for drying acetylene.
Caustic soda is used in acetylene purification section for desulfuration from
acetylene and in trichloroethylene production section
60
for washing of perchloroethylene. Sulfuric acid is used for drying acetylene gas in
Acetylene Purification Section.
Preparation for Start Up:
Steam:
10kg/cm2G steam pipe line.
Confirm that there is not welding refuse or dust in the pipe, after the passing test.
Note: existence of dust is confirmed at strainer of drain trap.
Under passing test, check if every steam trap (attached to piping’s and
equipment) work normally.
And if they do not work normally, clean the strainer or adjust the screw of
steam trap so that they will operate normally.
3kg/cm2G steam piping.
Confirmation of inside dust.
Checking of steam, trap, strainer.
Regulation of pressure by reducing valve.
Reduce 10kg/cm2G steam pressure to 3kg/cm2G steam
The procedure are as follows: