Trouble-shooting

Distillation processes are often plagued by problems that affect product purity and

capacity. Product purity is very important to the company because off specification

products can not be sold leading to entire batches of product being wasted. This

constitutes a waste of energy, time, and raw materials. Product capacity also affects a

companies bottom line because the more product that is produced the more that can be

sold. Problems in product purity and capacity may often be remedied fairly easily in

distillation processes. If a well-organized guideline is available for technicians and

engineers alike to follow losses incurred from off specification products and reduced

capacity may be minimized. Thus the design group for this particular process will outline

a guide to remedy problems incurred during start-up and normal operation of the column.

This guide will list common problems, their “symptoms”, and steps to remedy the

situation or problem. Preventative measures that should be adhered to when operating

the column are also given. This is an owner’s manual of sorts for the process.

Start-up

It is very important that the distillation process be brought online very slowly. In

particular the steam system for the reboiler may suffer severe damage if brought online

too quickly. Steam velocities are highest during start-up. Newly fitted pipes may contain

weld, mill slag, dirt, and rust. These solid particles combined with the high steam

velocities at start-up may cause damage due to corrosion and erosion19. Also during

start-up steam pipes are usually cold depending on ambient weather conditions. These

cold pipes lead to excessive condensation in the steam lines. Condensation already
present in a steam line acts as a barrier to heat transfer. Also condensation leads to

erosion due to water hammer10. Water hammer is damage caused by a fluid hitting a

valve, pump, or pipe wall with too much momentum. Finally non-condensibles are

usually present in their highest concentrations during start-up. Air entered the system

during installation and must be removed before optimal system performance will be

obtained.

Starting up the process slowly also helps to prevent damage to centrifugal pumps.

Centrifugal pumps create a region of low pressure at their impellers. This causes the

liquid to vaporize. As the stream moves through the pump regions of higher pressure are

encountered, causing the vapor bubbles to implode. This causes a form of damage

known as cavitation18. Slow start-ups help to ensure the pumps have enough net positive

suction head to prevent liquid vaporization thus preventing cavitation.

Auxiliary Equipment

Problems with column auxiliary equipment will undoubtedly lead to decreases in

efficiency and capacity. Thus a well-planned routine of maintenance and preventative

care will increase auxiliary equipment life and effectiveness. Reboilers mostly suffer

from corrosion and fouling problems. Tube side vaporization of product may leave

deposits on the tube increasing the thermal resistance of the system and leading to

decreased heat transfer. Technicians may watch for this behavior by closely monitoring

the reboiler temperature and pressure needed to maintain a given heat input. Rises in

pressure and temperature indicate fouling. Regular backwashing and choice of proper

metals for building materials may reduce fouling in the system.

Liquid Levels

Low and high liquid levels in the column are also of concern. Liquid levels in the

reboiler and condenser should be monitored periodically. Low liquid levels reduce

efficiency and are usually caused by flooding in the column. Low liquid levels also

increase vaporization induced fouling. Low liquid levels may be remedied by lowering

the vapor flow rate. Low liquid levels in the reboiler may be due to blockage of the tray

downcomers. Foreign objects in downcomers or improper feed treatment may cause this

blockage.

High liquid levels are also a problem. High liquid levels are characterized by

increases in column pressure drop. Dumping in the column may cause high liquid levels

in the reboiler. These high levels flood the vapor disengagement space throughout the

column. This leads to separation inefficiency. Dumping may be remedied by increasing

vapor flow rate in the column.

Condensers usually do not suffer from severe fouling. Solids are mostly removed

in the column during vaporization of the more volatile components. However low

coolant temperatures may lead to freezing of the product which will plug the product line.

Fouling may be a concern on the coolant side due to low fluid velocities, however this

phenomenon may be prevented with regular backwashings of the coolant lines. Other

common problems occur from product liquid back up in the condenser system. This may

be caused by excessive condensation or as a result of entrainment in the column. This

behavior may be remedied by installing the process drain in a nearly vertical arrangement

to employ the aid of gravity in preventing liquid back up.

Main column efficiency

 Fluctuations in column efficiency are to be expected in any distillation process.

Design specifications are set so that these fluctuations do not lead to off specification

products. If large changes in heating and cooling loads are observed to achieve a given

separation steps should be taken to bring the system back to its original operating

conditions. Flooding is one cause of column inefficiencies. Jet flooding is when liquid

on a particular tray is carried to higher trays by the vapor flow or as a result of foaming.

Technician may assume a column is jet flooding if increases in pressure drop across a

tray are observed or if surges of liquid are observed in the overhead product19. Flooding

may also be observed in the downcomers of the column. Excessive liquid flow may be to

blame for downcomer flooding. Feeds that are introduced at low temperatures may flash

in the downcomer causing flooding by entrainment. Also restrictions and blockage

caused by loose tools or loose tray parts may block the downcomer and cause the liquid

to back up. If a particular tray exhibits an unusually large pressure drop the downcomer

should be checked for blockage.

Weeping is when liquid flows down the column through the tray orifices or holes

and not over the weirs at the end of a tray. Weeping may be characterized by a reduction

in pressure drop across a tray. Increasing vapor flow rates within the column will

counteract weeping.

Effect to Cause

• Effect: Surges in overhead product, falling base liquid level, high column

temperature profile, erratic pressure drop, and reduction in product quality.

• Cause: Flooding, (downcomers backed-up, excessive vapor flow rate)

• Effect: High boil-up rate, off specification product, and excessive reflux rate.
• Cause: Inadequate liquid and vapor contact, poor disengagement