flpr 01 99 03:43p Gene Dedick 1-920-490-9893 P-2

..
..

Reynolds Recovery Systems

Provides the Solution

energy from your digester to efficient&clean foul condensates.

,InexpensiveStr!ping of Tupentine and

.-
,.

TRSfromyour Foul Condensate Streams ...

. .
.
..
~

WIREYNOLDS RECOVERY SYSTEMS

a di* ofTampa Tank, Inc.

-
 flpr 01 9 9 0 3 1 4 4 ~ G e n e Dedick 1-920-490-9893 P - ~

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The Foul condensate Stripper May Be Used to Clean the Following Streams
-

Decanter underflow
Blow heat-secondary and tertiary condensates
Primary heat recovery tank overflow
- Evaporator barometric seal tank condensate , ..

First and second stage washer filtrate tank vent condensate

Primary condenser condensate from inoperative partial condensate system
--
NCG knock-out and seal pot drain
Multi-stage stripping tower feed streams (cleans turpentine and TRS)
..

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.- i - Cooling Water

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-
Turpentine Recovery is the latest and mart efficientprocess to inexpemiuely sbip turpentine and
malodorous TRS h m your foul condensate streams.
-

-
 Apr 01 99 0 3 - 4 4 p Gene Dedick 1-920-490-9893 P- 4

-.

- -

--
Benefits of the Foul Condensate Stripper
In the Wrpentine Recovery Area:
-- Cost Effective
- No prime steam required to drive this shipping sgstem
-..
. - Inexpensive when compared to alternatives .,
..
- No extra labor or supervision required to operate this system
- Increases turpentine recovery
. .-
- Provides "clean" foulhot water for brown stock washing
- Cleans digester relief vapor of fiber and some liquid carry-over before
.- the vapor reaches the turpentine recowry system
- Can be part of the original &tern or an easy @rofiV'modification of
- existing system --..
- Pits easily into existing digeater relief vapor line .
" +

-
Reduces
- Cooling water supply requirements
- - Condenser surface requirements
- Vapor load on existing condensing system
..
- BOD load to waste plant
- TRS emissions to the water and air
-.

In .the Multi-Stage Stripper Area:

In addition to many of the benefits above,
the foul condensate stripper in the multi-

- b a viable back-up for the typical

multi-stage foul condensate stripping
system whose primgy function is to
remove methanol
- Cleans foul condensate feed there by
reducing (essentially eliminating) red
oil formation in the stripping tower

- Preheats multi-stage stripper feed ,

flpr 01 99 03:45p Gene Dedick 1-920-490-9893
P- 5

Turpentine
Recovery

A pulp mill with ~e complete RRS Twpentine Recovery System was recognized two
years in a row as having the Most Improved Turpentine Recovery of the 65 report-
ing mills in fie Pulp Chemical Associatio~.

Technical and Process -Jacksonville, FL

Ellis Reynolds
Tel. 904-733-6460 Fax 904-733-5756

-
Sales and Manufacturing Tampa, 'FL
Jim Daniels
Tel. 813-623-2675 F a x 81 3-626-1641

-
Sales Atlanta, GA
Frank Pontious
Tel. 770-419-2642 Fax 770-419-1537

REYNOLDS RECOVERY SYSTEMS

a division ofTampa Tank Inc.
5205 Adam0 mve Tampa,Florida 33675
Tel. 813-623-2675= Fax 8136261641
 Rpr 01 99 03-45p Gene D e d i c k 1-920-490-9893
P- 6

CST RECOVERY FROM BATCH DIGESTERS AND BLOW HEAT SYSTEM

Hilton Tyre
Director, Mill Technical Services
Glidco, Inc.
Jacksonville, Florida

ABSTRACT

The total concept of turpentine recovery. when stripped of the "mystics', can produce
both operating and monetary gains, as well as elimination of environmental and
potential safety hazards-
-
INTRODUCTION

--
Turpentine availability originates at the time the tree is cut and terminates when the rail
car or tank truck is closed for shipment. Our emphases is to maximize recovery which
will:
Contribute to the mill's operating income by sale of CST
Eliminate potential safety hazards
Eliminate potential environmental non-compliance
Reduce the mill's operating expenses for effluent treatment
In general, wood chips are fed to the digester and cooking liquor and black liquor is
added in sufficient quantity to cover the chips. Various methods are used to assure
uniform dense packing of the wood chips in the digester. After the chips and liquors
are added, the digester is closed, and the digester cook is started. This is
- accomplished by steaming the digester directly or indirectly. Direct steaming is done by
injecting steam directly into the digester; indirect steaming is done by circulating liquor
through external steam heat exchangers.
-
Three periods can be examined in a digester cook or cycle as they relate to turpentine
recovery. The first is the exhausting of the digester where a large percentage of "air" is
removed. Second is the heating up to cooking pressure and temperature, and the third
- period is the cooking period. The cooking period is determined by the mill's pulp needs,
and in all cases turpentine production plays a minor or non-existing role! In most
cases, periods one and two are fairly constant, and it is during these two periods that
-- the bulk of the turpentine is made available in vapor form.
Apr 0 1 99 0 3 : 4 6 p Gene Dedick 1-920-490-9893
P-7

A simplified turpentine recovery flow sheet would be as follows:

The digester gases (turpentine, steam, and noncondensable gases) are vented directly
to a separator system where any liquor or fiber carry-over is removed. After cleaning,
the gas vapors are transferred to the condenser(s), and the resulting condensate
(turpentine and water) goes to the decanter. The noncondensable gases from the
condenser are sent to a gas-cooler and then to a collection system for proper disposal.
The decanter will separate the turpentine from the water, with the turpentine overflow
going to storage and the water underflow going to process treatment or sewage.

Page -2-
 Apr 0 1 99 0 3 - 4 6 p Gene Dedick 1-920-490-9893 P-8

<-.

--
Typical loss in the system would be similar or propoftional to the following simplified
material balance:

PROCESS STEPS AND EQUIPMENT FUNCTlON

WOOD STORAGE
The wood or chip furnish is an area that we have little control over; there is not a lot to
discuss other than to emphasize that the fresher the chips the higher the turpentine
availability, therefore, higher turpentine production.
Several studies have been made to determine the causes of turpentine losses and the
.- effect of storage (over time) has on the availability of turpentine in the chipsz. The
causes of the turpentine losses are beyond the scope of this paper, but as you can see,

Page -3-
Rpr 0 1 99 0 3 : 4 6 p Gene Dedick 1-920-490-9893
P- 9

from the data compiled by these studies, the loss of turpentine was relatively small
during the first two (2) weeks. However, these studies showed a significant increase in
turpentine losses during the next six (6) weeks. This information would indicate a FIFO
system (First In First Out) would provide the best opportunity for higher recovery if your
chip pile can be rotated within a two to four week period. If the mill's rotation is longer,
then you may want to consider a LIFO system (Last In First Out). This will insure wood
furnish as fresh as possible during normal operations, but will mean poor recovery
when cleaning out the wood pile.
Another concern in wood storage is fines and sand in the chip pile. These foreign items
can cause problems in controlling the digester pressure, as well .as cause serious
damage to the recovery equipment. Many mills have experienced erosion problems
due to grit in the wood supply.

DIGESTERS
Minor losses in turpentine can be expected during chip loading if excessive steam
packing is done. It is possible to steam distill the turpentine on the suriace of the chips
and lose this material through the open digester head. The addition of liquor
simultaneously with the chips and the reduction of excessive steaming will help
eliminate those losses, but remember that over charging of a digester with liquor can
reduce pulp quality, reduce turpentine recovery, cause carry-over problems and add to
the operating expenses of the mill. This includes excess water which may be contained
with the chips due to rain or snow.

Page -4-
 Rpr 01 99 03:47p Gene D e d i c k 1-920-490-9893 p . 10

- The digester vent relief opening is normally equipped with a screen to prevent fiber
-- carry-over during the digester vent relief cycle. This screen should be checked after
each digester cook when the digester is opened for charging- Damage to this screen
-

- can cause problems 'down stream" in the recovery process, such as condenser foujing.

DIGESTER RELIEF PROFILE

Since little can be done once the chips are in the digester, a logical starting point in
discussion of the equipment would be the digester relief "profile" and vent relief
-. equipment. The "profileuof the digester vent relief should be programmed to:
Maintain pulp quality
Be compatible with mill's standard pulping practices
Minimize consumption of mill's prime steam usage
Optimize turpentine recovery
Quite often the digester 'profilem can be improved to assist in greater turpentine
production without penalty to pulp quality or production. Studies have shown that a
correlation does exist between high-quality pulp and turpentine recovery efficiency3. If
you improve one, you imprdve the other!
Proper digester vent relief is one of the most important factors in efficient turpentine
recovery. Air and other noncondensable gases must be vented to obtain the correct
pressure-temperature relationship and help improve circulation in the digester. Also,
the removal of air improves the quality of the pulp, since oxygen has an adverse effect
on the cellulose material in the presence of hot alkali". To obtain this proper vent relief,
various systems are being used by several mills, some with excellent results. The
simplest configuration is a dual orifice plate arrangement, however there are some
\

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 Rpr 01 99 03: 4 7 p Gene Dedick 1-920-490-9893 p. 1 1

-
--
inherent problems with this configuration such as orifice plate wear and excessive -
prime steam consumption. Today's standard is computer assisted automatic relief.
- This relief method provides the most consistent, repetitive and reliable results.

This is a simplified equipment diagram for the discussion of the relief profile. It is
important that all vent relief lines and headers up to and including the separator be
insulated (not shown). This will help prevent the vapors from cooling to a point where
turpentine will condense and be lost in the separator seal. This insulation will also help
protect operating personnel working in the area. The digester vessel is equipped with a
- temperature indicator, pressure indicator, chip screens (not shown) located in the vent
line immediately upon exiting the digester vent, and normally a 3-inch relief line. Valve
2 is a heavy-duty, normally 1 or 11/2-inch high pressure control valve. The output
- signal that regulates valve 2 is supplied, from a pressure tap on the digester so that
valve 2 is being closed gradually and responsively to maintaining an ascending digester
pressure to an "at pressure' value as determined by the specific pulp being cooked-
Valves 1 and 4 are hand ball valves for manual blocking of the relief line and normally
- left open during the cook. Valve 3 is an automatic block valve set to open shortly after
the beginning of the cook when the digester reaches a preselected value generally 4-5
p.s.i.g. It is set also to shut off periodically during a cook, while at the same time
- automatic valve 5 fully opens, along with valve 2 so that blow back steam can enter the
relief line, valves 2 and valve 1, blowing away fibrous material and other debris from
those valves and off the chip screens at the digester outlet. Valve 3 is set to perform
-
the same automatic blow back operation should the pressure in the digester reach 6-8
pounds above that corresponding to the pressure of saturated steam at the digester
temperature. This is false pressure, and this setting is an override of the periodic blow
back, which is normally set for intervals of 10-15 minutes.
-
CS
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 flpr U1 99 0 3 : 4 7 p Gene Dedick 1-920-490-9893 p. 12

-
A relatively simple repetitive relief profile was developed several years ago5 that is -
,-- . adjustable to the vast majoriiy of cooking procedures being implemented today. This
-
program was developed prior to mandated odor containment, and could cause some
serious emission problems today. The characteristics of Control Valve 2 determine the
relief profile, along with the pulp quality. The profile should be similar to the following:

This profile, as mentioned earlier, is adjustable, but is a good place to start in

customizing your mill's particular needs.

YOUR DIGESTER RELIEF PROFILE

UKE YOUR TURPENTlNE RECOVERY SYSTEM
MUST BE DESIGNED AND CUSTOMIZED
FOR YOUR PARTlCULAR MILL !!!
F

There is equipment available that will allow a detailed evaluation of your mill's particular
profile. This equipment would be connected to one digester and it would condense the
entire digester relief. The condensed streams can be measured and analyzed, thereby
allowing for optimization. Also, liquor removed from the digester during the relief can
be measured, and if necessary, can be adjusted accordingly.

Some benefits from other studies around the country are as follows:
Reduced excessive liquor charging, at one mill, by 1,500 gallons per cook
Improved pulp quality through consistant kappa number, due to containment of
active alkali at the beginning of the cook
Reduced prime steam consumption, at one mill, by approximately 200 million
pounds per year
Reduced cooking cycle, by reaching cooking temperature sooner, as much as
16 percent
Increased turpentine recovery at every test by 15-35 percent.

Page -7-
npr ui YY U3:49p Gene Dedick

SEPARATOR

R is carry-over from the digester that demands the first equipment in the turpentine
recovery procedure. The relief gases are composed of a mixture of varying proportions
which include:
1) water vapor
2) black liquor
3) pulp and wood fiber
4) organic vapor
5) noncondensable gases
Removal of black liquor and pulp from the relief gases is paramount to effective
turpentine recovery. The result of inefficient separation is fouled condenser heat
transfer surface and emulsification in the decanter. Too familiar is the off-white
emulsified mass encountered at one time or another in the turpentine decanter, and
black liquor carry-over is usually the culprit. The apparent effect of black liquor in the
decanter is that of a surfactant in- lowering the surface tension at the inte~ace,
destroying the immiscible qualities of pure turpentine and water.

Page -8-
 flpr 0 1 99 03:49p Gene Dedick 1-920-490-9893
p . 14

-
The standard separator used in turpentine recovery has been a cyclone type separator -
.- with a number of individual configurations. The most predominate being large diameter
(five foot or larger), cone bottom, tangential inlet and vertical vapor outlet. This
- separator is best designed for solid particle removal, however it will not necessarily give
the best separation of liquid from gas. The difference in behavior of droplets compared
with solid particles must be taken into account.
Gas flow in a cyclone develops forces in three dimensions:

It is desirable to keep the droplets away from the core to attain efficiency and this can
be done by proportioning VT as large as possible with VR. The liquid droplets
--
centrifuged to the outer'walls will coalesce and flow downward to the drain where a very
turbulent core exists in the center. Liquid in the form of droplets may be sheared away
by this turbulence and carried upward by the vertical component VA.
- A better design, being a departure from the low velocity, large volume separator, has
been made available to the industry.

Page -9-
 Hpr 01 99 03:SOp Gene Dedick 1-920-490-9893
p . 15

t -. This design makes use of the dynamic use of pressure gradients in developing effective
centrifugal force during the vertical helical flow of gases through the separator. In this
case, the tangential inlet velocity VT is the predominate force but by utilizing a
tangential outlet and tapering the vertical shell, VT is further assisted while radial
velocity VR is essentially eliminated. Axial velocity VA is the vertical movement of the
-.
resulting upward spiral. Due to skin friction, the velocity gradient approaches zero
immediately adjacent to the wall. The deposition of the liquid droplets into a wall film
provides the transportation medium for disposal of solids- and liquids without
accumulation. The liquid film will drain by gravity to the horizontal slotted baffle, which
divides the separation capacity of the separator from the deceleration surge chamber.
The. deceleration surge chamber removes the tangential velocity from the liquid,
-
provides surge capacity for high liquid influxes and allows gravity draining from the
bottom of the lower chamber.
With any type of separator, a hydraulic seal leg is a necessary part of the underflow line
- from the separator to prevent the loss of vapors through this line. The seal leg head
pressure can be calculated to ensure its being greater than the pressure drop through
the condensers. A drain valve at the bottom of the seal leg will indicate if the seal is
functioning properly. Additionally, an ultra sonic level alarm should be located at a
calculated distance below the horizontal baffle to indicate high liquor levels in the
separator. Nonall , the sensor is located at about 75% of the capacity of the
- r,
deceleration surge c amber. The sensor should be easily calibrated, have sensitivity
settings and selectable time delays, which will help eliminate false indication- A high
level alarm would indicate possible restriction in the seal leg or excessive liquor carry
Q over.
-

-
Page 10-
 ~ p Ur 1 9 9 0 3 : 5 0 p Gene D e d i c k 1-920-490-9893 p. 16

-
To prevent plugging of the seal leg, a small quantity of black liquor flush is continuously -
-.. introduced to the bottom of the separator. Hot black liquor is used, instead of water,
because it will not condense the vapors. It has a higher specific gravity to help flush
-- solids from the system and "liquor'sslicker'. A maximum of five (5) gallons per minute
is adequate to provide liquid flush on the baffle plate and a wet wall condition on the
lower third of the separator shell. If there are multiple separators in parallel, then the
-- quantity of flush liquor to each would be the same as though each were an independent
unit.

-. To protect the separator from excessive pressure, in the event that both seal leg and
condensers become plugged, a rupture disk should be installed atop the separator.
Routing should be made away from the separator(s) via appropriate conduit, to insure
personnel safety in case of a rupture disk failure. Normally, a 15 p-s-i. rupture disk is
.- sufficient, thereby eliminating any need for code stamped vessels that are more
expensive.
-
CONDENSERS
Latent heat removal from vapors is the basic objective of any condenser. The'use of a
cold surface to remove heat is conventional for a condenser and may take the form of
tubes, curved surfaces, direct contact with cooling medium or any economical
configuration to promote transfer of the heat from the vapor to the cooling medium,
- usually water.

'--:
With proper separation, the vapors entering the condenser is comprised of
- condensable vapors (primarily water and turpentine) and noncondensable vapors
(primarily air, sulfides, mercaptans, and light organic compounds generated in the
cooking process). The effect of these gases on the heat load is negligible, but their '

effect on the condensation process is quite detrimental. Since these gases remain as a
gas at the temperatures experienced, the concentration proportionally increase with
condensing. Condensing becomes increasingly difficult the higher the concentration of
noncondensables. Therefore, noncondensable gases must be continually removed
from the condenser through the cook cycle. These gases are saturated with turpentine
and water, depending on the vent temperature and pressure. The higher the vent
temperature or the lower the pressure the more turpentine is carried with the vapors.
-
This graph is the results of calculations for turpentine losses in the vent due to
excessive temperature and NCG evacuation. The turpentine loss in the vent is
calculated from the equations:
--
w = vt q T '24f7m2
W = turpentine lose (gallons per day)
Vt = volume of rni~ed'~ases at the temperature measured (cubic feet per hour)
@ = density of mixed gases at the temperature measured ( pounds per cubic feet)
T = weight fraction of turpentine in mixed gases

Page -1 1-
Apr 0 1 99 03r50p Gene Dedick 1-920-490-9893
p - 17

'
Normally, noncondensable venting from the condenser has been one of the single
largest loss points in a turpentine system.
There are several condenser designs and configurations being used successfully today
on turpentine recovery systems. The most efficient and effective condensers, for a
state-of-the art turpentine recovery system, should include the following features:
Vapors shell side, water tube side
Horizontal mounting
Removable tube bundle with square pitch tube pattern
* Waterside tube surface access for scale removal without
removing tube bundle
Also, the design should include a cooling water recirculating system. This control
system should provide constant water discharge temperature, constant water velocity in
the tubes, minimum use of cold water, fast response to load change and optimum
efficiency of condenser tube surface under all vapor load conditions. In operation, the
intake of cold water matches the vapor load on the condenser so that such variables as
the seasonal change in cooling water temperature or geographical location does not
effect process design operational ranges.

Page - 12-
 Rpr 0 1 99 0 3 : S E p G e n e Dedick

NCG COOLER

The NCG Cooler is vital to efficient decantation in the decanter, and safe operation of
the NCG Evacuation System. If the turpentine condenser controls the condensate to
maintain the most efficient separation, then turpentine is "driven over" to the NCG
system. This is a serious safety hazard and a potential catastrophic failure. If the
turpentine condenser controls the condensate to insure no turpentine is 'driven over" to
the NCG Evacuation System, then the decanter temperature is too low. This will
increase turpentine loss due to increase solubility and decrease separation efficiency.
The cooler can be run too low. This will increase the sulfur contamination due to
condensing TRS compounds. The increase in sulfur decreases the desirability of the
turpentine te the fractionator, as well as decrease the flashpoint of the turpentine in
most cases. Studies are on going at this time, but it is believed the decrease in the
flashpoint is mainly due to increases in methyl mercaptans.
CRUDE SULFATE TURPENTINE
FLASH POINT VS SULFUR,PPM

SULFUR, PPM

DECANTER
The purpose of a decanter is to separate the condensate mixture from the condenser
into the lighter turpentine (7.2 pounds per gallon) and the heavier water (8.34 pounds
per gallonj. This is readily accomplished, using a tank designed for turpentine overflow
and water underflow with an interface level between the two liquid phases.
A horizontal tank is preferred to a vertical tank as longer horizontal travel is available to
both phases and a shorter vertical travel for the droplets of turpentine to rise and the
droplets of water to sink. Also, a horizontal tank allows the interface surfacearea to be

- Page -13-
 npr ul YY us:aiz!p Gene Dedick 1-920-490-9893 p. 19

-
-_ increased as well. An evaluation of the condensate entering the decanter should be -
made to properly determine adequate retention time.
- Quiescent liquid condition within the decanter are most important for adequate
separation. It is considered good practice to introduce the condensate at about the
interface level through a stilling well to reduce turbulence. The decanter should be
located as close as possible to the condenser so the condensate does not experience
mixing from travel in empty lines, thereby hindering separation.
- It has been conventional practice to reduce the condensate temperature to
approximately 1200 Fahrenheit. Development has shown that this practice increases
the solubility of turpentine in m r 7 . The solubility curve for turpentine and water is
inversely proportional to temperature. At 150-1600 Fahrenheit, solubility reaches a
-
minimum equilibrium value. Also, the tendency to emulsify the turpentine in water is
reduced and the greatest. spread in the densities of the water and turpentine occur in
this temperature range to further assist in clean decanter operation. It should be noted,
at this temperature, the decanter must be vented back to the system prior to the
NCG coolerto condense the turpentine vapors emitted at this temperature.

- . A continuous decanter is an automatic means of separation using hydrostatic balancing

to maintain the interface at the desired location in the decanter. A proportion of 75%
water and 25% turpentine is satisfactory when measured on the vertical centerline axis
of the decanter. This allows enough turpentine volume to prevent water displacement
-
to the storage system in times of minor pressurization due to system upsets, as well as
adequate surface area at the interface of the two (2) mediums. The height of the water
in the hydrostatic leg fixes the position of the interface.

Page - 14-
npr ui YY u3:azp Gene Dedick 1-920-490-9893
p . 20

The interface location can be made easy by setting of a triangular notch weir plate- -
This weir can also be used to determine the decanter underflow rate, as well as
collecting samples for analysis to determine decanter efficiency.

FOUL CONDENSATE STRIPPING

As environmental regulations tighten, foul condensate streams will require cleaning
before they can be reused. The cleaning can be achieved by steam stripping the
condensates. There exists a patented process that allows stripping of collected foul
condensate streams using waste energy from the digester vent reliefa. The process
collects foul streams high is residual TRS compounds and turpentine, such as:
Turpentine decanter underflow
Blow heat secondary and tertiary condensates
r Evaporator surface condenser condensate
NCG condensate drains and "knockout pots"
These combined foul condensates is routed to the stripper body which is driven by the
waste energy available in the digester vent relief from a batch system, flashed vapors
from a continuous digester system or from refiner vents in a TMP operation. The foul
stream is heated to 2120 Fahrenheit or above to sufficiently increase the vapor
pressure of turpentine, TRS and methanol to cause their release. Then these
compounds can be carried over to the turpentine recovery system for selective
recovery.
There are few controls required to operate this stripper. A level control loop is the only
instrumentation required, with sensitive pressure and temperature gauges used for
quick on-site monitoring. A foul condensate receiver tank with level control and transfer
pump is also required. The stripper also functions as a relief gas washer to remove
fiber and liquor carry over during separator upsets. The process is not affected by
fluctuations in pressure or temperature, and should be considered as a first effort when
cleaning up foul streams because of the recoverability of the turpentine. This system
can be adapted to any turpentine recovery system, or can be incorporated into the
design of a new system.

STORAGE

Usually, turpentine stora e is a function of transportation; does the mill ship by rail car
1
or tank truck? Tank truc delivery indicates readily available transportation so storage
can be small (10,000 gallons), but ifrailcars are used and turnaround delivery is slow
then extra capac'w is needed. Today, most 10,000 gallon capacity railcars are being
phased out of service and replaced with 20,000, 23,000 or 26,000 gallon capacity
railcars. Therefore, storage capacity for railcar delivery should be at least the largest
capacity railcar provided. Recommended capacity should be the largest capacity plus
5-10 production days.

Page -15-
 flpr 0 1 99 03:53p Gene Dedick 1-920-490-9893 p.21

-- .
--
-
/c
The storage tank should be a flooded design to prevent severe vapor space corrosion.
--

--

--(--,
.-

The tank would be equipped with a hydraulic water leg w'kh the elevation of the leg the
same as the invert of the tank. This insures the storage tank is full at all times.
Turpentine entering the storage tank will displace the water out the leg due to head
pressure in the fill line, and the interface elevation will drop as the tank fills. The
interface level can be observed by use of a sight glass, but a sight glass can be broken

Page - 16-
 Rpr 01 99 03:54p Gene Dedick 1-920-490-9893
p - 22

-
A broken sight glass, due to freezing conditions, has been a source of turpentine loss at
-- many mills. A better way to determine the turpentine volume is by a level transmitter4

A nozzle with an extension atop the storage tank will act as a standpipe similar to the
turpentine fill line. As the turpentine capacity increases in the tank a corresponding
- increase to the elevation of the turpentine in the fill line results. This elevation increase
is proportional to the interface elevation, which can be calibrated with the tank capacity.

-
TURPENTINE LOADING

-
Whenever possible, both rail car and tank truck loading facilities should be available.
This gives the mill an alternative transportation outlet in case of transportation problems
(strikes, rail car delays).

- Page -17- .. .
flpr 0 1 99 0 3 : 5 4 p Gene Dedick

-0 load a transportation vessel,

the storage tank water leg is closed and padding water is introduced to the storage
tank. A check valve in line, between the decanter and storage tank, will prevent back
flow to the decanter, which collects the small turpentine production during the loading
process. The water displaces the turpentine out the turpentine outlet through the fill
pipe to the transportation vessel.
Since turpentine is classified by OSHA as a Class IC liquid, certain safety
considerations must be addressed. The tank should be remotely located and diked to
contain any spills or leaks. This should included prevention of soil c~ntamination."NO
SMOKINGu and "NO FLAMES OR SPARKS' signs should be conspicuously posted!
Also, static charge ignition control is required whenever turpentine is transferred from
the storage facilities to the transportation vessel.

The 1990 ANSIRVFPA Standard for Flammable and Combustible Liquids Code and the
National Fire Code has specific requirements for static ignition control. The stored
energy (ignition energy), released by spark, is related to the capacitance (C) and the
voltage (V) in accordance with the equation:
C * V2
Energy = r)

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 flpr 01 9 9 03:55p Gene Dedick 1-920-490-9893 p. 24

--- The ability of a spark to produce ignition is governed largely by its energy, and will
normally be some percentage of the total stored energy. Tests have shown that
-
-
discharges of 0.25 millijoules are sufficient for spark ignition in saturated hydrocarbon
gases and vapors. Information is available which indicates that sparks arising from
potential differences of less than 1500 volts are not likely to be hazardous in saturated
hydrocarbons. However, tests reveal that the human body in a dry cool atmosphere
accumulates a static charge resufting in voltage as high as several thousand volts.

- Since static is generated when turpentine and any dissimilar material are in relative
motion with each other, steps must be taken to prevent or control static ignition. There
are three (3) methods to control static ignition hazards:
-
1) Remove the ignitable mixture from the area where the
static may be discharged
2) Controt the amount or speed of the flow
3) Dissipate the charge after it has been generated
i

The first method would require loading from the bottom of the car, or providing a down
spout that extends near the bottom of the tank. The second method requires slowing
the fill rate. If the material flows at a low enough rate, a hazardous level of static
charge will not be generated. The acceptance of this method depends on operation
conditions at your mill. The third method is to relax or dissipate any static charge,
which has been generated, by bonding and grounding.
The bond connection should be made BEFORE the dome lid is opened, and SHOULD
NOT BE REMOVED until the dome lid is closed. The bond should be a metallic wire
permanently connected to the fill stem, and the free end should be provided with a
clamp for convenient attachment to some clean NON-PAINTED metallic part of the
cargo tank. The minimum size of the bonding wire should be determined by the
mechanical strength rather than by the current-carrying capacity. The bonding wire
may be insulated or uninsulated. Most prefer uninsulated so defects can be easily
spotted by visual inspection.
Another reason to eliminate free falling turpentine while loading is to prevent the
release of H2S which is dissolved in the turpentine. The free falling cascade will air strip
the turpentine similarly to removing H2S in drinking water. This could present a safety
concern to the operator loading the turpentine.
Remember, when loading turpentinef0:
.The fill pipe used to load the transportation vessel must extend to the bottom of
the tank to prevent static charge build-up and prevent air stripping ofHzS.
.If a hose is used, it must be an approved conductor.
*The filling pipe, transportation vessel and all parts of the loading station must
be electrically bonded and grounded.

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 flpr 0 1 9 9 03:55p Gene Dedick 1-920-490-9893 p - 25

- TROUBLESHOOTING A PARTIAL CONDENSATION RECOVERY SYSTEM - 01 $

,-.

w
%
it-
1%

SEPARATOR

The vapor header to the separator should be level or preferably pitched slightly toward
the separator. Under no circumstances should risers be contemplated in the relief line
before the separator. Insure the insulation is intact around the header to the separator
and the upper section of the separator to maintain superheated state of the vapors.
Insulating of the header after the separator is not required since heat loss is of no
consequence at this point before the condense. The length of the header pipeline is
not critical as long as no risers are present to provide a liquid trap. Here again,
horizontal or slightly downward pitch is desirable.
Insure the separator drain is clear and free of obstruction, by checking the seal leg
drain valve located at the bottom of the loop. The drain, if it is restricted, can be
cleared by slowly injectin steam or air through the line. The black liquor drain from the
?
seal discharge should low by gravity to a non-pressure receiving vessel. This
effectively isolates any pressure fluctuations from the seal and prevents any hydraulic
or pressure changes from affecting the draining characteristics or separator efficiency.

Page -20-
 Apr 01 99 03:56p Gene D e d i c k 1-920-490-9893 p. 26

SYSTEMTEMPERATUREANDPRESSURE
..

-
Temperature T I will vary greatly depending on vapor loading and instrument tuning. If
a wide cycling of temperature to either side of the set point is experienced, check
-
alignment of instrument in accordance with manufacturers instructions by a competent
instrument technician and insure control valves are not oversized. Over condensing is
the norm in partial condensation systems. Due to the cycling inherent with batch
systems, the condensate temperature will drop below the minimum temperature,
- thereby condensing turpentine. The fallowing temperature curve is indicative of a
('
t.- J primary condensate at or near atmospheric pressure:

Page -21-
 Rpr 01 99 03:58p Gene Dedick

A sample tap, as well as a means to measure the flow in this line, is needed to
determine potential losses. -

Temperature T2 will normally vary within range depending on the vapor load to the
condenser.
Temperature readings below range would indicate one or more of the following:
Little or no vapor load on the condenser
Water leak from cooling water to vapor side of condenser
Plugged condenser baffle drains in the condenser
Controller out of service
Temperature readings above range would indicate one or more of the following:
Vapor load exceeding capacity
Recirculation pump has failed
High cooling water input temperature
If the decanter is located remotely from the condenser, a sample tap would be
recommended but is not mandatory.
Temperature T3 is dependent on the condensate temperature T2. Some heat loss will
be encountered to the air surrounding the decanter. Underflow temperature T3 is the
coolest water coming from the bottom of the decanter. Low temperature, with T2
normal, would indicate very little load on the unit and further evidenced by a low flow
rate over the weir plate. Ifa direct contact NCG cooler is used, too high a flow rate of
water to the cooler will reduce this temperature below normal- A sample tap is needed
at this location, as well as a means to measure the flow. If the system has a weir and
the cover is removable, then a sample can be obtained as the condensate overflows
the weir.
Temperature T4 measures the exit gas temperature from the NCG cooler. Normally
this temperature will cycle somewhat as the batch digester cycles. Under surge
conditions this temperature may slowly climb but should return to normal. Excessive
temperature and/or excessive NCG evacuation which results in low pressure will result
in:
Turpentine loss
Equipment and process upsets
Can be a potential safety concern
Can be a potential environmental problem
Temperature readings consistently above range would indicate one or more of the
following:
Insufficient cooling water to the cooler-
- Excessive vapor temperature from the secondary condenser.

-- A sample tap and means to measure the flow of the cooler condensate is helpful, but
not mandatory.

Page -22-
 Apr 01 99 03:58p G e n e Dedick 1-920-490-9893 p - 28

.-

SAMPLE COLLECTION AND ANALYSIS -

.--,
samples should not be taken at laminar flow points.
- Sample should be taken through taps with vertical pipe nipples to allow for
full, clean samples.
If your sample overflows, dump the sample and collect another.
.-
Use wide mouth POLY liter bottles that can be sealed.
All hot samples should be cooled prior to collection. A cooling coil is
normally adequate.
- The distillable turpentine available in a liquid sample may be determined by refluxing
the turpentine contaminated sample and collecting the turpentine in a trap.

Determine the liquid sample 'tear', and place the sample in a three (3) liter flask. Bring
the sample temperature up slowly to boiling. If you are analyzing a black liquor sample,
- add a few drops of 'defoamef and slowly bring the sample to boiling. Reflux until the
turpentine volume in the trap remains constant. Cool and measure the turpentine.
The distillable turpentine calculation is as follows:ll
rnl turpentine * 0.863 * 100
Percent distillable turpentine' =
-. grams of sample
The turpentine loss is calculated as follows:12
Q-
i.:
Turpentine loss = Percent distillable turpentine * Stream flow rate
-

- Page -23-
 Apr 0 1 99 0 3 1 5 8 ~ Gene Dedick 1-920-490-9893

A state-of-the-artturpentine recovery system would have the following:

TAPER NECK SEPARATOR Remove intrained fiber and liquor from the
-. digester relief
FOUL CONDENSATE STRIPPER Remove residual turpentine and TRS
-.
contaminates from foul condensate streams using waste energy,
rendering the stream useful for reuse in the mill. The stripper would
eliminate the primary condenser
- TURPENTINE CONDENSER Cool and condense water vapor and
turpentine for decantation
- TURPENTINE CONDENSER TEMPERING LOOP Provides consistent
temperature control of condensate for optimum decanter operation
NCG COOLER Controls NCG stream to remove water vapor and
-- turpentine while allowing TRS compounds to enter the NCG disposal
system

--
NCG EVACUATION PRESSURE REGULATOR Prevent excessively low
pressures, from the NCG disposal system, in the turpentine condenser
and the NCG cooler

- Page -24-
 flpr 0 1 99 03:59p Gene Dedick

-
BLOW HEAT RECOVERY
Due to the increasing cost of energy, heat recovery from batch digesters has been
-- practiced for several decades. Today, additional emphasis has been placed on heat
recovery efficiency and to fully contain the miscellaneous foul smelling compounds
released with the digester blow. It is this additional emphasis which we want to address
- in this short course, specifically turpentine collection for the blow heat recovery
systems.

--
In the early forties when energy was inexpensive, blow heat recovery systems were
designed to a heat recovery efficiency of 70-75%. A typical arrangement of a blow heat
recovery system provided only a primary condenser. Time progressed and the
recovery system added a secondary condenser, and eventually evolved to incorporate
-- independent cooling water for the two condensers. Some major deficiencies with this
system were:
Slow reaction to upsets
Over condensing
a Bad stratification in the accumulator
No containment of noncondensed gases
Still, the main purpose was to recover heat; containment of the malodorous gases not
condensed (NCG gases) was not considered. These noncondensed digester gases
were released to the atmosphere.
-i L
'

As federal regulations regarding sulfur emissions tightened, in the late 60's and early
70's, additional design considerations were required for blow heat recovery. Those
considerations, included not only improving heat recovery to 85-90%, but containment
of the malodorous digester gases as well. A tertiary condenser and a non-condensable
--
gas evacuation system was added to the recovery system, thereby, containing a
significant portion- of the NCG gases that had previously been discharged to the
atmosphere. However, the tertiary condensate was combined with the secondary
condensate, and these foul streams (high in organic compounds) are commonly routed
- to the hot water accumulator. Even though the gases had been contained in the
recovery system, the malodorous sulfur compounds would be released when the mill
uses the foul water from the top of the accumulator. For example, when the foul water
- from the accumulator is used for stock washing, these 'light' malodorous sulfur
compounds will be released with the washer hood exhaust gases, which are rarely
contained.
-
Then in the 80's a new blow heat design was incorporated capable of heat recovery of
95-98%. Also, the inadequacy in containing the malodorous compounds was improved
by routing the secondary and tertiary condensates away from the hot water
..... accumulator to the turpentine recovery

Page -25-
 flpr 0 1 99 03: 59p Gene Dedick 1-920-490-9893 p-31

(-- The volume of organic compounds routed to the turpentine recovery system is directly
related to the efficiency of the digester relief. Observations at several mill locations
- reveal a range of 10-40% of the turpentine "available to the system for recovery" is
released during the digester blow. The average is approximately 25% of the availability
from the chips.
-.
The efficiency of recovering turpentine from the blow heat system is around 60-65% at
best. The losses are due to the cyclic nature of the batch digester and from the NCG
temperature. It is much easier and more efficient to recover the turpentine from the
digester relief, however if you recover from the blow heat this turpentine volume can
provide additional revenue to the mill, eliminate expenses in treating the foul
condensates, eliminate potential safety hazards, and correct a potential environmental
deficiency.

Page -26-
0 1 99 0 3 : 5 9 p Gene D e d i c k 1-920-490-9893 p. 3 2

PROCESS DESCRIPTION -

A state-of-the-art blow heat recovery system, as far as turpentine collection, would

have the following key items:
CYCLONE SEPARATOR Remove intrained fiber and/or liquor from the
vapor stream
PRIMARY CONDENSER Extracts the bulk of energy released during
digester blow
HOT WATER ACCUMULATOR TANK Stores the extracted energy in
the form of hot water
SECONDARY CONDENSER Super cooling of water vapors, baring
TRS and VOC.
SECONDARY CONDENSER TEMPERING LOOP Condenser 'turndown'
and temperature control of condensate for optimum decanter operation.
TERTIARY CONDENSER Super cooling NCG stream to remove water
and turpentine vapor before entering the disposal system
NON-CONDENSABLE GAS PRESSURE REGULATOR Prevent excess
pressures, from the disposal system, in the secondary and tertiary
condensers

Page -27-
flpr 01 99 04:OOp Gene Dedick

The digester steam, released when the digester is blown to the blow tanks at the end of
a cook, is vented from the blow tanks to the cyclone separator. The cyclone separator
would provide the same service as the separator in the turpentine recovery system.
The steam enters the cyclone separator toward the bottom of the vessel then expands
in a large distributing dome so that the velocity of the steam is greatly reduced. This
low velocity steam minimizes pulp and liquor carry-over to the primary condenser. The
"cleaned steam' enters the primary condenser where it is partially condensed by direct
contact with water pumped from the bottom of the accumulator. The temperature of the
primary condensate in most cases is a function of the mills demand fof hot water.
However, the temperature should be +I-2080 Fahrenheit to insure that the organic
compounds are 'driven over" to the secondary condenser. Approximately 75-85% of
the vapor load would be expected to condense. Steam not condensed in the primary
condenser, along with the NCG gases, are purged from the accumulator to the
secondary condenser.
The secondary condenser, in series with the primary, should be provided with an
automatic tempering water loop with a typical temperature controller. This tempering
loop provides constant water discharge temperature, constant water velocity in the
tubes, minimum use of cooling water, and allows for a large condenser "turn downn
while maintaining a proper temperature profile. The secondary condensate should be
controlled so the temperature of the condensate, upon entering the turpentine
decanter, does not impact the decanter's optimum operation temperature.
Development has shown that subcooled condensate temperatures has hindered
decanter operations due to solubility and tendency to emulsify the turpentine in water
especially when transfers are made via pumps or long piping systems. To insure
optimum efficiency, the decanter temperature. as addressed earlier, should be
maintained around 1500 Fahrenheit. Any gases not condensed in the secondary
condenser are relieved to the tertiary condenser.
The tertiary condenser, in most cases, is strictly a non-condensable gas cooler.
Excessive moisture and any remaining organic compounds are condensed prior to the
non-condensable gas collection system. The tertiary exit gases should be controlled at
a temperature of 90-1000 Fahrenheit. This insures most of the turpentine has been
removed from the NCG gas stream, and the majority of the light sulfur compound are
directed to incineration via the NCG Evacuation Sysferh.
The NCG Collection System is designed with several features to prevent ignition and
flame propagation since these gases are flammable. One feature is to evacuate the
gases sufficiently to maintain the velocity of the NCG gases above flame propagation
(flashback). This evacuation will normally impose excessive negative pressure in the
secondary and' tertiary condenser. A pressure control valve, located just past the
tertiary condenser is needed to prevent excessive evacuation in the condensers.
Generally, a pressure of 0-5' of negative water column is sufficient for evacuation of the
noncondensable gases. This pressure will not cause any "flashing," and after the gases
have passed the pressure control valve, they can be transported at any pressure or
velocity necessary. However, each system should be evaluated singularly.

Page -28-
 flpr 0 1 99 0 4 - 0 0 p G e n e Dedick 1-920-490-9893

Drew, J., Russell, J., Bajak, H. W., Sulkte Turpentine Recovery,

Pulp Chemical Association, Atlanta, 1971.
Thornburg, W. L., TAPPl 46, No. 8, 453 (1963), Stone, J. N., The
Glidden Company, Internal Report, 1968.
Miller, F. A, Pulp and Paper 42, No. 35 (1968), Chemical
Engineering Progress 64, No. 12 (December 1968).
Sawyer, F. G., Holtzer, W. F., ~ c ~ l o t h o L.
n ,A, 'Modern Chemical
Progress,' Reinhold. New York, 1952.
Marks, R. E., Reynolds, E. W., The 'Glidden Company, Internal
Report, (June 1974).
Drew, J., Russell. J., Bajak, H. W., Sulfate Turpentine Recovery,
Pulp Chemical Association, Atlanta, 1971.
Drew, J., 'Solubility of Turpentine in Water Vs. Temperature,'
Chemical Recovery Meeting, Pulp Chemical Association, Ponte
Vedra, Florida, (September 1967).
Reynolds, E. W., US. Patent 4,915,784. (April 1990).
Reynolds, E. W., Glidco Organics, Internal Communication,
(January 1989).
Propst, M. E., 'Safety in Turpentine Recove ,"Chemical Recovery
Meeting, Williamsburg, Virginia, (March 19927.
Drew, J., Russell, J., Bajak, H. W., Sulfate Turpentine Recovery,
Pulp Chemical Association, Atlanta, 1971.
Drew, J., Russell, J., Bajak, H. W., Sulfate Turpentine Recovery,
Pulp Chemical Association, Atlanta, 1971.
Fleet, S. V., 'Digester Optimization and Control," Pulp and Paper
Manufacture, 1989.

- Page -30-