Modification of Uhde forced

circulation AN solution plant to

achieve higher AN solution
concentration
Presentation to the ANPSG meeting
in Park City, Utah, USA
September 2007
by Leif Kjærgaard Rasmussen
assisted by Axel Erben, Uhde
 Page 2

Background
• The background for this presentation goes back to a year
long personal cooperation with MCFI, a small fertiliser
producer on the island of Mauritius
• MCFI made AN based N, NP, NK and NPK fertilisers for
the domestic market with some export to Africa.
• The MCFI granulation process was based on the
spherodizer granulation technology working with a slurry
containing all plant nutrients
• The fertiliser production in MCFI is stopped since 2005 for
economical reasons and replaced by bulk blending
The plants ( HNO3 and AN solution ) are now for sale.
 Page 3

The MCFI Plant Set-up

Liq. NH3 NH3

import Storage
NPK
Plant
HNO3
Plant

AN ( 90%) N, NK, NP or NPK fertilisers

56% HNO3 Solution
Storage Plant

MOP import

DAP import
 Page 4

The MCFI Problem (1)

• In high N grades like 20-10-10 or CAN 27, grades with a
rather low acceptable inlet drying air temperature due to
the risk of melting, the production capacity was limited
due to the low ( 90% ) AN solution concentration
• What were the possibilities for obtaining a higher AN
solution concentration ?
• An increase in HNO3 concentration, which would directly
lead to a higher AN solution concentration, was not
possible
• HNO3 was already preheated to 66ºC and NH3 gas to
60ºC in the AN solution plant; further heating would lead
to severe corrosion problems
 Page 5

The MCFI Problem (2)

• Possible solutions:
A) New AN solution concentration unit
B) New concept: modification of the existing AN
neutralisation, developed in discussions with MCFI
• Before we discuss this, just a few words about the MCFI
AN solution plant being an Uhde forced circulation plant
 Page 6

Flowsheet for the Uhde Forced

Circulation AN Vacuum Neutralisation
10
Steam
1 Neutraliser
duplicate 2 Vapour Separator & Scrubber
CW 9 pH control 3 Circulation Pump
2-3 in 10% 4 NH3 Heater
2oo3 temp. 5 HNO3 Heater
control 2 6 Neutraliser Tank
7 AN Solution Tank
8 AN Solution Pump
9 Condenser
10 Steam Ejector
4 11 Process Condensate Tank
NH3 gas
12 Process Condensate Pump

NH3 (duplicate)
pH control
5-6 in 10%
HNO3 5 1
6 AN solution

Process
condensate
3

12 8
7
11 © Uhde GmbH
 Page 7

Pro’s and Con’s

for the Uhde Process
Pro’s:
- 100% NH3 reaction efficiency due to the acid surplus
- Total N efficiency > 99,9% depending scrubbing method
- Low risk for strongly acidic spots due to the forced
circulation
- Temp. well controlled all over the neutralisation loop
- Well proven technology

Con’s :
- Acidic operation (pH = 2-3 in 10% solution)
- Max. operational temp. 160 ºC after the reactor due to the
low pH (standard Uhde design: 140-145 °C)
 Page 8

Natural Limitations on the

Achievable Concentration
• With a selected circulation rate, the maximum outlet temp.
from the vapour separator = the maximum inlet temp. to
the reactor is determined by the equation :
m 3/
hr x kg/m3 x kJ/kg K x ( 160 ºC – Tmax. reactor in) = Hreaction [kJ/hr]

• The reactor outlet temp. can be adjusted by the flash

evaporation rate in the vapour separator, i.e. with the
vapour pressure (MCFI: 0.45 bar abs)
• Here the maximum accepted outlet temp. from the separa-
tor must be minimum 10 ºC above the crystallisation temp.
of the AN solution to avoid any risk of crystallisation in the
loop
 Page 9

New Idea for an Increase in the

AN Concentration
• Based on experiences from a forced circulation concentra-
tion unit for phosphoric acid, following question came up:

Could we not install a heating element in the loop to supply

extra energy to obtain a more concentrated AN solution from
the plant ?

• Simple calculations were made for the MCFI case, which

were later confirmed by Uhde
 Page 10

Flowsheet for the Modified

AN Vacuum Neutralisation
10
Steam
1 Neutraliser
duplicate 2 Vapour Separator & Scrubber
CW 9 pH control 3 Circulation Pump
2-3 in 10% 4 NH3 Heater
2oo3 temp. 5 HNO3 Heater
control 2 6 Neutraliser Tank
7 AN Solution Tank
Steam 8 AN Solution Pump
9 Condenser
Cond. 10 Steam Ejector
Alternative A
4 11 Process Condensate Tank
NH3 gas
12 Process Condensate Pump

NH3 (duplicate)
pH control
5-6 in 10%
HNO3 5 1
6 AN solution

Process
condensate Steam

Cond.
12 8
7
11 Alternative B
3 © Uhde GmbH
 Results Case 1
Page 11

with Constant Circulation Rate

and the Heater after the Reactor
Plant parameters Existing plant Modified plant 1
Plant capacity ( mtpd 100% AN ) 225,0 225,0
Circulation rate ( t AN solution / hr ) 198,0 198,0
Circulation rate ( m3/hr ) 141,0 139,0
Boiling temp. in the vapour separator ( °C ) 115,5 131,3
Vacuum in the vapour separator ( bar abs.) 0,45 0,45
Reactor inlet temperature (= min. loop temp.) ( °C ) 115,5 131,3
Temp. increase over the reactor ( °C ) 24,5 25,0
Reactor outlet temperature ( ºC ) 140,0 156,3
Temp. increase over the new AN heater ( ºC ) n.a. 3,7
Heater outlet temperature ( °C ) 140,0 160,0
Maximum vapour pressure bar abs 1,04 1,31
Crystallisation temp. of the final AN solution ( °C ) 93,6 115,0
Required heat input ( kW ) n.a. 390
AN solution concentration ( % AN ) 90,0 94,1
 Page 12

Comments to Case 1 (1)

• One design criteria is that boiling must be avoided in
front of the orifice at the inlet to the vapour separator.
To avoid boiling the vapour pressure of the solution must
stay below 1.4 bar abs. (which was the original pressure
before the orifice)
In our case the solution vapour pressure is 1.31 bar abs,
not considering the additional pressure drop over the
heater (approx 0.1 bar abs ).
• To safely avoid the boiling we need to increase the
solution pressure by reducing the orifice diameter at the
inlet of the vapour separator, which results in the
replacement of the pump impeller or of the whole pump
 Page 13

Comments to Case 1 (2)

• Other considerations to keep in mind :
- We are now circulating and heating an acidic AN
solution with a concentration of 94.1%, which is more
risky with respect to decomposition and crystallisation
- The increase in loop temperature might influence the
material choice in part of the loop
 Page 14

Impact of Changed Circulation Rate

• The question came up whether a change in circulation
rate could further open up for an even higher heat input to
the loop resulting in an even more concentrated AN
solution (e.g. 95 %wt.)
• Uhde was involved in the theoretical considerations and
the outcome of the considerations are presented in the
next slide
 Results Case 2
Page 15

with Modified Circulation Rate and

the Heater after the Reactor
Plant parameters Existing plant Modified plant 2
Plant capacity ( mtpd 100% AN ) 225,0 225,0
Circulation rate ( t AN solution / hr ) 198,0 256,5
Circulation rate ( m3/hr ) 141,0 180,0
Boiling temp. in the vapour separator ( °C ) 115,5 137,8
Vacuum in the vapour separator ( bar abs.) 0,45 0,45
Reactor inlet temperature (= min. loop temp.) ( °C ) 115,5 137,8
Temp. increase over the reactor ( °C ) 24,5 18,6
Reactor outlet temperature ( ºC ) 140,0 156,4
Temp. increase over the new AN heater ( ºC ) n.a. 3,6
Heater outlet temperature ( °C ) 140,0 160,0
Maximum vapour pressure bar abs 1,04 1,12
Crystallisation temp. of the final AN solution ( °C ) 93,6 120,6
Required heat input ( kW ) n.a. 494
AN solution concentration ( % AN ) 90,0 95,0
 Page 16

Comments to Case 2 (1)

• The is no risk for boiling in this case due to the higher
AN concentration, but we need to replace the loop pump
• Other things to keep in mind :
- We are now circulating and heating an acidic AN
solution with a concentration of 95,0%, which is more
risky with respect to decomposition and crystallisation
- The increase in loop temperature might influence the
material choice in part of the loop
 Page 17

Comments to Case 2 (2)

• Comparing case 1 ( unchanged circulation rate ) with
case 2 ( increased circ. rate ) it is rather obvious that
case 2 is more attractive:
- in case 1 we need to change (or modify) the pump
anyway
- in case 2 we gain additional 0.9% on the AN
concentration
- the concerns are virtually the same in the 2 cases
 Page 18

How to Introduce the Energy

into the Loop ?
• The heat supply can basically be added to the loop
either in front of or after the reactor
• There might be good reasons to add it in front of the
reactor.
• To avoid overheating ( > 160 °C ) during stops of the
circulation the steam pressure for the steam heat
exchanger must be selected with great care not to
exceed the max. loop temp. of 160 ºC. This is less
problematic if the heat exchanger is put in front of the
reactor (where temp. is 25 °C lower) while maintaining a
sufficient DTln over the heater
• Electric heating should for the same reason be avoided
 Page 19

Energy Supply to the Loop

• Keeping the previous slide in mind we can limit the
steam temperature to 160 ºC ( or 6,3 bar abs.), which will
prevent any heating of the loop above 160 ºC
• The steam shall be saturated
 Page 20

Safety considerations
• The new steam heat exchanger requires as a minimum
the following additional plant instrumentation or inter-
lockings :
- the steam supply shall be tripped in case of failing
desuperheating ( temp. > 160º)
- in case of a plant trip the steam supply to the heater
shall be stopped by interlock
- conductivity measurement on the condensate from the
heat exchanger to avoid any contamination of the steam
system with AN
 Page 21

Required investment
• At the moment there are no economical data available to
judge whether the proposed modification is attractive
compared to an equivalent concentration unit
• A comparable evaporation unit would require additional
investment for:
- (falling film) evaporator and vapour separator
- vapour condensor and vacuum equipment
- AN condensate system
- additional AN monitoring devices (temp., pH)
- AN melt tank with heating coils and AN melt pumps
- Separate instrumentation
 Page 22

A First Reference Plant ?

• The idea presented in this paper is basically free for
anybody who might like to implement it
• The speaker nor his previous employer accept any
liability related to the implementation of the idea
• Uhde cannot accept any liabilities for the correctness of
the calculations and assumptions or any consequences
of their application
• Further case-to-case consultancy is necessary before
modification of any existing plant
• Are there any companies present here today who might
be interested in looking deeper into this idea ?
 Page 23

Conclusion
• A new idea, which allows for the production of a
more concentrated AN solution even at lower
HNO3 concentrations in a traditional Uhde forced
circulation vacuum neutralisation has been
presented
• The main concern related to the modified process
is a safety concern, which must be looked upon
carefully from case to case. However, this
concern can be handled.
• The economic feasibility is expected to be
positive when compared to conventional
alternatives. However, this can only be
evaluated for the individual case.
 Page 24

Acknowledgements
• Thanks to my earlier employer Kemira-GrowHow and to
MCFI for giving me the opportunity to present this paper
at ANNA 2007
• Thanks to Uhde, Germany, and especially Axel Erben for
giving me important support for the preparation of the
paper