VIII INTERNATIONAL FORUM ON INDUSTRIAL SAFETY VIII INTERNATIONAL FORUM ON INDUSTRIAL SAFETY Saint Petersburg 24 Saint Petersburg 24 – – 27 May 2010 27 May 2010 “ “ Safe Safe m m anagement anagement of an industrial process including of an industrial process including exothermic reactions and gaseous ammonia generation exothermic reactions and gaseous ammonia generation ” ” Giorgio Mari , Roberto Lauri Italian National institute for safety and health, Roma, Italy (www.ispesl.it) Carmela Metaponte Pharmacy Faculty, University of Rome “La Sapienza” Viro Romani Biosint, Via del Murillo, 16, Sermoneta, Italy Управление Управление безопасностью безопасностью производственного производственного процесса процесса , , включающего включающего экзотермические экзотермические реакции реакции и и выделение выделение паров паров аммиака аммиака Джорджио Джорджио Мари Мари , , инженер инженер Государственный Государственный институт институт Италии Италии по по вопросам вопросам безопасности безопасности труда труда ( ( Италия Италия ) )
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VIII INTERNATIONAL FORUM ON INDUSTRIAL SAFETYVIII INTERNATIONAL FORUM ON INDUSTRIAL SAFETYSaint Petersburg 24 Saint Petersburg 24 –– 27 May 201027 May 2010
““ SafeSafemmanagementanagementof an industrial process including of an industrial process including exothermic reactions and gaseous ammonia generationexothermic reactions and gaseous ammonia generation””
Giorgio Mari, Roberto Lauri Italian National institute for safety and health, Roma, Italy (www.ispesl.it)
Carmela MetapontePharmacy Faculty, University of Rome “La Sapienza”
Viro RomaniBiosint, Via del Murillo, 16, Sermoneta, Italy
PRODUCT PRODUCT ““CC”” IS CONVERTED TO AN HYDROCHLORIDE FORMIS CONVERTED TO AN HYDROCHLORIDE FORM
REACTION CALORIMETER USED FOR THE PROCESS STUDY REACTION CALORIMETER USED FOR THE PROCESS STUDY ((MettlerMettler Toledo RC1)Toledo RC1)
TRIALS PERFORMED USING 2 LITRESTRIALS PERFORMED USING 2 LITRESSIMULATION OF THE CONDENSERSIMULATION OF THE CONDENSERSIMULATION OF THE AMMONIA TREATMENTSIMULATION OF THE AMMONIA TREATMENTCONTINUOUS ADDITION OF REACTANTS IS CONTINUOUS ADDITION OF REACTANTS IS SIMULATED IN SMALL STEPSSIMULATED IN SMALL STEPSCATALYST (LiNHCATALYST (LiNH22) DESTRUCTION IS SIMULATED) DESTRUCTION IS SIMULATEDENERGY BALANCEENERGY BALANCE�� AGITATION IS CONSIDEREDAGITATION IS CONSIDERED�� ADDITION OF ADDITION OF ““COLDCOLD”” REACTANTS IS CONSIDERED REACTANTS IS CONSIDERED �� THERMAL DISPERSION OF THE CALORIMETER IS THERMAL DISPERSION OF THE CALORIMETER IS
CONSIDEREDCONSIDERED�� THERMAL LOSS DUE TO THE CONDENSATION IS NOT THERMAL LOSS DUE TO THE CONDENSATION IS NOT
AUTOMATICALLY CONSIDEREDAUTOMATICALLY CONSIDERED
CALORIMETRIC TRIALSCALORIMETRIC TRIALS
GRAPHIC OF THE CALORIMETRIC TRIALSGRAPHIC OF THE CALORIMETRIC TRIALS
Batch and jacket temperatures chart during reactants (“A” + “B”) addition
GRAPHIC OF THE CALORIMETRIC TRIALSGRAPHIC OF THE CALORIMETRIC TRIALSHeat generation chart during reactants (“A” + “B”) addition
Discovered Slightly Exothermic: 12 kJ/kg reagents
GRAPHIC OF THE CALORIMETRIC TRIALSGRAPHIC OF THE CALORIMETRIC TRIALSHeat generation chart during catalyst (LiNH2) excess destruction
Discovered Exothermic: 53 kJ/kg water
INDUSTRIAL BATCHINDUSTRIAL BATCH
MASS AND ENERGY BALANCES WERE CALCULATEDMASS AND ENERGY BALANCES WERE CALCULATED
REACTOR: 3500 LITRESREACTOR: 3500 LITRES
SEVERAL PROBLEMS OF PHASES (WATER SEVERAL PROBLEMS OF PHASES (WATER VSVS. SOLVENT) . SOLVENT)
Atm+50NH3 to treatmentDemi water150 litres@ 50 lt/h
Generation of LiOHand NH3
Catalyst (Lithium amide) excessdestruction
Atm+80NH3 to treatment (solvent
condensation)
1200 lt@ 300 lt/h
Alkylation ReactionReactants continuous addition in the reactor
Atm+4-25 kgCatalystCatalyst LiNH 2 load
Atm+4-400 ltDry solvent load
pressureT°C
VentMaterial movedNotesProcess step
REACTOR HEAD COOLING EXCHANGERS
POWDER ADDITION POWDER ADDITION SYSTEMSYSTEM
� ROTATING MECHANISM
� NITROGEN INJECTION PIPES
� PNEUMATIC BARRIER REACTOR / ENVIRONMENT
� NITROGEN PADDING ALWAYS ACTIVE
GLASS LINED BAFFLE
� CROSS SECTION “C” SHAPED . (CEPП) – good for suspensions
� pH MEASURE
� MEMBRANE PUMP
� TEMPERATURE MEASURE
� NITROGEN BUBBLING
� SAFE SAMPLING
REACTANTS REACTANTS ““AA””++””BB”” ARE GRADUALLY ADDED IN THE REACTOR.ARE GRADUALLY ADDED IN THE REACTOR.A PUNCTUAL AND GRADUAL ADDITION OF THEM IS ENSURED BY A PROPER A PUNCTUAL AND GRADUAL ADDITION OF THEM IS ENSURED BY A PROPER
INSTRUMENTATION INSTRUMENTATION
PRESSURE CONTROL ON THE PUMP DISCHARGE BY FREQUENCY VARIATOR (INVERTER)
FLOWRATE IS CONTROLED BY A MASS-FLOW-METER AND A CONTROL VALVE (FACILITATED BY THE CONSTANT PRESSURE)
� GASEOUS AMMONIA HAS TO BE REMOVED AS MUCH AS POSSIBLE
� SOLVENT HAS TO BE CONDENSED AS MUCH AS POSSIBLE
� AMMONIA IS MORE SOLUBLE IN THE COLD SOLVENT !!!
!!��CONDENSATION IS DONE AT 2 DIFFERENT TEMPERATURES (+40CONDENSATION IS DONE AT 2 DIFFERENT TEMPERATURES (+40°°C C AND THEN +5AND THEN +5°°C) IN ORDER TO MAXIMIZE THE AMMONIA REMOVAL C) IN ORDER TO MAXIMIZE THE AMMONIA REMOVAL FROM THE BATCHFROM THE BATCH�� AT THE SAME TIME A GOOD CONDENSATION OF THE SOLVENT IS AT THE SAME TIME A GOOD CONDENSATION OF THE SOLVENT IS ACHIEVED ACHIEVED �� 2 CONDENSATORS IN SERIES OPERATE AT +40 AND +52 CONDENSATORS IN SERIES OPERATE AT +40 AND +5°°CC
PROCESS IS MANAGED IN PROCESS IS MANAGED IN ORDER TO ENSURE AN ORDER TO ENSURE AN OUTLET AMMONIA OUTLET AMMONIA FLOWRATE, WHICH ALLOWS FLOWRATE, WHICH ALLOWS A PROPER OPERATION OF A PROPER OPERATION OF THE ABSORPTION COLUMNSTHE ABSORPTION COLUMNS
�� REACTANTS “A”+”B” ARE GRADUALLY ADDED IN THE REACTOR
� CONTROLLED AND GRADUAL DESTRUCTION OF LITHIO AMIDE
� AMMONIA CONVERTION TO AMMONIUM SULPHATE
CONCLUSIONSCONCLUSIONS
� POTENTIALLY DANGEROUS PROCESS
� METHOD FOLLOWED
� DETAILED STUDY OF THE PROCESS BY CALORIMETRIC TRIALS.
� TRIALS ARE PERFORMED WITH A QUANTITY WHICH ALLOWS A REALISTIC SIMULATION OF THE INDUSTRIAL PROCESS